Pyrazolat und Tetrazolat als Brückenliganden in [Pt(pz)2]3, [Pt(pz)2]∞ und [Pt(tz)2]∞ Die Kristallstruktur von [Pt(pz)2]3

Pyrazolat and Tetrazolat as Bridging Ligands in [Pt(pz)₂]₃, [Pt(pz)₂]_∞, and [Pt(tz)₂]_∞ Crystal Structure of [Pt(pz)₂]₃ . [Pt(pz)₂(Hpz)₂]₂ (Hpz = pyrazole) suspended in mesitylene decomposes at 185°C in a sealed tube to [Pt(pz)₂]₃ and [Pt(pz)₂]_∞. The reaction of K₂PtCl₄ with K(pz) under hydrothermal conditions at 150°C yields [Pt(pz)₂H₂O]_∞. [Pt(tz)₂ H₂O]_∞ (Htz = tetrazole) is obtained at 25°C from K₂PtCl₄ and Li(tz) in water. [Pt(pz)₂]₃ crystallizes in the tetragonal space group I4₁/a with a = 1694.9 pm, c = 3127.5 pm and Z = 16. It forms a ring structure with the symmetry D_3h. In the structure the Pt atoms are each bridged by two pyrazolato ligands. Short but nonbonding Pt? Pt distances range from 303.4 pm to 306.7 pm. The average Pt? N distance is 201 pm.     

Synthese und Kristallstruktur von (PPh4)2[Mo2Cl10]

Synthesis and Crystal Structure of (PPh₄)₂[Mo₂Cl₁₀] The title compound is obtained in the reaction of [MoCl₄(Ph? C?C? Ph)]₂ with tetraphenylphosphonium chloride in dichloro methane, forming brown crystals. It is characterized by the i.r. spectrum and a crystal structure analysis by the aid of X-ray diffraction data. The complex crystallizes triclinic in the space group P1 with one formula unit per unit cell. The cell dimensions are a = 1122 pm, b = 1137 pm, c = 1283 pm; α = 63.4°, β = 69.1°, γ = 86.5°. The crystal structure determination (2959 observed, independent reflexions, R = 4.5%) shows the constants of the unit cell to consist of on centrosymmetric anion, two cations and one disordered molecule of dichloro methane. The distance Mo? Mo in the anion is 380 pm, which excludes direct magnetic interaction between the molybdenum atoms.     

Kaliumtriamidostannat(II), K[Sn(NH2)3] – Synthese und Kristallstruktur

Potassium Triamidostannate(II), K[Sn(NH₂)₃] – Synthesis and Crystal Structure Rusty‐red crystals of K[Sn(NH₂)₃] were obtained by the reaction of SnBr₂ and KNH₂ in a 1 : 3 molar ratio in liquid ammonia at 233 K in the form of platelets. The structure was determined from single crystal X‐ray diffractometer data: Space group P3; Z = 2; a = 6.560(1) Å, c = 7.413(2) Å. The structure contains trigonal pyramidal complex anions [Sn(NH₂)₃]^– and potassium cations. These ions are arranged to one another following the motif of a strongly distorted hexagonal close packing of sequence A(Sn) B(Sn) A′(K) B′(K) …     

Lithiumtriamidostannat(II), Li[Sn(NH2)3] – Synthese und Kristallstruktur

Lithium Triamidostannate(II), Li[Sn(NH₂)₃] – Synthesis and Crystal Structure Rusty-red glistening, transparent crystals of Li[Sn(NH₂)₃] were obtained by reaction of metallic lithium with tetraphenyl tin in liquid ammonia at 110 °C. The structure was determined from X-ray single-crystal diffractometer data: Space group P 2₁/n, Z = 4, a = 8.0419(9) Å, b = 7.1718(8) Å, c = 8.5085(7) Å, β = 90.763(8)°, R₁ (F _o ≥ 4σ(F _o)) = 2.8%, wR₂ (F ≥ 2σ(F )) = 5.3%, N(F ≥ 2σ(F )) = 1932, N(Var.) = 65. The crystal structure contains trigonal pyramidal complex anions [Sn(NH₂)₃]^– with tin at the apex, which are connected to layers of sequence A B A B … by lithium in tetrahedra-double units [Li(NH₂)_2/2(NH₂)₂]₂.     

