Crystal Structure of [Zn(2-Bromobenzoato)<Subscript>2</Subscript>]<Subscript><Emphasis Type="Italic">n</Emphasis></Subscript> and [Zn(2-Bromobenzoato)<Subscript>2</Subscript>(<Emphasis Type="Italic">N</Emphasis>-Methylnicotinamide)]<Subscript>2</Subscript>

Abstract  

The syntheses and structural characterizations of two novel 2-bromobenzoatozinc(II) complexes—[Zn(2-BrC₆H₄COO)₂] _n (I) and [Zn(2-BrC₆H₄COO)₂(mnad)]₂ (II), where mnad is N-methylnicotinamide are reported. Compound (I) crystallized with a monoclinic lattice (space group P2₁/c) and is polymeric in solid state. Its cell parameters are: a = 7.37220(10) Å, b = 19.9639(3) Å, c = 30.2756(5) Å, β = 94.7510(7)°, V = 4440.59(12) ų, Z = 4. The coordination environments of all zinc atoms are distorted tetrahedra built from four carboxylate oxygen atoms coming from four 2-bromobenzoato ligands. Compound (II) crystallized with a monoclinic lattice (space group P2₁/c) with a = 11.7488(2) Å, b = 20.3683(3) Å, c = 9.30130(10) Å, β = 100.3941(11)°, V = 2189.30(5) ų, Z = 2. This dimeric molecule features a paddle-wheel [Zn₂O₈] cage in solid state; the coordination environment of the central atom is square pyramidal consisting of four carboxylate oxygen atoms and the pyridine N atom of the mnad ligand.     

Synthesis and Structure of [Fe<Subscript>3</Subscript>O(O<Subscript>2</Subscript>CCH<Subscript>2</Subscript>OMe)<Subscript>6</Subscript>(H<Subscript>2</Subscript>O)<Subscript>3</Subscript>][FeCl<Subscript>4</Subscript>]

Abstract  The structure of [Fe₃O(O₂CCH₂OMe)₆(H₂O)₃][FeCl₄] · 2.5H₂O has been determined. The three iron atoms and the μ₃-oxo are coplanar. Each carboxylic ligand is bidentate and links two iron atoms in the cluster. The clusters are linked by intra-trimer hydrogen bonding to form a zigzag motif that forms sheets via hydrogen bonding involving disordered waters of hydration. The [FeCl₄]⁻ anion is intercalated between the hydrogen-bonded sheets. Crystal data: space group P2₁/n, a = 10.276(2), b = 22.793(5), c = 17.091(3) ?, β = 96.66(3)°, V = 3976(1) ?³, Z = 4, R = 0.0837, wR ₂ = 0.1836. Graphical Abstract  The structure of [Fe₃O(O₂CCH₂OMe)₆(H₂O)₃][FeCl₄] · 2.5H₂O has been determined in which the clusters are linked by intra-trimer hydrogen bonding to form a zigzag motif that forms sheets via hydrogen bonding involving disordered waters of hydration.      

<Emphasis Type="Italic">Trans-</Emphasis>dichlorodioxobis(triphenylphosphate)molybdenum(VI), MoO<Subscript>2</Subscript>Cl<Subscript>2</Subscript>[OP(OPh)<Subscript>3</Subscript>]<Subscript>2</Subscript>

Abstract  The molecular structure of trans-dichlorodioxobis(triphenylphosphate) molybdenum(VI), MoO₂Cl₂[OP(OPh)₃]₂ has been determined. Crystal data: Monoclinic, Pn, a = 11.767(2), b = 10.341(2), c = 15.682(3) ?, β = 92.27(3)°, V = 1906.8(7) ?⁻³, Z = 2. Trans-dichlorodioxobis(triphenylphosphate)molybdenum(VI) was obtained by the reaction of molybdenum oxide, HCl and triphenylphosphate and was characterized by elemental analysis, IR, and ¹H-NMR spectroscopy. Index Abstract   Trans-dichlorodioxobis(triphenylphosphate)molybdenum(VI), MoO₂Cl₂[OP(OPh)₃]₂ V. Huch¹, R. Kumar², S. Mathur¹, R. Ratnani² The immediate environment around Mo is distorted octahedral with two cis-oxygen atoms and two trans-chlorine atoms along with two triphenylphosphate moieties.      

