Solvothermal synthesis and characterisation of new one-dimensional indium and gallium sulphides: [C10N4H26]0.5[InS2] and [C10N4H26]0.5[GaS2]

Two new main group metal sulphides, [C₁₀N₄H₂₆]_0.5[InS₂] (1) and [C₁₀N₄H₂₆]_0.5[GaS₂] (2) have been prepared solvothermally in the presence of 1,4-bis(3-aminopropyl)piperazine and their crystal structures determined by single-crystal X-ray diffraction. Both compounds are isostructural and crystallise in the monoclinic space group P2₁/n (Z=4), with a=6.5628(5), b=11.2008(9), c=12.6611(9) Å and β=94.410(4)° (wR=0.035) for compound (1) and a=6.1094(5), b=11.2469(9), c=12.7064(10) Å and β=94.313(4)° (wR=0.021) for compound (2). The structure of [C₁₀N₄H₂₆]_0.5[MS₂] (M=In,Ga) consists of one-dimensional [MS₂]⁻ chains which run parallel to the crystallographic a axis and are separated by diprotonated amine molecules. These materials represent the first example of solvothermally prepared one-dimensional gallium and indium sulphides.     

Hydrothermal synthesis of [C6H16N2][In2Se3(Se2)]: A new one-dimensional indium selenide

A new organically templated indium selenide, [C₆H₁₆N₂][In₂Se₃(Se₂)], has been prepared hydrothermally from the reaction of indium, selenium and trans-1,4-diaminocyclohexane in water at 170 °C. This material was characterised by single-crystal and powder X-ray diffraction, thermogravimetric analysis, UV-vis diffuse reflectance spectroscopy, FT-IR and elemental analysis. The compound crystallises in the monoclinic space group C2/c (a=12.0221(16) Å, b=11.2498(15) Å, c=12.8470(17) Å, β=110.514(6)°). The crystal structure of [C₆H₁₆N₂][In₂Se₃(Se₂)] contains anionic chains of stoichiometry [In₂Se₃(Se₂)]²⁻, which are aligned parallel to the [1 0 1] direction, and separated by diprotonated trans-1,4-diaminocyclohexane cations. The [In₂Se₃(Se₂)]²⁻ chains, which consist of alternating four-membered [In₂Se₂] and five-membered [In₂Se₃] rings, contain perselenide (Se₂)²⁻ units. UV-vis diffuse reflectance spectroscopy indicates that [C₆H₁₆N₂][In₂Se₃(Se₂)] has a band gap of 2.23(1) eV.     

Hydrothermal synthesis and characterization of two new layered vanadium tellurites Cu(TATP)V2TeO8 and Cu(DPPZ)V2Te2O10

Two new vanadium tellurites, Cu(TATP)V₂TeO₈ (1) and Cu(DPPZ)V₂Te₂O₁₀ (2), (TATP=1,4,8,9-tetranitrogen-trisphene, DPPZ=dipyridophenazine) have been synthesized under hydrothermal conditions and structurally characterized by elemental analyses, IR, and single-crystal X-ray diffraction. Compound 1 features an interesting two-dimensional layer structure constructed by [V₂TeO₈]_n double-chain-like ribbons linked by [Cu(TATP)]²⁺ bridges. Compound 2 consists of two types of chiral layers: one left-handed and the other right-handed, which lead to racemic solid-state compound. In each layer, there exist two types of inorganic helical chains (V₄Te₄O₈)_n and (Te₂O₂)_n, with same handedness. Two types of helical chains are linked by μ₃(O6) atoms to generate a V/Te/O inorganic anionic layer. The [Cu(DPPZ)]²⁺ cationic complex fragments are covalently bonded to the layer, projecting below and above the vanadium tellurites layer.     