Synthese und Kristallstruktur von (AsPh4)2[Cl5WNSNWCl5]

Synthesis and Crystal Structure of (AsPh₄)₂[Cl₅WNSNWCl₅] . The chlorothionitrene complex [WCl₄(NSCl)]₂ reacts with excess tetraphenylarsonium chloride via the intermediate AsPh₄[Cl₅W(NSCl)] to yield the title compound. This was characterized by its i.r. spectrum and an X-ray crystal structure determination (4078 reflexions uncluding Friedel pairs, R = 0.059). (AsPh₄)₂[Cl₅WNSNWCl₅] crystallizes in the monoclinic system, a = 1110.5, b = 1714.6, c = 1521.7 pm, β = 107.24°, Z = 2. The space group is either P2₁/n with anions statistically disordered in two different positions or Pn with an apparent higher symmetry due to the presence of inversion twins. Bond distances and angles correspond to the formula      

Synthese,Kristallstruktur und Magnetismus von Natriumtetrachlorotitanat(II), Na2TiCl4

Synthesis, Crystal Structure and Magnetism of Sodium Tetrachlorotitanate(II), Na₂TiCl₄ Na₂TiCl₄ is obtained as single crystals by metallothermic reduction of TiCl₃ with sodium (525°C, 90 d, Ta container). Pure powder samples may be prepared by synproportionation of TiCl₃ with Ti in the presence of NaCl (950–520°C, 21 d). The structure refinement from four-circle diffractometer data confirms that Na₂TiCl₄ is isotypic with Sr₂PbO₄ (orthorhombic, space group Pbam (No. 55), Z = 2 a = 694.2(1), b = 1 198.9(2), c = 385.6(1) pm, R = 0.055, R_w = 0,038). Ti²⁺ is surrounded by a distorted octahedron of Cl^?. The octahedra are connected via common edges to chains, [TiCl_2/1Cl_4/2]^2?, that run in the [001] direction. Magnetic susceptibility data were recorded in the 2 to 300 K temperature range at various field strengths. The interpretation of the data was carried out with the aid of crystal-field calculations taking magnetic interactions into account. The non-Curie behaviour of the reciprocal magnetic susceptibility of Ti²⁺ in Na₂TiCl₄ is due to the influence of spin-obit coupling.     

Zur Kristallstruktur von KGaO2 und NaGaO2(II) [1]

The Crystal Structure of KGaO₂ and NaGaO₂(II) By annealing intimate mixtures of K₂O, Na₂O and β-Ga₂O₃ (K : Na : Ga = 2.2 : 1.1 : 1) we obtained single crystals of K₂Na₄[(GaO₃)₂] and KGaO₂ (Ag-cylinder; 600°C, 26 d). Structure refinement for KGaO₂ (four-circle diffractometer data, Mo-Kα , 1 390 or 1 390 I_o(hkl); R = 5.55%, R_w = 3.05%) confirms the space group Pbca; a = 552.1 pm, b = 1 107.5 pm, c = 1 580.7 pm, Z = 16. According to K[GaO_4/2] we have a stuffed cristobalite-related structure. Single crystals of NaGaO₂(II) were grown by annealing intimate mixtures of Na₂O₂ and GaAs (Na₂O₂ : GaAs 4.1 : 1) in Ag-cylinders that were not completely closed (570°C, 6 weeks). Structure refinement for NaGaO₂(II) (four-circle diffractometer data, Mo-Kα , 588 of 616 I_o(hkl); R = 4.54%, R_w = 4.06%) confirms the spacegroup Pna2₁; a = 549.8(1) pm, b = 720.6(1) pm, c = 529.8(1) pm, Z = 4. In NaGaO₂(II) we have a wurtzite-related structure.     