Reaction of (<Emphasis Type="Italic">n</Emphasis>-Bu<Subscript>4</Subscript>N)<Subscript>2</Subscript>[Re<Subscript>2</Subscript>Cl<Subscript>8</Subscript>] with a 2-Oxocarboxylic Acid: Crystallographic Characterization of a New Dirhenate(III) Complex

Abstract  

The reaction of tetra-n-butylammonium-octachloridodirhenate(III), (Bu₄N)₂[Re₂Cl₈], with molten 2-oxobutanoic acid Et(CO)CO₂H at 75 °C afforded pale-green tetra-n-butylammonium-hexachlorido-(2-oxobutanoato)-dirhenate(III), (Bu₄N)[Re₂(O₂C(CO)Et)Cl₆]. Slow evaporation of a solution in CHCl₃ yielded shiny, mint-green crystals of the dirhenate complex. The X-ray crystal structure determination (monoclinic, P2₁/n, a = 11.6557(3) ?, b = 20.5382(5) ?, c = 13.9281(3) ?, β = 112.508(1)°, Z = 4) revealed the presence of [Re₂(O₂C(CO)Et)Cl₆]⁻ anions and tetra-n-butylammonium cations. The central [Re₂]⁶⁺ core with a Re≣Re quadruple bond of 2.2263(3) ? length is μ₂-bridged by one 2-oxobutanoato ligand and additionally coordinated by six chlorido ligands. Each dirhenate unit is linked via two Re···Cl contacts to dimeric, centrosymmetric entities of the constitution {[Re₂(O₂C(CO)Et)Cl₆]₂}²⁻. In the crystal, these dimers of dinuclear complexes are separated from each other by the bulky tetra-n-butylammonium cations.     

Synthesis and Structure of Ba<Subscript>5</Subscript>(V<Subscript>2</Subscript>O<Subscript>7</Subscript>)<Subscript>2</Subscript>Cl<Subscript>2</Subscript>

Abstract  A new barium chlorovanadate, Ba₅(V₂O₇)₂Cl₂, was isolated by a high-temperature (850 °C) reaction employing a CsCl/RbCl flux. The structure was determined by single crystal X-ray diffraction methods. This compound crystallizes in an orthorhombic crystal system, Pmmn (No. 59), with a = 11.558(2) ?, b = 15.164(3) ?, c = 10.023(2) ?, Z = 4 and V = 1756.7(6) ?³. The structure of Ba₅(V₂O₇)₂Cl₂ was determined by full-matrix, least-squares methods with R ₁ = 0.0398, wR ₂ = 0.1069 and GOF = 1.048 for all data. This new structure can be described as a composite lattice made up of mixed covalent and ionic moities. The extended framework is orchestrated by stacked [Ba(V₂O₇)Cl]³⁻ slabs that are interconnected by Ba²⁺ cations through Ba–O bonds to the [V₂O₇] units. The Ba²⁺ and Cl^- ions form BN-type “[BaCl]” sheets with pseudo-hexagonal windows that are centered by [V₂O₇]⁴⁻ pyrovanadate units. Graphical Abstract  The structure of a new chlorovanadate, Ba₅(V₂O₇)₂Cl₂, exhibits an interesting BN-type salt lattice that consists of an extended [BaCl] sheet containing pseudo-hexagonal windows that are centered by [V₂O₇] pyrovanadate units.      

Synthesis and Crystal Structures of Octahedral Sn(IV) Complexes Prepared from SnCl<Subscript>2</Subscript>·2H<Subscript>2</Subscript>O and 2-Hydroxyacetophenone (<Emphasis Type="Italic">S</Emphasis>-benzydithiocarbazate) Ligand (H<Subscript>2</Subscript>L)

