Synthese,Kristallstruktur und Festkörper-NMR-spektroskopische Untersuchungen von K5H(CN2)3

Synthesis, Crystal Structure, and Solid State MAS-NMR Spectroscopic Investigation of K₅H(CN₂)₃ Single phase K₅H(CN₂)₃ was synthesized by reaction of KHCN₂ with metallic potassium in liquid ammonia or by reaction of KNH₂ with melamine C₃N₃(NH₂)₃ at 320 °C, respectively. The crystal structure was determined from X-ray powder and single crystal data: K₅H(CN)₃, space group Im3m, a = 795.68(7) pm, Z = 2, R1 = 0.025, wR2 = 0.0438. In the solid K₅H(CN₂)₃ contains K⁺ and CN₂^2–, the anions exhibit D_∞h symmetry. According to ¹H and ¹³C solid state MAS-NMR investigations, temperature dependent impedance spectroscopy, and FTIR spectroscopy the protons are only loosely bound to the CN₂^2– ions. The proton conductivity shows a sharp increase above 70 °C.     

Synthese und Kristallstruktur von Te3O3(PO4)2, einer Verbindung mit fünffach koordiniertem Tellur(IV)

Synthesis and Crystal Structure of Te₃O₃(PO₄)₂, a Compound with 5‐fold Coordinate Tellurium(IV) Polycrystalline Te₃O₃(PO₄)₂ is formed during controlled dehydration of (Te₂O₃)(HPO₄) with (Te₈O₁₀)(PO₄)₄ as an intermediate product. Colourless single crystals were prepared by heating stoichiometric amounts of the binary oxides P₂O₅ und TeO₂ in closed silica glass ampoules at 590 °C for 8 hours. The crystal structure (P2₁/c, Z = 4, α = 12.375(2), b = 7.317(1), c = 9.834(1)Å, β = 98.04(1)°, 1939 structure factors, 146 parameters, R[F² > 2σ(F²)] = 0.0187, wR2(F² all) = 0.0367) was determined from four‐circle diffractometer data and consists of [TeO₅] polyhedra und PO₄ tetrahedra as the main building units. The framework structure is made up of cationic zigzag‐chains of composition [Te₂O₃]²⁺ which extend parallel to [001] and anionic [Te(PO₄)₂]^2— units linked laterally to these chains. This leads to the formation of [Te₂O₃][Te(PO₄)₂] layers parallel to the bc plane which are interconnected via weak Te‐O bonds.     

Selten‐Erd‐Metall‐Koordinationspolymere: Synthese und Kristallstrukturen von fünf neuen Adipinaten, [M2(Adi)3(H2O)4](AdiH2)(H2O)4 (M = La,Nd), [Er(Adi)(H2O)5]Cl(H2O) und [M(Adi)(H2O)5](NO3)(H2O) (M = Gd,Er)

Rare‐Earth‐Metal Coordination Polymers: Synthesis and Crystal Structures of Five New Adipinates, [M₂(Adi)₃(H₂O)₄](AdiH₂)(H₂O)₄ (M = La, Nd), [Er(Adi)(H₂O)₅]Cl(H₂O) and [M(Adi)(H₂O)₅](NO₃)(H₂O) (M = Gd, Er) The new rare‐earth compounds [M₂(Adi)₃(H₂O)₄](AdiH₂)(H₂O)₄ (M = La ( 1 ), Nd ( 2 )), [Er(Adi)(H₂O)₅]Cl(H₂O) ( 3 ) and [M(Adi)(H₂O)₅](NO₃)(H₂O) (M = Gd ( 4 ), Er ( 5 )) were obtained from the reaction of adipinic acid with La(OH)₃·xH₂O, Nd₂O₃, ErCl₃·6H₂O, Gd(NO)₃·xH₂O and Er₂O₃, respectively. Their crystal structures were determined by single‐crystal X‐ray diffraction. The coordination polymers [M₂(Adi)₃(H₂O)₄](AdiH₂)(H₂O)₄ crystallize in the triclinic space group (no. 2) with a = 875.4(1), b = 1000.4(2), c = 1179.0(2) pm, α = 74.70(1), β = 69.85(1), γ = 86.18(2)° and Z = 1 (crystal data for M = La, ( 1 )). The quasi‐isostructural compounds [Er(Adi)(H₂O)₅]Cl(H₂O) ( 3 ) and [M(Adi)(H₂O)₅](NO₃)(H₂O) (M = Gd ( 4 ), Er ( 5 )) crystallize with monoclinic symmetry, space group C2/c (no. 15) with lattice parameters of a = 1231.5(1), b = 1532.6(1), c = 895.4(1) pm, β = 123.44(1)° and Z = 4 (crystal data for ( 3 )). The rare‐earth cations have the coordination numbers 10 ( 1 , 2 ) and 9 ( 3 , 4 and 5 ), respectively. The compounds [M₂(Adi)₃(H₂O)₄](AdiH₂)(H₂O)₄ are constructed of infinite chains of edge‐sharig [MO₈(H₂O)₂] polyhedra that are cross‐linked by adipinic acid molecules to form framework structures. In [Er(Adi)(H₂O)₅]Cl(H₂O) ( 3 ) and [M(Adi)(H₂O)₅](NO₃)(H₂O) (M = Gd ( 4 ), Er ( 5 )) the central cations are bridged by adipinic acid molecules in a bidentate‐chelating manner to positively charged zigzag chains. Between these the counter ions and crystal water molecules are incorporated.     