Synthese und Kristallstruktur von [Fe(MeCN)6][Fe2OCl6]

Synthesis and Crystal Structure of [Fe(MeCN)₆][Fe₂OCl₆] [Fe(MeCN)₆][Fe₂OCl₆] ( 2 ) is obtained by passing dry air through a solution of FeCl₂ in acetonitrile in almost quantitative yield. 2 crystallises in the trigonal space group R 3 [a = b = 12.121(1), c = 29.875(6) Å, Z = 6]. The oxygen atom in the Fe₂OCl₆ anion occupies the 3 position and causes therefore an Fe–O–Fe angle of 180°. The refinement in the triclinic space group P1 leads to a slightly bent arrangement of the Fe–O–Fe fragment.     

Synthese und Kristallstruktur von [N(Hex)4][Cu2(CN)3]

Synthesis and Crystal Structure of [N(Hex)₄] [Cu₂(CN)₃] [N(Hex)₄][Cu₂(CN)₃] has been prepared by solvothermal reaction of CuCN with Tetra‐n‐hexylammoniumiodide in acetone. The crystal structure is built up by condensed (CuCN)₆ and (CuCN)₇ rings, forming a zeolith type cyanocuprate(I) framework [Cu₂(CN)₃^—]. Space group R3; α = 44.482(6), c = 21.283(4) Å, V = 36471(9) ų; Z = 9.     

Synthese und Kristallstruktur von (Ph3PNPPh3)2[Cu(N3)4]

Inhaltsübersicht. Die Titelverbindung entsteht neben CuN₃ · PPh₃ bei der Einwirkung von Natriumazid auf CuCl₂ und Triphenylphosphan in siedendem Acetonitril bei Anwesenheit von 15-Krone-5 als Lösungsvermittler für NaN₃. (Ph₃PNPPh₃)₂[Cu(N₃)₄] bildet schwarze Kristalle, die wir durch das IR-Spektrum und durch eine röntgenographische Strukturanalyse charakterisiert haben. Raumgruppe Pbca, Z = 4, (4245 beobachtete unabhängige Reflexe, R = 7,2%), Gitter-abmessungen (20°C):a = 1980, 1;b = 1618,8; c = 2014,3 pm. Die Verbindung besteht aus Kationen [Ph₃PNPPh₃]⁺ und Anionen [Cu(N₃)₄]^2– der Symmetrie C_i, in denen das Cu-Atom planar von den α-N-Atomen der Azidgruppen mit Cu–N-Abständen von 197,2(4) und 189,5(4) pm umgeben ist. Synthesis and Crystal Structure of (Ph₃PNPPh₃)₂[Cu(N₃)₄] The title compound is prepared besides CuN₃ · PPh₃ by the reaction of sodium azide with CuCl₂ and PPh₃ in boiling acetonitrile in the presence of 15-crown-5. (Ph₃PNPPh₃)₂[Cu(N₃)4] forms black crystals, which have been characterized by their IR spectrum as well as by an X-ray structure determination. Space group Pbca, Z = 4 (4245 observed independent reflexions, R = 0.072), lattice dimensions (20°C): A = 1980.1; b = 1618.8; c = 2014.3 pm. The compound consists of Ph₃PNPPh₃⁺ cations and anions [Cu(N₃)₄]^2– with symmetry C₁, in which the copper atom is planarly surrounded by the four nitrogen atoms of the azide groups with bond lengths Cu–N of 197.2(4) and 189.5(4) pm, respectively.     