Synthesis, Structure and Thermal Property of [(n-C16H33)N(CH3)3]2[TiF6]·2H2O

A new compound dicetyltrimethylammonium hexafluorotitanium dihydrate, [(n-C₁₆H₃₃)N(CH₃)₃]₂[TiF₆]·2H₂O (compound 1), was hydrothermally synthesized at 150 °C and characterized by single crystal X-ray diffraction, Fourier-transform infrared (FTIR) spectroscopy, elemental analysis, and thermogravimetric analysis. Compound 1 crystallizes in the monoclinic system, space group C2/c. It consists of hexafluorotitanium cations [TiF₆]²⁻, water molecular (H₂O), and cetyltrimethylammonium ions [(n-C₁₆H₃₃)N(CH₃)₃]⁺, which are connected together by extensive hydrogen bonding.     

Synthesis, crystal structure and NLO property of a nonmetal pentaborate [C6H13N2][B5O6(OH)4]

A nonmetal pentaborate [C₆H₁₃N₂][B₅O₆(OH)₄] (1) has been synthesized by 1,4-diazabicyclo[2.2.2] octane (DABCO) and boric acid, and characterized by single-crystal X-ray diffraction, FTIR, elemental analysis, and thermogravimetric analysis. Compound 1 crystallizes in the monoclinic system with space group Cc (no. 9), a=10.205(2) Å, b=14.143(3) Å, c=11.003(2) Å, β=113.97(3)°, V=1451.1(5) Å³, Z=4. The anionic units, [B₅O₆(OH)₄]⁻, are interlinked via hydrogen bonding to form a three-dimensional (3D) supramolecular network containing large channels, in which the protonated [C₆H₁₃N₂]⁺ cations are located. Second-harmonic generation (SHG) measurements on the powder samples reveal that 1 exhibits SHG efficiency approximately 0.9 times that of potassium dihydrogen phosphate (KDP).     

Syntheses, structures, and magnetic and optical properties of the compounds [Hg3Te2][UCl6] and [Hg4As2][UCl6]

Two new quaternary salts, [Hg₃Te₂][UCl₆] and [Hg₄As₂][UCl₆], have been synthesized and their structures determined by single-crystal X-ray diffraction analysis. [Hg₃Te₂][UCl₆] is the product of a reaction involving UCl₄, HgCl₂, and HgTe at 873 K. The compound crystallizes in space group P2₁/c of the monoclinic system. [Hg₄As₂][UCl₆] results from the reaction of U, Hg₂Cl₂, and As at 788 K. It crystallizes in space group Pbca of the orthorhombic system. [Hg₃Te₂][UCl₆] has a two-dimensional framework of layers, whereas [Hg₄As₂][UCl₆] has a three-dimensional framework of layers interconnected by Hg atoms linearly bonded to As atoms. Both framework structures contain discrete [UCl₆]²⁻ anions between the layers. [Hg₃Te₂][UCl₆] exhibits temperature-independent paramagnetism. The optical absorption spectra of these compounds display f-f transitions.     

Synthesis and structure of organically templated lanthanum sulfate [C4N3H16][La(SO4)3]·H2O

The first organically templated one-dimensional lanthanum sulfate [C₄N₃H₁₆][La(SO₄)₃]·H₂O has been prepared employing hydrothermal methods in the presence of diethylenetriamine (DETA). The structure was determined by single-crystal X-ray diffraction (XRD). The title compound crystallizes in the triclinic system, space group P-1 (No.2) with cell parameters M=551.30, a=8.2773(7) Å, b=9.5660(6) Å, c=10.4363(6) Å, α=105.661(2)°, β=102.849(3)°, γ=104.376(3)°, V=732.72(9) Å³, Z=2, R=0.0285, wR=0.0778. The structure consists of infinite linear chains. The chains are held together by hydrogen bond interactions involving the hydrogens of the amine and the framework oxygens. The as-synthesized product is characterized by powder XRD, inductive couple plasma analysis and thermogravimetric analysis.     