Synthese und Kristallstruktur der Rhenium(VII)‐Nitridchloride ReNCl4 und ReNCl4·H2O

Syntheses and Crystal Structures of the Rhenium(VII) Nitride Chlorides ReNCl₄ and ReNCl₄·H₂O Rhenium(VII) nitride chloride, ReNCl₄ ( 1 ) is obtained in form of brown needles with metallic luster by the reaction of ReCl₅ with Cl₃VNCl at 140 °C under vacuum in a sealed glass ampoule. It crystallizes in the tetragonal space group I4 with the lattice parameters a = 826.7(4), c = 405.1(2) pm, and Z = 2. The square pyramidal molecules are connected by asymmetric nitrido bridges to form chains along the crystallographic c axis. The shorter Re‐N distance of 163.0(5) pm corresponds to a triple bond, while the pronounced longer distance of 242.0(5) pm can be interpreted with a weak donor bond. The reaction of ReCl₅ with VN at 170 °C under vacuum in a sealed glass ampoule yields red needles of ReNCl₄·H₂O ( 2 ). It crystallizes in the orthorhombic space group Pnma with a = 1075.4(2), b = 1108.5(2), c = 547.7(5) pm and Z = 4. The Re atoms exhibit a distorted octahedral coordination with the aqua ligand in trans position to the nitrido ligand. The Re‐N triple bond has a bond distance of 166.1(11) pm. The complexes are connected by hydrogen bridges O‐H···N to form chains.     

Das wasserfreie Lanthanacetat,La(CH3COO)3, und sein Precursor,NH4)3[La(CH3COO)6] · 1/2 H2O: Synthese,Strukturen, thermisches Verhalten

Anhydrous Lanthanum Acetate, La(CH₃COO)₃, and its Precursor, ·NH₄)₃[La(CH₃COO)₆] · 1/2 H₂O: Synthesis, Structures, Thermal Behaviour Single crystals of (NH₄)₃[La(CH₃COO)₆] · ½ H₂O are obtained by refluxing La₂O₃in (CH₃COO)₃ · 1.5 H₂O with an excess of NH₄CH₃COO in methanol. The crystal structure (trigonal, R3 , Z = 6, a = 1 365.0(3) pm, c = 2 360(1) pm, R = 0.088, R_w = 0.061 exhibits the coordination number of nine for La³⁺, which is surrounded by three chelating-type bidentate and three unidentate acetate groups. Characteristic are monomeric units of [La(CH₃COO)₆]^3? which are connected to a three-dimensional network by hydrogen bonds with the NH ions. Thermal decomposition consists of four steps with La(CH₃COO)₃, La₂(CO₃)₃ and La₂O₂CO₃ as intermediates and La₂O₃ as the final Product. Single crystals of La(CH₃COO)₃ are obtained from La₂O₃ in a melt of NH₄CH₃COO (molar ratio 1:12) in a sealed glass ampoule. The crystal structure (trigonal, R3 , Z = 18, a = 2 203.0(5) pm; c = 987.1(3) pm, R = 0.027, R_w = 0.023) shows the coordination number of ten for La³⁺. These are three-dimensionally connected by oxygen atoms of the acetate groups with two tetradentate double-bridging and one Z,Z-type-bridging bidentate acetate group.     