Synthese und Kristallstruktur von CsAu(SO4)2

Synthesis and Crystal Structure of CsAu(SO₄)₂ Light yellow single crystals of CsAu(SO₄)₂ were obtained upon evaporation of a solution of Au(OH)₃ and Cs₂SO₄ in sulfuric acid (96 % H₂SO₄). In the crystal structure (monoclinic, P2₁/c, Z = 4, a = 1029.7(2), b = 893.4(2), c = 901.0(1) pm, β = 111.08(1)°) Au³⁺ is in square planar coordination of oxygen atoms which belong to four SO₄^— ions. According to [Au(SO₄)_4/2]^— puckered layers are formed which are connected by the Cs⁺ ions. The latter are surrounded by five chelating and three monodentate sulfate groups leading to a CN of 13.     

Synthese und Kristallstruktur von Ba2ScCl7, ein Bariumchlorid-hexachloroscandat(III), Ba2Cl[ScCl6]

Synthesis and Crystal Structure of Ba₂ScCl₇, a Barium Chloride Hexachloroscandate(III), Ba₂Cl[ScCl₆] Colourless single crystals of Ba₂ScCl₇ are obtained from a 1 : 1 molar mixture of BaCl₂ and ScCl₃. It crystallizes with the non-centrosymmetric monoclinic space group P2₁ with a = 688,88(7), b = 1349,4(1), c = 1207,4(1), β = 94,93(1)° in a new structure that contains isolated [ScCl₆] octahedra and one ‘‘lonesome”︁”︁ chloride ligand according to Ba₂Cl[ScCl₆].     

Synthese und Kristallstruktur von LiAl[(P2O6)2]

Synthesis and Crystal Structure Determination of LiAl[(P₂O₆)₂] Single crystals of previously unknown LiAl[(P₂O₆)₂] have been obtained by reaction of Li₂CO₃, Al₂O₃ and H₃PO₄ (1:1:16) at 350°C. The title compound crystallizes in Pbcn (a = 1 244.54(1), b = 823.40(1), c = 892.46(1) pm; Z = 4). The least-squares refinement (with anisotropic temperature factors) was performed using 766 observed reflections yielding R = 0.029 and R(w) = 0.075. Four anion chains are running parallel to the shortest axis in the unit cell, the period of identity amounting to four. Aluminium is surrounded by an almost regular octahedron, lithium by a distorted tetrahedron of oxygen.     

Darstellung und Kristallstruktur von [Li(DME)2I]

Synthesis and Crystal Structure of [Li(DME)₂I] . LiI can be dissolved at 50°C in toluene/DME (2:1). At - 20°C [Li(DME)₂I] ( 1 ) was isolated in 75% yield. 1 was characterized by NMR techniques as well as an X-Ray structure determination. 1 crystallizes in the space group C2/c with a = 1 356.9(2), b = 813.2(1), c = 1 259.1(2) pm, and β = 99.74(1)°.     

Synthese und Kristallstruktur von [Na(12-Krone-4)2]2[Hg(Se4)2] · 1,5 DMF

Synthesis and Crystal Structure of [Na(12-Crown-4)₂]₂[Hg(Se₄)₂] · 1.5 DMF . The title compound has been prepared by the reaction of Na₂Se₄ with mercury acetate in DMF solution in the presence of 15-crown-5, forming dark red crystal needles. [Na(12-crown-4)₂]₂[Hg(Se₄)₂] · 1.5 DMF crystallizes in the space group C2/c with eight formula units per unit cell. The structure was determined with 3 824 observed unique reflections, R = 0.085. Lattice dimensions at - 70°C: a = 2 884(2), b = 1 407.7(7), c = 2 843(2) pm, β = 93.93(5)°. The structure consists of [Na(12-crown-4)₂]⁺ ions with a sandwichlike coordination of the crown ether molecules, and of [Hg(Se₄)₂]^2? ions, in which the mercury atom is coordinated by two tetraselenido ions in a chelating fashion. The [Hg(Se₄)₂]^2? ions are arranged to infinite chains via Se…?Se contacts.     