Abstract  

Two coordination octahedral Sn(IV) complexes [Sn(L)₂] and cis-[SnCl₂(L)(dmso)], where H₂L is 2-hydroxyacetophenone (S-benzydithiocarbazate), were prepared and characterized by elemental analysis, IR, NMR (¹H, ¹³C), ¹¹⁹Sn M?ssbauer spectroscopies and X-ray diffraction techniques to investigate their structural properties. Both crystallize in the Monoclinic system, with parameters: a = 8.1905(3), b = 30.8811(15), c = 12.8959(7) ?, β = 94.465(3)° and Z = 4 for [Sn(L)₂] and a = 8.5247(2), b = 21.5445(7), c = 12.3706(3) ?, β = 96.932(2)° and Z = 4 for cis-[SnCl₂(L)(dmso)]. In both complexes, the Sn(IV) central atom is coordinated in a distorted octahedral geometry with the thiolate ligand (L²⁻) coordinated via O, N and S atoms. The ¹¹⁹Sn M?ssbauer spectroscopy of the complexes were studied and the results revealed that both complexes posses isomer shift (δ) and quadrupole splitting (Δ), which are almost the same.     

Hydrothermal Synthesis and Structure of Fe<Subscript>6.36</Subscript>Mn<Subscript>0.64</Subscript>(PO<Subscript>3</Subscript>(OH))<Subscript>4</Subscript>(PO<Subscript>4</Subscript>)<Subscript>2</Subscript>

Abstract  

Single crystals of iron and manganese phosphate Fe_6.36Mn_0.64(PO₃(OH))₄(PO₄)₂ was synthesized by hydrothermal method. The compound crystallizes in the Fe₇(PO₄)₆ structure type and is isotypic with the solid solution \textM_{7 - \textx} \textM_\textx^￠ ( \textHPO₄ )₄ ( \textPO₄ )₂ {\text{M}}_{{7 - {\text{x}}}} {\text{M}}_{\text{x}}^{\prime} \left( {{\text{HPO}}_{4} } \right)_{4} \left( {{\text{PO}}_{4} } \right)_{2} where M is Fe, Co, Mg, Mn. The compound is triclinic, P-1, a = 6.571(5), b = 7.993(3), c = 9.547(2) Ǻ, α = 103.97(1)°, β = 109.29(2)°, γ = 101.57(3)°. The structure is based on a three-dimensional framework of distorted edge-sharing MO₆ and MO₅ polyhedra, forming infinite chains, which are interlinked by corner-sharing with PO₄ tetrahedra. The formula unit is centrosymmetric, with all atoms in general positions except for one Fe atom, which has site symmetry −1.     

Synthesis,Spectrum Properties,and Crystal Structure of a New Pentaborate,Na<Subscript>2.18</Subscript>K<Subscript>0.82</Subscript>SrB<Subscript>5</Subscript>O<Subscript>10</Subscript>

Abstract  

A novel quaternary borate, Na_2.18K_0.82SrB₅O₁₀, has been prepared by high-temperature solution reaction below 800 °C. Single-crystal XRD analyses showed that it crystallizes in the triclinic P[`1] P\bar{1} group with a = 7.3900(15) ?, b = 7.6490(15) ?, c = 9.773(2) ?, α = 79.31(2)°, β = 70.85(2)°, γ = 62.09(1)°, Z = 2. The basic structural unit in Na_2.18K_0.82SrB₅O₁₀ is a double ring [B₅O₁₀]⁵⁻ composed of one BO₄ tetrahedron and four BO₃ triangles. The [B₅O₁₀]⁵⁻ groups are arranged around crystallographic centers of symmetry to form [B₁₀O₂₀]¹⁰⁻ columns that are held together by Na⁺, K⁺/Na⁺, and Sr²⁺ cations via electrostatic interactions. The IR spectrum further confirmed the presence of both BO₃ and BO₄ groups. UV–vis diffuse reflectance spectrum showed a band gap of about 3.80 eV. Solid-state fluorescence spectrum exhibited the maximum emission peak at around 337.6 nm.     