Ce10[Si10O9N17]Br, Nd10[Si10O9N17]Br and Nd10[Si10O9N17]Cl oxonitridosilicate halides with a new layered structure type

The isotypic oxonitridosilicate halides Ce₁₀[Si₁₀O₉N₁₇]Br, Nd₁₀[Si₁₀O₉N₁₇]Br and Nd₁₀[Si₁₀O₉N₁₇]Cl were obtained by the reaction of the respective lanthanide metals, their oxides and halides with “Si(NH)₂” in a radiofrequency furnace at temperatures around 1800 °C, using CsBr, resp. CsCl, as a flux. The crystal structures were determined by single-crystal X-ray diffraction (Pbam, no. 55, Z=2; Ce/Br: a=10.6117(9) Å, b=11.2319(10) Å, c=11.688(8) Å, R1=0.0356; Nd/Br: a=10.523(2) Å, b=11.101(2) Å, c=11.546(2) Å, R1=0.0239; Nd/Cl: a=10.534(2) Å, b=11.109(2) Å, c=11.543(2) Å, R1=0.0253) and represent a new layered structure type. The structure refinements were performed utilizing an O/N-distribution model according to Paulings rules, i.e. nitrogen was positioned on all bridging sites and mixed O/N-occupation was assumed on the terminal sites resulting in charge neutrality of the compounds. The layers consist of condensed [SiN₂(O/N)₂] and [SiN₃(O/N)] tetrahedra of Q² and Q³ type. The chemical composition of the compounds was derived from chemical analyses for Nd₁₀[Si₁₀O₉N₁₇]Br and electron probe micro analyses (EPMA) for all three compounds. The results of IR spectroscopic investigations are reported.     

Synthesis and structure of a 1,6-hexyldiamine heptaborate, [H3N(CH2)6NH3][B7O10(OH)3]

A new 1,6-hexyldiamine heptaborate, [H₃N(CH₂)₆NH₃][B₇O₁₀(OH)₃] (1), has been solvothermally synthesized and characterized by single-crystal X-ray diffraction, FTIR, elemental analysis, and thermogravimetric analysis. Compound 1 crystallizes in monoclinic system, space group P2₁/n with a=8.042(2) Å, b=20.004(4) Å, c=10.103(2) Å, and β=90.42(3)°. The anionic [B₇O₁₀(OH)₃]_n²ⁿ⁻ layers are interlinked via hydrogen bonding to form a 3D supramolecular network containing large channels, in which the templated [H₃N(CH₂)₆NH₃]²⁺ cations are located.     

Eu(C10H9N2O4)(C10H8N2O4)(H2O)3]•0.5bipy•3H2O配合物的合成、晶体结构及荧光性质

在水-乙醇混合体系中, 以2-羰基丙酸水杨酰腙(C₁₀H₁₀N₂O₄)、2,2-联吡啶(C₁₀H₈N₂, 简写bipy)与Eu(NO₃)₃•4H₂O反应, 首次培养出黄色单晶[Eu(C₁₀H₉N₂O₄)(C₁₀H₈N₂O₄)(H₂O)₃]•0.5bipy•3H₂O. 该晶体属三斜晶系, 空间群为P-1, 晶胞参数a＝0.93392(16) nm, b＝1.3100(2) nm, c＝1.3895(2) nm, α＝97.205(3)°, β＝105.411(2)°, γ＝106.364(2)°, V＝15.35(2) nm³, Z＝2, μ＝2.118 mm^－1, D_c＝1.686 Mg/m³, F(000)＝786, R＝0.0116, wR＝0.0507, GOF＝0.995. 晶体测试结果表明, 该单晶结构为铕的9配位配合物, 两个2-羰基丙酸水杨酰腙分别以负一价和负二价酮式和三个水分子同时参与配位; 每个2-羰基丙酸水杨酰腙中的羧基氧、酰胺基中的羰基氧和C＝N中的氮与Eu^3＋配位, 形成两个共边的稳定五元环, 另三个配位原子则分别来自三个水分子中的氧原子, 该配合物在空间呈扭曲的单帽四方反棱柱, 而在不对称单位中还有游离的一个2,2-联吡啶分子和三个水分子, 这些游离分子与配位分子之间存在大量分子内和分子间氢键, 整个分子在空间呈三维网状结构. 发光性能测试表明该配合物具有很好的荧光性质.     