Synthese und Kristallstruktur von Na2Zn(OH)4

Synthesis and Crystal Structure of Na₂Zn(OH)₄ Crystallization from saturated sodium hydroxozincate solutions yields colourless platelets of crystals of Na₂Zn(OH)₄. The X‐ray structure determination on these crystals was successful including all hydrogen positions. P2₁/n, Z = 4, a = 7.959(3) Å, b = 6.534(1) Å, c = 8.501(3) Å, β = 93.97(3)°, N(F²_o ° 2σ F²_o) = 1668, N(Var.) = 81, R₁/wR₂ = 0.043/0.107. Na₂Zn(OH)₄ crystallizes in a layered structure. Alternate layers contain Na⁺ in octahedral and Zn²⁺ in tetrahedral coordination by OH^–.     

Synthese und Kristallstruktur von (PPh4)2Se6

Synthesis and Crystal Structure of (PPh₄)₂Se₆ (PPh₄)₂Se₆ has been prepared by the reaction of selenium with K₂Se₂ in dimethylformamide solution in the presence of K₃[Mn(CN)₆] and PPh₄Br, forming black crystal needles. According to the crystal structure determination the compound consists of PPh⁺₄ ions and chainlike hexaselenide ions. Space group P6 , Z = 2,4683 Observed unique reflections, R = 0.066. Lattice dimensions at ?90°C: a = 951.0, b = 1094.8, c = 2137.4 pm, α = 82.66°, β = 83.36°, γ = 89.96°.     

Synthese und Kristallstruktur von [{(tBu2P)2InCl}2]

Synthesis and Crystal Structure of [{(tBu₂P)₂InCl}₂] The reaction of InCl₃ with tBu₂PSiMe₃ leads to [{(tBu₂P)₂InCl}₂] ( 1 ). 1 crystallizes in the space group P2₁/c. The lattice constants (at 216 K) are: a = 945.9(5) pm, b = 1 604.1(9) pm, c = 1 636.8(8) pm, β = 100.55(4)°. 1 contains a planar In₂P₂ ring. Each In atom is coordinated by two bridging tBu₂P groups, a terminal tBu₂P group and a terminal Cl atom. The coordination geometry of the In atoms is roughly tetrahedral.     

Kristallstruktur und Stereochemie von [2-(Diorganophosphinyl)phenyl]-dimethylzinnchloriden

Crystal Structure and Stereochemistry of [2-(Diorganophosphinyl)phenyl]-dimethyltin Chlorides The crystal structure of [2-(Diphenylphosphinyl)phenyl]-dimethyltin chloride (1) has been determined and refined to an R value of 0.038. The configuration around the tin atom corresponds to a distorted trigonal bipyramid with an intramolecular distance Sn…0 of 235.7(9) pm. The planar arrangement of the five-membered chelate ring represents the transition between two envelope conformations. Temperature and solvent dependent NMR measurements confirm for [2-(t-Butylphenylphosphinyl)phenyl]-dimethyltin chloride (2) a stable configuration of the ligand polyhedron at the tin atom within the NMR time scale.     

Synthese und Kristallstruktur von Bis(1,2-dimethyl-5-nitro-imidazol)dichlorocobalt(II)

Synthesis and Crystal Structure of Bis(1,2-dimetyl-5-nitro-imidazole)dichlorocobalt(II) Bis(1,2-dimethyl-5-nitro-imidazol)dichlorocobalt(II) was obtained by reaction of CoCl₂ · 6 H₂O with 1,2-dimethyl-5-nitro-imidazole in methanol. The compound forms blue crystals which were characterized by IR and UV-vis spectroscopy and by an X-ray crystal structure determination. Co(C₅H₇N₃O₂)₂Cl₂: tetragonal, space group I4 2d, Z = 8, a = 1142.1(1) pm, c = 2577.3(2) pm. R = 0.036 for 670 independent reflexions. The Co atom is tetrahedrally surrounded by two chlorine and two N atoms at distances of 222.8(2) and 203.5(4) pm.