Crystal structure of [WI2(CO)3{P(OMe)3}2]

[WI₂(CO)₃{P(OMe)₃}₂]crystallizes in the orthorhombic space group Pca2₁, with a = 26.924(5), b = 10.726(2), c = 14.136(3) Å, and Z = 8. There are two molecules in the asymmetric unit, the metal atoms in each case being seven-coordinate with a capped fac-(CO)₃ octahedral geometry. The molecular dimensions in the two molecules are nearly identical. The W–P distance to the capping atom 2.397 Å (average) is significantly shorter than the other W–P distance, 2.525 Å (average).     

Structure of a binuclear silver(I) complex [Ph3PAg(O2CCH2Ph)]2

The reaction of [Ph₃PAgI]₄ with sodium phenylacetate in MeOH and CH₂Cl₂ at room temperature gave rise to a binuclear silver complex with triphenylphosphine and phenylacetate mixed ligands, [Ph₃PAg(O₂CCH₂Ph)]₂. The crystal and molecular structure of the complex has been determined by single crystal X-ray diffraction analysis. The space group is witha=9.198(2),b=9.516(2),c=13.842(3) Å, =102.00(3), =108.34(3), =93.58(3)°,Z=1, andDc=1.506 g cm^–3. The silver atoms are each coordinated by one phosphorus atom from triphenylphosphine and two oxygen atoms from the carboxylate groups in a T-shape. The complex is further characterized by its IR,¹H, and³¹P NMR spectra.     

Synthesis, structure and characterization of a new inorganic-organic hybrid complex (C3H5N2)2[Cd(C3H4N2)2Nb2O3F8]·2H2O

(C₃H₅N₂)₂[Cd(C₃H₄N₂)₂Nb₂O₃F₈]·2H₂O (C₃H₄N₂=imidazole) (1) was prepared from the hydrothermal reaction of Nb₂O₅, 3CdSO₄·8H₂O, C₃H₄N₂, HF and H₂O at 403 K, and characterized by single crystal X-ray diffraction and IR spectra. 1 crystallizes in the orthorhombic system, space group Pba2, with a=11.0192(9), b=16.8012(14), c=6.8717(6) ?, and Z=2. The crystal is made up of [Cd(C₃H₄N₂)₂Nb₂O₃F₈]²⁻ anions, [C₃H₅N₂]⁺ complex cations and H₂O molecules of crystallization. And the backbone of the compound is a one dimension coordination polymeric chain containing the anions. The complex cations and anions are linked through hydrogen bonding interactions. Co-crystallized water molecules fill in the pores and hydrogen bond to the host. Bond valence sums show that O1, O3 and F3 have much more negative charge, which are in agreement with the crystal structure that they act as bridging atoms.Supplementary material CCDC-606794 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdc.cam.ac.uk/ const/retrieving.html or from the Cambridge Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033 or e-mail: deposit@ccdc.cam.ac.uk.     

Crystal structure of [Co(o-SC6H4NH2){P(OMe)3}3]PF6

A cobalt-thiolato-phosphite complex [Co(o-SC₆H₄NH₂){P(OMe)₃}₃]PF₆ has been prepared and characterized by X-ray crystallography. The complex crystallizes in the triclinic space group with a = 10.590(4), b = 11.122(3), c = 13.577(5) Å, = 101.85(1), = 108.50(1), = 101.75(1)°, V = 1420.6(8) ų, and Z = 2. The structure comprises discrete [Co(o-SC₆H₄NH₂){P(OMe)₃}₃]⁺ cations and PF ₆ ^– anions where the metal atom is coordinated in a highly distorted square-pyramidal environment by one chelate o-SC₆H₄NH ₂ ^– (abt) and two P(OMe)₃ ligands in the basal positions, and a third P(OMe)₃ in the axial site with Co–N,, 1.847(5), Co–S, 2.166(2), Co–P, 2.157(2), 2.147(2), and 2.125(2) Å.     

Chiral bisphosphanes XII: Synthesis and molecular structure of cis-{rac,trans-1,2-bis[bis(morpholin-4-yl)-phosphino]cyclopentane}dimethylplatinum(II), cis-[C5H8{P[N(C2H4)2O-cyclo]2}2Pt(CH3)2]

Crystals of the title compound are monoclinic, space group P2₁/c, with a = 10.2621(8), b = 15.372(5), c = 17.612(2) Å, = 95.928(9)°, and Z = 4. Coordination about the central metal deviates slightly from ideal square-planar geometry. The five-membered chelate ring adopts an envelope conformation with one of the two P atoms (P1) deviating from the least-squares plane spanned by the central metal, the bridging CH carbons, and donor atom P2. While the morpholino substituents at the latter show little axial-equatorial discrimination for their orientation with respect to the coordination plane, the spatial alignments of the N(C₂H₄)₂O rings attached to P1 differ significantly between a more equatorial and a more axial disposition. The conformationally dissimilar arrangement of the two P donor groups within the envelope-like chelate ring manifests itself in unequal Pt–P bond lengths: d(Pt–P1) = 2.2677(16), d(Pt–P2) = 2.2825(16) Å. The Pt–CH₃ distances amount to 2.114(6) (trans to P2) and 2.141(6) Å (trans to P1), respectively.     