AlCl3 · 2NH3 – eine Verbindung mit der Kristallstruktur eines Tetraammindichloroaluminium-tetrachloroaluminats – [AlCl2(NH3)4]+[AlCl4]−

ACl₃ · 2NH₃ – a Compound with the Crystal Structure of a Tetraammine Dichloroaluminiumtetrachloroaluminate – [AlCl₂(NH₃)₄]⁺[AlCl₄]^? Ammoniates of aluminiumchloride AlCl₃ · xNH₃ are in discussion as starting materials for the synthesis of aluminiumnitride. Therefore the reactions of melts of monoamminealuminiumchloride with ammonia were investigated. They react at 150°C within 10 min with one mole of ammonia to the diammoniate, [AlCl₂(NH₃)₄]⁺[AlCl₄]^?. The pure compound can be obtained by sublimation at 200°C in vacuumline apparatus. X-ray structure determination on [AlCl₂(NH₃)₄]⁺[AlCl₄]^? was carried out: see “Inhaltsübersicht”.     

AlCl3 · 3NH3 — eine Verbindung mit der Kristallstruktur eines Tetraammindichloroaluminium-diammintetrachloroaluminats: [AlCl2(NH3)4]+[AlCl4(NH3)2]−

AlCl₃ · 3NH₃ — a Compound with the Crystal Structure of a Tetraammine Dichloro Aluminium-Diammine Tetrachloro Aluminate: [AlCl₂(NH₃)₄]⁺[AlCl₄(NH₃)₂]^? . AlCl₃ · 3 NH₃ ? [AlCl₂(NH₃)₄]⁺ [AlCl₄(NH₃)₂]^? forms during the reaction of two mole NH₃ with AlCl₃(NH₃) at T ≥ 200°C. Repeated heating and cooling within 48 h between 200°C and 250°C gives a homogeneous product with total uptake of the necessary amount of NH₃. Slow sublimation in a vacuum line apparatus at 200°C gives crystals of the triammoniate sufficient for a X-ray structure determination: The compound contains elongated [AlCl₂(NH₃)₄]⁺ octahedra and compressed [AlCl₄(NH₃)₂]^? octahedra. Besides ionic bonding hydrogen bridge bonds with 3.369 Å ? d(N—H … Cl) ? 3.589 Å stabilize the atomic arrangement.     

Synthese und Kristallstruktur von Rb8[P4N6(NH)4](NH2)2 mit dem adamantanartigen Anion [P4N6(NH)4]6−

Synthesis and Crystal Structure of Rb₈[P₄N₆(NH)₄](NH₂)₂ with the Adamantane-like Anion [P₄N₆(NH)₄]^6? RbNH₂ reacts with P₃N₅ (molar ratio 6:1) at 400°C within 5 d to colourless Rb₈[P₄N₆(NH)₄](NH₂)₂. Suitable crystals for a X-ray structure determination were obtained: The compound contains adamantane-like molecular anions [P₄N₆(NH)₄]^6?. Their centres of gravity are arranged in a distorted hexagonal primitive array. All trigonal prisms of this array contain one amide ion. Rubidium ions connect the anions irregularly.     

Über Neue Oxoruthenate vom Typ der 6 L-Perowskite: Ba3SrRu2−xTaxO9 (x = 0,8 und 1,4) mit einem Beitrag über Ba3CaRu2O9

On Novel Oxoruthenates of the 6 L-Perovskite Type: Ba₃SrRu_2?xTa_xO₉ (x = 0.8 and 1.4) with a Comment on Ba₃CaRu₂O₉ Single crystals of the phases Ba₃SrRu_2?xTa_xO₉ [(I): x = 0.8 and (II): x = 1.4] and the compound (III): Ba₃CaRu₂O₉ were prepared by a BaCl₂ flux and investigated by X-ray methods. (I)–(III) crystallizes with hexagonal symmetry space group P6 2c with lattice constants: (I) a = 6.003 Å; c = 15.227 Å; (II) a = 5.988 Å; c = 15.220 Å and (III) a = 5.891 Å; c = 14.571 Å. The crystal structures of these substances corresponds to the 6 layer perovskites with the stacking sequence (hcc)₂. All of them show a so far not described slightly distorted oxygen framework caused by the Sr²⁺ and Ca²⁺ ions.     