Synthesis, vibrational and NMR spectroscopic characterization of [N(CH3)4][IO2F2] and X-ray crystal structure of [N(CH3)4]2[IO2F2][HF2]

The salt, [N(CH₃)₄][IO₂F₂], was prepared from [N(CH₃)₄][IO₃] and 49% aqueous HF, and characterized by Raman, infrared, and ¹⁹F NMR spectroscopy. Crystals of [N(CH₃)₄]₂[IO₂F₂][HF₂] were obtained by reduction of [N(CH₃)₄][cis-IO₂F₄] in the presence of [N(CH₃)₄][F] in CH₃CN solvent and were characterized by Raman spectroscopy and single-crystal X-ray diffraction: C2/m, a = 14.6765(2) Å, b = 8.60490(10) Å, c = 13.9572(2) Å, β = 120.2040(10)°, V = 1523.35(3) Å³, Z = 4 and R = 0.0192 at 210 K. The crystal structure consists of two IO₂⁻F₂ anions that are symmetrically bridged by two H⁻F₂ anions, forming a [F₂O₂I(FHF)₂IO₂F₂]⁴⁻ dimer. The symmetric bridging coordination for the H⁻F₂ anion in this structure represents a new bonding modality for the bifluoride anion.     

Hydrothermal synthesis and crystal structure of a layered vanadium oxide with an interlayer metal coordination complex: [Co(phen)3][V10O26]·H2O

A novel compound, [Co(phen)₃][V₁₀O₂₆]·H₂O, was hydrothermally synthesized and characterized by single-crystal X-ray diffraction. This compound crystallizes in the orthorhombic space group Ccca with a=13.447(3), b=29.936(6), c=23.252(5) Å, V=9360(3) Å³, Z=8 and R=0.0285. Data were collected on a Rigaku R-AXIS RAPID IP diffractometer at 293 K in the range of 1.36<θ<24.99°. The structure of the compound consists of vanadium oxide layers, which are built up from the infinite VO₄ chains by corners and edges sharing. The [Co(phen)₃]²⁺ complexes occupy the interlayer space and contact each other via π−π stacking interactions of the phen groups to form infinite one-dimensional chains.     

Hydrothermal Synthesis and Characterization of (H3N(CH2)4NH3)[V6O14]

A new layered vanadium oxide [H₃N(CH₂)₄NH₃](V₆O₁₄) was synthesized hydrothermally under autogenous pressure at 180°C for 48 h from a mixture of H₂N(CH₂)₄NH₂ and V₂O₅ in aqueous solution. Its structure was determined from single-crystal X-ray diffraction at room temperature with final R=0.0774 and R_w=0.0893. It crystallizes in the monoclinic system (space group P2₁/n with a=9.74(2) Å, b=6.776(5) Å, c=12.60(2) Å, β=96.1(1)°, V=827(2) ų and Z=2). This compound contains mixed-valence V⁵⁺/V⁴⁺ vanadium oxide layers built from [V^VO₄] tetrahedra and pairs of edge-sharing [V^IVO₅] square pyramids with protonated organic amines occupying the interlayer space.     