Co-crystal Structure of 11-Hydroxy-2,3,9-trimethoxy-6<Emphasis Type="Italic">H</Emphasis>-chromeno[3,4-<Emphasis Type="Italic">b</Emphasis>]chromen-12-one and 11-Hydroxy-2,3,9-trimethoxy-chromeno[3,4-<Emphasis Type="Italic">b</Emphasis>]chromene-6,12-dione

Abstract  

A 1:1 co-crystal structure of 11-hydroxy-2,3,9-trimethoxy-6H-chromeno[3,4-b]chromen-12-one and 11-hydroxy-2,3,9-trimethoxy-chromeno[3,4-b]chromene-6,12-dione (stemonone) was crystallized from the reaction mixture of 6-deoxyclitoriacetal and methanesulfonyl chloride, and its structure was characterized by X-ray diffraction. This co-crystal crystallizes in a triclinic crystal system, space group P(−1) with unit cell parameters of a = 8.1317(3) Å, b = 9.8224(4) Å, c = 10.7268(3) Å, α = 78.116(1)°, β = 77.463(1)°, γ = 77.140(1)°, Z = 2 and V = 804.11(3) Å³. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F ² to final values of R ₁ = 0.0501 and wR ₂ = 0.1520.     

[KCl<Subscript>3</Subscript>{H<Subscript>2</Subscript>dabco}]: A Unique 3-D Charge-Assisted Hydrogen-Bonded Hybrid Network of Anionic KCl<Subscript>3</Subscript> Chains and Organic Cations

Abstract  The 3-D hybrid network [KCl₃{H₂dabco}] resulted from the assemblage of KCl and [{H₂dabco}Cl₂] (1,4-diazabicyclo[2.2.2]octane) in H₂O. The compound crystallizes in the trigonal space group R-3c with a = b = 16.0437(2) Å, and c = 22.3094(2) Å. The structure consists in polymeric chains of anionic {KCl₃}²⁻ linked to {H₂dabco}²⁺ units by hydrogen bonds. Each organic cation establishes such charge-assisted H···Cl interactions with two inorganic arrays leading to a 3-D network. Index Abstract  Assemblage of KCl and [{H₂dabco}Cl₂] (1,4-diazabicyclo[2.2.2]octane) in H₂O resulted in a 3-D hybrid network of inorganic {KCl₃}²⁻ chains H-bonded to bridging organic cations.      

The synthesis and structure of a novel alternating 1-D cobalt coordination polymer [Co(2,5-PDC)<Subscript>2</Subscript>(H<Subscript>2</Subscript>O)<Subscript>2</Subscript>Co(H<Subscript>2</Subscript>O)<Subscript>4</Subscript>]·4H<Subscript>2</Subscript>O

A novel cobalt complex [Co(2,5-PDC)₂(H₂O)₂Co(H₂O)₄]·4H₂O (2,5-PDCH₂ = 2,5-pyridinedicarboxylic acid) was synthesized and its crystal structure has been determined by X-ray diffraction. The crystallographic data are: triclinic P−1, a = 7.112(2) ?, b = 8.939(3) ?, c = 9.719(3) ?, α = 91.153(5)°, β = 101.136(5)°, γ = 108.001(4)°, V = 574.4(3) ?³, Z = 1. The compound [Co(2,5-PDC)₂(H₂O)₂Co(H₂O)₄]·4H₂O exhibits a novel one-dimensional network constructed from the interconnection of Co(2,5-PDC)₂(H₂O)₂ and Co(H₂O)₄, in which two kinds of six-coordinated Co(II) atoms have both octahedral coordination environments. Each 2,5-PDC anion connects two different coordinated cobalt ions alternately in an one-dimensional chain. The zigzag 1D alternating chains are linked by extensive hydrogen bonds to form a three-dimensional (3D) supramolecular structure, in which uncoordinated solvate molecules act as space filling particles. Supplementary data CCDC-264249 contains the supplementary crystallographic data for this paper. Copies of this information may be obtained free of charge from the Director, CCDC, 12 Union Road, Cambridge, CB2 1EZ, UK (fax: t44–1223–336033; e-mail: deposit@ccdc.cam.ac.uk or ) or also available from the author Xiaoqing Wang.     