Synthese und Kristallstruktur von Cu4[PhN3C6H4N3(H)Ph]4(μ2-O)2, einem vierkernigen Kupfer(II)-Komplex mit 1-Phenyltriazenido-2-phenyltriazenobenzol als Ligand

Synthesis and Crystal Structure of Cu₄[PhN₃C₆H₄N₃(H)Ph]₄(μ₂-O)₂, a Tetranuclear Copper(II) Complex with 1-Phenyltriazenido-2-phenyltriazeno-benzene as Ligand Cu₄[PhN₃C₆H₄N₃(H)Ph]₄(μ-O)₂ ( 1 ) results from the reaction of an aqueous solution of [Cu(NH₃)₄]²⁺ with 1,2-bis(phenyltriazeno)benzene in ether. 1 crystallizes in the orthorhombic space group Pba2 with the lattice parameters a = 1661.5(5), b = 1914.7(7), c = 1269.2(5) pm; Z = 2. In the tetrameric complex with the symmetry C₂ the Cu²⁺ cations form a tetrahedron (Cu? Cu: 298.3(1)?337.1(1) pm). The μ₂-oxo ligands occupy the twofold axis and bridge two opposite edges of the Cu₄ tetrahedron (Cu? O: 190.0(3) and 192.5(4) pm). The 1-phenyltriazenido-2-phenyltriazeno benzene anions bridge two Cu²⁺ ions chelating one metal ion and coordinating monodentate the neighbouring one (Cu? N: 191.0(5)–204.1(4) pm).     

Synthese,Struktur und magnetische Eigenschaften der Verbindungen NaMIIZr2F11 (MII = Ti,V und Cu) und einem Anhang über NaPdZr2F11

Synthesis, Structure, and Magnetic Properties of Compounds NaM^IIZr₂F₁₁ (M^II = Ti, V, Cu) and a Notice on NaPdZr₂F₁₁ By synthesizing NaTiZr₂F₁₁ in form of red single crystals, it was possible to obtain a complex fluoride with Ti²⁺ for the first time. It crystallizes like the analogous greenish blue vanadium compound isotypic to AgPdZr₂F₁₁ [1] monoclinic, spacegroup C2/m–C (No. 12) with a = 918.0/911.5 pm, b = 682.6/675.7 pm, c = 780.8/776.6 pm, β = 116.2/116.2º and Z = 2. Colourless NaCuZr₂F₁₁ however crystallizes as a result of the Jahn-Teller distortion of Cu²⁺ triclinic (space group P1 –C (No. 2), a = 552.7 pm, b = 568.2 pm, c = 768.0 pm, α = 111.0º, β = 97.4º, γ = 106.4º) and is – as expected – isotypic to NaAgZr₂F₁₁ [1].     

Über die Reaktion von Cp2TiCl2 mit [C(NMe2)3][(CO)4FeC(O)NMe2] – Kristallstruktur von [C(NMe2)3]2[FeCl4]

Concerning the Reaction of Cp₂TiCl₂ with [C(NMe₂)₃][(CO)₄FeC(O)NMe₂] – Crystal Structure of [C(NMe₂)₃]₂[FeCl₄] The title compound forms by the reaction of Cp₂TiCl₂ with [C(NMe₂)₃][(CO)₄FeC(O)NMe₂] in THF solution. It crystallizes in the space group Pbcn with a = 1 566.6(3); b = 976.4(2); c = 1 580.4(4) pm; Z = 4; R = 3.8%. Each [FeCl₄]^2? in is surrounded by eight cations. Two cations each are connected with one Cl atom by relatively short H …? Cl contacts leading to a distortion of the tetrahedral geometry of the anion.     

Synthese und Struktur von Tetrachloro[4-tert-butyl-2(diphenylphosphanyl-κP-methyl)phenolato-κO]tantal(V), ein neuartiger TaV-Komplex mit einem chelatisierenden Aryloxyphosphanliganden

Synthesis and Structure of Tetrachloro[4- tert -butyl-2(diphenylphosphanyl-κP-methyl)phenolato-κO]tantalum(V), a Novel Ta^V Complex with a Chelating Aryloxy Phosphane Ligand 4-tert-Butyl-2-(diphenylphosphanylmethyl)anisol ( 1 ) is prepared from 2-chlormethyl-4-tert-butylanisol and potassium diphenylphosphide in very good yields as a novel oxygen-phosphorus compound with potentially hemilabile ligand properties. Compound 1 reacts with tantalum pentachloride under cleavage of methylchloride revealing the complex tetrachloro[4-tert-butyl-2-(diphenylphosphanyl-κP-methyl)phenolato-κO]tantalum(V) ( 2 ) with a distorted octahedrally coordinated tantalum atom and a chelating aryloxy phosphane ligand. Complex 2 crystallizes in the tetragonal, chiral space group P4₁2₁2 with a = 11.719(5), c = 37.95(5) Å, V = 5171(7) ų, Z = 8. ³¹P NMR spectroscopic studies of 2 establish the coordination of the phosphane unit to the Ta^V center in solution.     