The new silver(I)thioantimonate(III) [C4N2H14][Ag3Sb3S7] and a new structural variant of the silver(I)thioantimonate(III) [C2N2H9]2[Ag5Sb3S8] both synthesized under solvothermal conditions

The novel silver(I)thioantimonates(III) [C₄N₂H₁₄][Ag₃Sb₃S₇] (I) (C₄N₂H₁₂=1,4-diaminobutane) and [C₂N₂H₉]₂[Ag₅Sb₃S₈] (II) (C₂N₂H₈=ethylenediamine) were synthesized under solvothermal conditions using AgNO₃, Sb, S and the amines as structure directing molecules. Both compounds crystallize as orange needles with lattice parameters a=6.669(1) Å, b=30.440(3) Å, c=9.154(1) Å for I (space group Pnma), and a=6.2712(4) Å, b=15.901(1) Å, c=23.012(2) Å, β=95.37(1)° for II (space group P2₁/n). In both compounds the primary building units are trigonal SbS₃ pyramids, AgS₃ triangles and AgS₄ tetrahedra. In I the layered [Ag₃Sb₃S₇]²⁻ anion is constructed by two different chains. An [Sb₂S₄] chain running along [100] is formed by vertex sharing of SbS₃ pyramids. The second chain contains a Ag₃SbS₅ group composed of the AgS₄ tetrahedron, two AgS₃ units and one SbS₃ pyramid. The Ag₃SbS₅ units are joined via S atoms to form the second chain which is also directed along [100]. The layered anion is then obtained by condensation of the two individual chains. The organic structure director is sandwiched by the inorganic layers and the shortest inter-layer distance is about 6.4 Å. In II the primary building units are linked into different six-membered rings which form a honeycomb-like layer. Two such layers are connected via Ag-S bonds of the AgS₄ tetrahedra giving the final undulated double layer anion. The structure directing ethylenediamine cations are located in pairs between the layers and a sandwich-like arrangement of alternating anionic layers and organic cations is observed. The inter-layer separation is about 5.4 Å. Both compounds decompose in a more or less complex manner when heated in an argon atmosphere. The optical band gaps of about 1.9 eV for the two compounds proof the semiconducting behavior. For II the conductivity was measured with impedance spectroscopy and amounts to σ_295K=7.6×10⁻⁷ Ω⁻¹ cm⁻¹. At 80 °C the conductivity is significantly larger by one order of magnitude.     

Inorganic-Organic Hybrid Materials: Synthesis and X-Ray Structure of N,N′-Dimethylimidazolium Salts [(Me2Im)2][Cd2(SCN)6] and N,N′-Dicyclohexylimidazolium [(Cy2Im)2][Cd2(SCN)6]·C3H6O

Two novel N,N′-dialkylimidazolium thiocyanate-cadmium complexes [(R₂Im)₂][Cd₂(SCN)₆] for R=Me (3), and cyclohexyl (4) have been synthesized and characterized by single-crystal X-ray diffraction. Compound 3 crystallizes in the monoclinic unit cell dimensions of 17.468(3), 7.7273(12), 10.6750(16) Å, 104.833(2)°, and space group C2 with two [(Me₂Im)₂] [Cd₂(SCN)₆] per unit cell. The two cadmium atoms in 3 are octahedrally coordinated in 4N2S and 2N4S coordination environment, and linking into one-dimensional zigzag chains. Compound 4 belongs to the monoclinic space group Cc with unit cell of dimensions 13.3049(12), 17.5550(16), 20.8012(19) Å, 101.494(2)°, and four [(Cy₂Im)₂][Cd₂(SCN)₆]·C₃H₆O per unit cell. The cadmium atoms in 4 are all 3N3S hexa-coordinated with six bridging SCN⁻ ions in an fac configuration and form infinite zigzag polymeric chains. The infinite chains in 3 form an approximate hexagonal array, making triangular channels which are occupied by N,N′-dimethylimidazolium ions, whereas the chains in 4 form layered structure, and the layers are stacked perpendicularly with respect to the orientation of the infinite anionic chains alternatively. N,N′-dicyclohexylimidazolium cations and solvent molecules fill in between layers.     