Synthesis and crystal structure of anhydrous copper suberate: [Cu<Subscript>2</Subscript>(OOC-(CH<Subscript>2</Subscript>)<Subscript>6</Subscript> -COO)<Subscript>2</Subscript>]

The title compound [Cu₂(OOC-(CH₂)₆-COO)₂] was synthesized and its crystal structure has been determined by single crystal X-ray diffraction methods. The complex crystallizes in the triclinic space group P-1 with a=5.1077(5) ?, b=8.362(2) ?, c=11.378(2) ?, α=93.773(6)°, β=97.587(9)°, γ=90.493(’9)° and D _cal=1.629 mg/m³ for Z=1.  The structure is polymeric and consists of discrete anhydrous centrosymmetric binuclear units [Cu₂(OOC-(CH₂)₆-COO)₂]. The two copper(II) centres bridged by the suberate groups in a syn-syn conformation, are in pentacoordinated distorted square-pyramidal coordination environment, with an intramolecular Cu–Cu distance of 2.5793(10) ?. Each binuclear unit, related to the next through μ_oxo bridges with a Cuμ_oxo–Cuμ_oxo separation of 3.2326(10)?, defines infinite chains of one-edge sharing CuO₅ square pyramid.     

Synthesis and Crystal Structure of a Polymorph of the DMF Solvate of the Dicoppertetracarboxylate Paddlewheel Complex Cu<Subscript>2</Subscript>(p-aminobenzoate)<Subscript>4</Subscript>(DMF)<Subscript>2</Subscript>

Abstract  Reaction between p-aminobenzoic acid (HpABA) and Cu(NO₃)₂ · 2.5H₂O in basic MeOH/DMF affords green crystals of the dicopper paddlewheel complex, Cu₂(pABA)₄(DMF)₂ · 2DMF, 1, identified by single crystal X-ray crystallography: triclinic P-1, with a = 10.3728(2) ?, b = 10.617(2) ?, c = 11.128(2) ?, α = 81.705(3)°, β = 79.984(2)°, γ = 65.965(2)° and Z = 2. The crystal structure of 1 reveals that it is the second polymorph of Cu₂(pABA)₄(DMF)₂ · 2DMF and experiments on the stability of 1 indicate that it can be converted to Form I through desolvation followed by exposure to DMF. Graphical Abstract  Crystal structure of a polymorphic discrete dicoppertetracarboxylate is investigated for the conversion between the two forms influenced by hydrogen bonds.      

Crystal Structure and Physical Characterisation of [Zn<Subscript>2</Subscript>(Benzoato)<Subscript>4</Subscript>(Caffeine)<Subscript>2</Subscript>]·2 Caffeine

Abstract  

The crystal structure of [Zn₂(benzoato)₄(caffeine)₂]·(caffeine)₂ was determined by direct method and Fourier technique. The structure was refined by full-matrix least-squares method to a weighted R factor of 0.0582. The structure consists of centrosymmetric dimeric units where the two zinc(II) atoms are coordinated by four bridging benzoates in a syn–syn arrangement and two caffeine ligands at the apices of a bicapped square prism. Remaining two caffeines are bound only by hydrogen bonds. The Zn–Zn distance is 2.961(1) ?. The Zn(II) atoms are displaced by 0.365 ? from the basal plane containing four oxygen atoms towards the apical caffeine molecules. The dimeric structure of the complex is consistent with spectrum and thermal data. The structural data are compared with those found in similar [Zn₂(RCOO)₄(NL)₂] complexes.     

Synthesis,Crystal Structure and Luminescence Property of a Chiral Magnesium (II) Mixed-ligand Complex [Mg(H<Subscript>2</Subscript>O)<Subscript>2</Subscript>(phen)(HBDC)<Subscript>2</Subscript>](phen)

Abstract  

A new mixed-ligand complex of [Mg(H₂O)₂(phen)(HBDC)₂](phen) (phen = 1, 10-phenanthroline, H₂BDC = 1,3-benzene dicarboxylic acid) has been synthesized and its crystal structure determined by single-crystal X-ray diffraction. It is noteworthy that this complex was formed from achiral reactants, and found to crystallize in the chiral space group C2. Structure analysis shows that each Mg(II) ion is coordinated by the two nitrogen atoms of phen, one oxygen atom from each of the two 1,3-HBDC molecules and one oxygen atom from each of the two water molecules, leading to a distorted octahedral geometry. The mixed-ligand complexes are assembled into a two-dimensional supramolecular network through the formation of intermolecular hydrogen bonds. The luminescence property and thermal stability behavior of the complex were also investigated. The complex shows a strong blue luminescence emission. Crystal data: a = 24.5856(16), b = 10.1598(6), c = 7.1460(4) ?, β = 105.226(2)o, V = 1722.30(18)?³, Z = 2, R ₁ = 0.0367, wR ₂ = 0.0833 [I>2σ(I)].     