Über die Kristallstrukturen der Cyanokomplexe [Co(NH3)6][Fe(CN)6], [Co(NH3)6]2[Ni(CN)4]3 · 2 H2O und [Cu(en)2][Ni(CN)4]

On the Crystal Structures of the Cyano Complexes [Co(NH₃)₆][Fe(CN)₆], [Co(NH₃)₆]₂[Ni(CN)₄]₃ · 2 H₂O, and [Cu(en)₂][Ni(CN)₄] Of the three title compounds X‐ray structure determinations were performed with single crystals. [Co(NH₃)₆][Fe(CN)₆] (a = 1098.6(6), c = 1084.6(6) pm, R3, Z = 3) crystallizes with the CsCl‐like [Co(NH₃)₆][Co(CN)₆] type structure. [Co(NH₃)₆]₂[Ni(CN)₄]₃ · 2 H₂O (a = 805.7(5), b = 855.7(5), c = 1205.3(7) pm, α = 86.32(3), β = 100.13(3), γ = 90.54(3)°, P1, Z = 1) exhibits a related cation lattice, the one cavity of which is occupied by one anion and 2 H₂O, whereas the other contains two anions parallel to each other with distance Ni…Ni: 423,3 pm. For [Cu(en)₂][Ni(CN)₄] (a = 650.5(3), b = 729.0(3), c = 796.5(4) pm, α = 106.67(2), β = 91.46(3), γ = 106.96(2)°, P1, Z = 1) the results of a structure determination published earlier have been confirmed. The compound is weakly paramagnetic and obeys the Curie‐Weiss law in the range T < 100 K. The distances within the complex ions of the compounds investigated (Co–N: 195.7 and 196.4 pm, Ni–C: 186.4 and 186.9 pm, resp.) and their hydrogen bridge relations are discussed.     

Synthese und Kristallstruktur von Na10[P4(NH)6N4](NH2)6(NH3)0,5 mit dem adamantanartig aufgebauten Anion [P4(NH)6N4]4−

Synthesis and Crystal Structure of Na₁₀[P₄(NH)₆N₄](NH₂)₆(NH₃)_0.5 with an Adamantane-like Anion [P₄(NH)₆N₄]^4? Crystals of Na₁₀[P₄(NH)₆N₄](NH₂)₆(NH₃)_0.5 were obtained by the reaction of P₃N₅ with NaNH₂ (molar ratio 1:20) within 5 d at 600°C in autoclaves. The following data characterize X-ray investigations: Fm3 m, Z = 8, a = 15.423(2) Å, Z(F) = 261 with F ≥ 3 σ(F) Z(Variables) = 27, R/R_w = 0.086/0.089 The compound contains the hitherto unknown anion [P₄(NH)₆N₄]^4?, which resembles adamantane. The total structure can be described as follows: The centers of gravity of units of [Na₈(NH₂)₆(NH₃)]²⁺ – 8Na⁺ on the corners of a cube, 6NH₂^? on the ones of an inscribed octahedron with NH₃ in the center – follow the motif of a cubic-closest packed arrangement. Units of [Na₁₂(NH₂)₆]⁶⁺ – 12Na⁺ on the corners of a cuboctahedron and 6NH₂^? on the ones of an inscribed octahedron – occupy all octahedral and those of [P₄(NH)₆N₄]^4? all tetrahedral sites.     

Über Oxidtelluride (M2O2Te) der leichten Lanthanide (M = La–Nd,Sm–Ho) im A-Typ mit anti-ThCr2Si2-Struktur