Syntheses, crystal structures and spectroscopic properties of Ag2Nb[P2S6][S2] and KAg2[PS4]

Ag₂Nb[P₂S₆][S₂] (1) was obtained from the direct solid state reaction of Ag, Nb, P₂S₅ and S at 500 °C. KAg₂[PS₄] (2) was prepared from the reaction of K₂S₃, Ag, Nd, P₂S₅ and extra S powder at 700 °C. Compound 1 crystallizes in the orthorhombic space group Pnma with a=12.2188(11), b=26.3725(16), c=6.7517(4) Å, V=2175.7(3) Å³, Z=8. Compound 2 crystallizes in the non-centrosymmetric tetragonal space group with lattice parameters a=6.6471(7), c=8.1693(11) Å, V=360.95(7) Å³, Z=2. The structure of Ag₂Nb[P₂S₆][S₂] (1) consists of [Nb₂S₁₂], [P₂S₆] and new found puckered [Ag₂S₄] chains which are along [001] direction. The Nb atoms are located at the center of distorted bicapped trigonal prisms. Two prisms share square face of two [S₂²⁻] to form one [Nb₂S₁₂] unit, in which Nb-Nb bond is formed. The [Nb₂S₁₂] units share all S²⁻ corners with ethane-like [P₂S₆] units to form 14-membered rings. The novel puckered [Ag₂S₄] chains are composed of distorted [AgS₄] tetrahedra and [AgS₃] triangles that share corners with each other. These chains are connected with [P₂S₆] units and [Nb₂S₁₂] units to form three-dimensional frame work. The structural skeleton of 2 is built up from [AgS₄] and [PS₄] tetrahedra linked by corner-sharing. The three-dimensional anionic framework contains orthogonal, intersecting tunnels directed along [100] and [010]. This compound possesses a compressed chalcopyrite-like structure. The structure is compressed along [001] and results from eight coordination sphere for K⁺. Both compounds are characterized with UV/vis diffuse reflectance spectroscopy and compound 1 with IR and Raman spectra.     

An organosilyl derivative of trivacant tungstophosphate. Synthesis, characterization and crystal structure determination of α-A-[NBu4]3[PW9O34(C2H5SiO)3(C2H5Si)]

In the presence of NBu₄ⁿBr acting as phase-transfer reagent, organosilicon trichloride C₂H₅SiCl₃ reacts in acetonitrile with the trivacant tungstophosphate sodium salt β-A-Na₈H[PW₉O₃₄]·24H₂O to give hybrid organosilyl polyoxotungstate derivative α-A-[NBu₄ⁿ]₃[PW₉O₃₄(C₂H₅SiO)₃(C₂H₅Si)]. X-ray single crystal structural analysis indicates that the title compound is monoclinic, space group Cc, with lattice constants a=26.828(5), b=22.459(5), c=17.517(4) Å, β=103.19(3)°, V=10,276(4) Å³, Z=4, R=0.0462. According to the result of X-ray single crystal diffraction and chemical analysis, the hybrid polyanion consists of one α-A-[PW₉O₃₄]⁹⁻ framework on which are grafted simultaneously three RSiO groups through six Si-O-W bridge bonds, each of which is attached to the fourth RSi group through three Si-O-Si bridge bonds. The hybrid polyanion becomes a partial saturated, closed cage structure and also has an assembly of virtual C_3V symmetry.     

The crystal structure of the monohydrate R2Mo6O21·H2O (R=Pr, Nd, Sm, and Eu): a layer structure containing disordered [Mo2O7] groups