Expanded Prussian Blue Analogue Based on Octahedral {Nb<Subscript>6</Subscript>} Clusters and {K<Subscript>2</Subscript>} Dimers as Nodes

Abstract  The preparation, structures, and characterization of two new compounds containing octahedral niobium cyanochloride clusters as building units and (Et₄N)⁺ as cation are reported. The reaction between Nb₆Cl₁₄ · 8H₂O, KCN and (Et₄N)Cl led to the formation of (Et₄N)₄[Nb₆Cl₁₂(CN)₆] · 2.67H₂O (1) which crystallizes in triclinic P-1 space group (No. 2) with a = 12.552(2), b = 12.818(2), c = 12.919(2) ?, α = 105.157(3)°, β = 104.188(3)°, γ = 117.390(2)°, V = 1611.7(5) ?³ and Z = 1. 1 has a 2D hydrogen-bonded layer structure based on [Nb₆Cl₁₂(CN)₆]⁴⁻ units connected through hydrogen bonding between cyanide ligands and solvent water molecules. In the presence of large excess of K⁺ ions, similar reaction leads to formation of K₂(Et₄N)₂[Nb₆Cl₁₂(CN)₆] (2) which crystallizes in the tetragonal I4/m space group (No. 87) with a = b = 10.9597(3), c = 19.178(1) ?, V = 2303.6(2) ?³ and Z = 2. Its 3D structure is based on [Nb₆Cl₁₂]²⁺ and [K₂]²⁺ nodes bridged by cyanide ligands to form an expanded Prussian blue type framework with (Et₄N)⁺ acting as charge compensating ions. Index Abstract  An expanded Prussian blue type 3D framework based on hexanuclear {Nb₆} and dinuclear {K₂} units which are bridged by cyanide linker was synthesized and characterized. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Structural Studies of [Ru(1,8-naphthyridine)<Subscript>4</Subscript>]<Superscript>2+</Superscript> and [Ru(1,5-cyclooctadiene)(1,8-naphthyridine)<Subscript>2</Subscript>]<Superscript>2+</Superscript> as their Tetraphenylborate Salts

Abstract  

The previously reported [Ru(naph)₄]²⁺ complex (naph = 1,8-naphthyridine) has been prepared by a simplified route using [RuCl₂(1,5-COD)] _x (COD = cyclooctadiene) as starting material and isolated as its tetraphenylborate salt. The salt crystallizes in the monoclinic space group P2₁/n with a = 13.6531(3) ?, b = 12.5389(4) ?, c = 20.0349(5) ?, β = 96.5884(15)o, V = 3407.22(16) ?, D _calc = 1.300 at 150(1) K. The dication has crystallographically imposed inversion symmetry. Although the iron analogue has been found to have a coordination number of eight, the ruthenium complex is only six-coordinate, which is achieved by the presence of two monodentate and two bidentate 1,8-naphthyridine ligands. The observation of a higher coordination number for Fe(II) vs. Ru(II) can be explained by the high spin nature of the iron complex. A byproduct complex, [Ru(1,5-COD)(naph)₂][B(C₆H₅)₄]₂, could also be synthesized, isolated pure, and structurally characterized. The organometallic complex possesses an 18 electron configuration by virtue of the dicationic metal center being coordinated by the diene ligand and all four nitrogen lone pairs. This salt crystallizes in the triclinic space group \textP[`1] {\text{P}}\bar{1} with a = 12.9538(3) ?, b = 14.9485(3) ?, c = 17.4291(3) ?, α = 69.0649(11)o, β = 78.3211(9)o, γ = 78.5629(10)o, V = 3057.50(11) ?³, D _calc = 1.293 at 150(1) K.     