On Oxytellurides (M₂O₂Te) of the Early Lanthanides (M = La–Nd, Sm–Ho) with A- or anti -ThCr₂Si₂-Type Crystal Structure By reacting elementary lanthanide metal (M = La–Nd, Sm–Ho) with tellurium dioxide (TeO₂) in a 2 : 1 molar ratio, it is possible to obtain pure and single-phase oxytellurides of the composition M₂O₂Te at 750 °C in evacuated silica tubes within a few days. When larger quantities of cesium chloride (CsCl) are added as flux, plate-like single crystals with square cross-section are formed which are not sensitive to hydrolysis and very suitable for crystal structure refinements from X-ray data. In the anti-ThCr₂Si₂ analogous crystal structure (tetragonal, I4/mmm, Z = 2; La₂O₂Te: a = 412.31(4), c = 1309.6(1) pm; Ce₂O₂Te: a = 408.17(4), c = 1294.7(1) pm; Pr₂O₂Te: a = 405.62(4), c = 1285.8(1) pm; Nd₂O₂Te: a = 403.08(4), c = 1277.1(1) pm; Sm₂O₂Te: a = 399.83(4), c = 1265.5(1) pm; Eu₂O₂Te: a = 397.56(4), c = 1257.9(1) pm; Gd₂O₂Te: a = 396.20(4), c = 1253.2(1) pm; Tb₂O₂Te: a = 393.89(4), c = 1245.4(1) pm; Dy₂O₂Te: a = 392.34(4), c = 1240.3(1) pm; Ho₂O₂Te: a = 390.57(6), c = 1239.0(3) pm) the M³⁺ cations are surrounded by nine anions (4 O^2– und 4 + 1 Te^2–) in the shape of a capped square antiprism. The anions show coordination numbers of four (O^2–: tetrahedra) and eight plus two (Te^2–: bicapped cubes) with respect to the cations. PbO-analogous square {[OM_4/4]₂}²⁺ triple layer slabs are present parallel (001), which originate through two-dimensional infinite linking of [OM₄]¹⁰⁺ tetrahedra via two trans-orientated pairs of edges (i. e. four edges altogether). These cationic layers are piled alternatingly along [001] with likewise quadratic single layers of Te^2– anions, which take care of the three-dimensional coherence as well as of the charge balance.     

Ein Beitrag Über die Verbindung CaBeNd2O5 und Phasen der Zusammensetzung M1−xM′xBeLn2O5 (M = Ca,Ba; M′ = Sr; x = 0,5)

A Contribution on the Compound CaBeNd₂O₅ and Phases of the Composition M_1?xM_x'BeLn₂O₅ (M = Ca, Ba; M′ = Sr; x = 0.5). CaBeNd₂O₅ and the phases (I): Ba_0,5Sr_0,5BeLa₂O₅ and (II): Ca_0,5Sr_0,5BeDy₂O₅ have been prepared by high temperature reactions using a CO₂-LASER. They crystallize with orthorhombic symmetry, space group D-Pnma, CaBeNd₂O₅: a = 9.448(1), b = 7.155(1), c = 6.483(1) Å; (I) a = 9.821(4), b = 7.436(3), c = 6.734(3) Å; (II): a = 9.352(2), b = 7.016(2), c = 6.375(2) Å; Z = 4, and belong to the isotypic series CaBeLn₂O₅ and SrBeLn₂O₅. Calculations of Coulomb energies of ordered BaBeLn₂O₅ and EuBeLn₂O₅ and disordered CaBeLn₂O₅, SrBeLn₂O₅ and EuBeNd₂O₅ show dependencies of the ionic radii of the M²⁺ and Ln³⁺ ions as well as of the order/disorder state.     

Untersuchungen über Zinn(IV)-alkoxide. II. Isolierung und Charakterisierung der Verbindung Sn3O(OiBu)10 · 2i-BuOH. Das erste Beispiel für ein partielles Hydrolyseprodukt eines Zinn(IV)-alkoxids

Investigations into Tin(IV) Alkoxides. II. Isolation and Characterization of the Compound Sn₃O(OⁱBu)₁₀₁₀ · 2i-BuOH. The First Example of a Partially Hydrolized Tin(IV) Alkoxide The partial hydrolysis product Sn₃O(OⁱBu)₁₀ · 2i-BuOH was obtained by slow hydrolysis of the reaction product of tin tetrachloride with sodium isobutoxide. The compound forms colourless, moisture sensitive crystals, which easily release the coordinated solvent molecules in dry air. Its crystal and molecular structure has been determinated by single crystal X-ray diffraction. The compound crystallizes in the triclinic space group P1 with a = 1363.5(7), b = 1462.7(10), c = 1637.7(7) pm, α = 95.40(5)°, β = 96.79(4)°, γ = 102.12(5)° and Z = 2. The crystal structure consists of discrete, trimeric molecules with octahedrally coordinated tin atoms which are connected to each other corresponding to the formulation Sn₃(μ₃-O)(μ₂-OⁱBu)₃(O¹Bu)₇ · (i-BuOH)₂ by three isobutoxide groups bridging two metal atoms and a single threefold bridging oxygen atom