Although R₂O₃:MoO₃=1:6 (R=rare earth) compounds are known in the R₂O₃-MoO₃ phase diagrams since a long time, no structural characterization has been achieved because a conventional solid-state reaction yields powder samples. We obtained single crystals of R₂Mo₆O₂₁·H₂O (R=Pr, Nd, Sm, and Eu) by thermal decomposition of [R₂(H₂O)₁₂Mo₈O₂₇]·nH₂O at around 685-715 °C for 2 h, and determined their crystal structures. The simulated XRD patterns of R₂Mo₆O₂₁·H₂O were consistent with those of previously reported R₂O₃:MoO₃=1:6 compounds. All R₂Mo₆O₂₁·H₂O compounds crystallize isostructurally in tetragonal, P4/ncc (No. 130), a=8.9962(5), 8.9689(6), 8.9207(4), and 8.875(2) Å; c=26.521(2), 26.519(2), 26.304(2), and 26.15(1) Å; Z=4; R₁=0.026, 0.024, 0.024, and 0.021, for R=Pr, Nd, Sm, and Eu, respectively. The crystal structure of R₂Mo₆O₂₁·H₂O consists of two [Mo₂O₇]²⁻-containing layers (A and B layers) and two interstitial R(1)³⁺ and R(2)³⁺ cations. Each [Mo₂O₇]²⁻ group is composed of two corner-sharing [MoO₄] tetrahedra. The [Mo₂O₇]²⁻ in the B layer exhibits a disorder to form a pseudo-[Mo₄O₉] group, in which four Mo and four O sites are half occupied. R(1)³⁺ achieves 8-fold coordination by O²⁻ to form a [R(1)O₈] square antiprism, while R(2)³⁺ achieves 9-fold coordination by O²⁻ and H₂O to form a [R(2)(H₂O)O₈] monocapped square antiprism. The disorder of the [Mo₂O₇]²⁻ group in the B layer induces a large displacement of the O atoms in another [Mo₂O₇]²⁻ group (in the A layer) and in the [R(1)O₈] and [R(2)(H₂O)O₈] polyhedra. A remarkable broadening of the photoluminescence spectrum of Eu₂Mo₆O₂₁·H₂O supported the large displacement of O ligands coordinating Eu(1) and Eu(2).     

Preparation,crystal and molecular structure of,and NMR parameters for,the exopolyhedral heterocyclic platinaundecaborane [μ-2,7-(SCSNEt2)-7-(PMe2Ph)-NIDO-7-PtB10H11]

The compound [μ-2,7-(SCSNEt₂)-7-(PMe₂Ph)-nido-7-PtB₁₀H₁₁] has been obtained in a yield of 52% from the reaction of [7,7-(PMe₂Ph)-nido-7-PtB₁₀H₁₂] and [AuBr₂(S₂CNEt₂)], and identified by single crystal X-ray diffraction analysis and multi-element single and double resonance NMR spectroscopy. The yellow-orange compound crystallizes in the monoclinic space group P2₁/n with a 1179.2(2), b = 1244.9(5), c = 1641.4(2) pm, β = 95.45(1)°, Z = 4, and the structure (R 0.0209, R_w = 0.0211 for 3719 observed reflections) is that of a nido-7-platinaundecaborane with an exopolyhedral N,N-diethyldithiocarbamate ligand bridging the Pt(7) and B(2) positions to give a $\text{-Pt-B-C-S-}$ five-membered ring. The tetrahapto platinum-to-borane bonding has a considerable twist distortion relative to other nido-7-platinaundecaboranes which do not possess this cyclic feature. The NMR parameters exhibit no anomalies and are consistent with the crystal molecular structure. A plot of δ(¹¹B) vs δ(¹H) for directly bound exo-terminal hydrogen atoms shows good correlation with the slope 16 : 1.     

Synthesis and Structural Characterization of a Layered Tin(II) Phosphate, [Sn2(PO4)2][C2N2H10]·H2O

A new layered tin(II) phosphate [Sn₂(PO₄)₂]²⁻[C₂N₂H₁₀]²⁺·H₂O was synthesized by hydrothermal technique. It crystallizes in monoclinic space groupP2₁/c(No. 14) with lattice parametersa=9.4112(1) Å;b=8.5998(1) Å;c=15.9921(2) Å;β=100.009(1)°;V=1274.61(2);Z=4;R=2.06%;R_w=2.17%. The structure consists of inorganic layers, comprising a network of strictly alternating SnO₃and PO₄moieties and held together by strong hydrogen bonding between the layers. Protonated ethylenediamine and water molecules are trapped between the layers.