Convenient Route to Alkylene Dithiophosphato Ligands: Synthesis and Crystallographic Analysis of [OCH<Subscript>2</Subscript>CMe<Subscript>2</Subscript>CH<Subscript>2</Subscript>OPS<Subscript>2</Subscript>HNEt<Subscript>3</Subscript>]

Abstract  

Triethylammonium salts of O,O′-alkylene dithiophosphato like OGOPS₂HNEt₃, [where, G = –CH₂CMe₂CH₂–(1), –CH₂CEt₂CH₂–(2), –CMe₂CH₂CHMe–(3) and –CMe₂CMe₂–(4)] have been synthesized in quantitative yield by the direct reaction of P₂S₅ with 1,2- and 1,3-substituted glycols in presence of triethylamine, Et₃N, in 1:2:2 molar stoichiometry in toluene. These have been mainly characterized by molecular weight, IR and NMR (¹H, ¹³C and ³¹P) spectroscopic studies. Single crystal X-ray structure analysis of [OCH₂CMe₂CH₂OPS₂HNEt₃] reveals that phosphorus atom is tetrahedrally bonded to two sulfur atoms and two oxygen atoms in the ring and the molecule exists as discrete cation and anion. The structure is stabilized by cation–anion N–H···S hydrogen bonded interactions. Antiparallel pattern of triethylammonium ion is sandwiched within the two-dimensional layers of the ring system.     

Structure of Triammonium <Emphasis Type="Italic">fac</Emphasis>-Trichloridotrioxidorhenate(VII) Chloride with <Emphasis Type="Italic">C</Emphasis><Subscript>3<Emphasis Type="Italic">v</Emphasis></Subscript> Crystallographic Symmetry of the Complex Anion

Abstract  

The unstable crystals of triammonium fac-trichloridotrioxidorhenate(VII) chloride have been obtained from ammonium rhenate(VII) solution in concentrated hydrochloric acid. The crystal structure consists of fac-trichloridotrioxidorhenate(VII) anions, chloride anions and ammonium cations. Each fac-trichloridotrioxidorhenate(VII) anion and each chloride anion lies in special position of 3m site symmetry (cell parameters: a = 9.026(3) Å; c = 7.690(4) Å; space group: P6₃ mc). The ammonium cation lies in special position of m site symmetry. The following anion geometrical parameters of the fac-trichloridotrioxidorhenate(VII) anion have been obtained: Re–O bond length of 1.720(2) Å, Re–Cl bond length of 2.5428(9) Å, the bond angles: O–Re–O of 103.5(1)° and Cl–Re–Cl of 79.8(1)°.     

Synthesis,Characterization, and Structure of a Cyano-bridged Two-dimensional Cu<Superscript>II</Superscript>Co<Superscript>III</Superscript> Coordination Polymer Derived from <Emphasis Type="Italic">Trans</Emphasis>-1,2-diaminocyclohexane as Blocking Ligand

Abstract  The synthesis, characterization, and structure of a cyano-bridged two-dimensional supramolecule, [Cu^II(trans-chxn)₂]₃[Co^III(CN)₆]₂·2H₂O (1; chxn = 1,2-diaminocyclohexane), have been described. The title compound crystallizes in the triclinic Pī space group with the unit cell parameters: a = 9.141(5) ?, b = 12.406(5) ?, c = 15.064(5) ?, α = 95.190(5)°, β = 94.460(5)°, γ = 109.510(5)°, V = 1593.0(12) ?³, and Z = 1. The compound contains two crystallographically different copper(II) and cobalt(III) centers. Each of the two copper(II) ions is hexacoordinated by two diamines and two bridging cyanides. Two trans cyanides of one type of hexacyanometalate link one type of copper(II) center to result in one-dimensional chain, while two pairs of trans cyanides of the second type of hexacyanometalate link both the types of copper(II) ions to result in the second dimension. There are extensive hydrogen bonding interactions within the two-dimensional cyano-bridged sheet involving the solvated water molecule, amine groups, and cyanide nitrogens. Index Abstract  Synthesis, characterization, and structure of a cyano-bridged two-dimensional Cu^IICo^III coordination polymer derived from trans-1,2-diaminocyclohexane as blocking ligand Malabika Nayak, Samit Majumder, Pascale Lemoine, and Sasankasekhar Mohanta* The synthesis, characterization, and structure of a cyano-bridged two-dimensional supramolecule, [Cu^II(trans-chxn)₂]₃[Co^III(CN)₆]₂ · 2H₂O (chxn = 1,2-diaminocyclohexane), have been described.