Synthesis and crystal structure of the thiophene-3-acetonitrile complex fac-[Mo(CO)3{NCCH2(C4 H 3S-3)}3]

Reaction of fac-[Mo(CO)₃(NCMe)₃] with three equivalents of NCCH₂(C₄ H ₃S-3) in acetonitrile gives the tris(thiophene-3-acetonitrile) complex, fac-[Mo(CO)₃{NCCH₂(C₄H₃S-3)}₃] (1) in 7% yield. Complex 1 crystallizes out in the orthorhombic space group Pnma with a = 12.714(17), b = 16.41(2), c = 11.304(16) Å, Z = 4. The structure has crystallographic m symmetry and the metal is in an almost perfect octahedral environment, with a facial arrangement of carbonyl and thiophene-3-acetonitrile groups. The thiophene rings are disordered.     

Structure of 2-{2-[3-methyl-3-(2,4,6-trimethylphenyl) cyclobutyl]-2-oxoethyl}isoindole-1,3-dione

2-{2-[3-Methyl-3-(2,4,6-trimethylphenyl)cyclobutyl]-2-oxoethyl}isoindole-1,3-dione (C₂₄ H₂₅NO₃) was synthesized, and its crystal structure was determined by X-ray crystallographic techniques. The compound crystallizes in the triclinic space group P-1, with unit cell parameters: a = 14.109(9) Å, b = 14.130(8) Å, c = 12.152(6) Å, = 105.62(5)°, = 113.75(4)°, = 98.78(5)°, V = 2039.8(19) ų, D _c= 1.223 g/cm³, and Z = 4. The crystal structure has two crystallographically independent molecules, I and II. These molecules are held together by weak intermolecular C—H···O interactions, forming a continuous chain. The dihedral angles between the N-substituted phthalimide moiety and cyclobutane ring in molecules I and II are 60.37(14) and 68.18(18)°, respectively.     

Syntheses,characterization and crystal structures of two structurally similar Schiff bases isonicotinic acid [1-(3-methoxy-2-hydroxyphenyl)methylidene]hydrazide and isonicotinic acid [1-(4-dimethylaminophenyl)methylidene]hydrazide monohydrate

The Schiff base compounds, isonicotinic acid [1-(3-methoxy-2-hydroxyphenyl) methylidene]hydrazide (C₁₄H₁₃N₃O₃, 1) and isonicotinic acid [1-(4-dimethylaminophenyl) methylidene]hydrazide monohydrate (C₁₅H₁₆N₄O·H₂O, 2) have been synthesized by the condensation of equimolar 3-methoxysalicylaldehyde or 4-dimethylaminobenzaldehyde with isonicotinic acid hydrazide in MeOH or EtOH. The compounds were characterized by elemental analysis, IR, ¹HNMR spectra, and single crystal X-ray diffractions. Compound 1 crystallizes in the monoclinic space group P-1 with unit cell dimensions a = 7.662(1) ?, b = 16.249(2) , c = 10.874(2) ?, β = 110.426(3)°, V = 1268.7(3) ′³, Z = 4, R ₁ = 0.0644, and wR ₂ = 0.1283. Compound 2 crystallizes in the orthorhombic space group P2₁2₁2₁ with unit cell dimensions a = 7.388(1) ?, b = 11.812(1) ?, c = 17.197(2) ?, V = 1500.7(2) ′³, Z = 4, R ₁ = 0.0585, and wR ₂ = 0.1143. X-ray structure determinations revealed that the molecules of both compounds display trans configurations with respect to the C=N double bonds. In the crystal structure of 1, molecules are linked through N–H···N intermolecular hydrogen bonds, forming layers parallel to the bc plane, while in the crystal structure of 2, molecules are linked through N–H···O, O–H···O, and O–H···N intermolecular hydrogen bonds, forming a network. Supplementary material CCDC-615072 and 620235 contain the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdccam. ac.uk/const/retrieving.html or from the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223–336033 or e-mail: deposit@ccdc.cam.ac.uk.     

Methyl 4-((E)-2-{3-[(3-{ (E)-2-[4-(methoxycarbonyl)phenyl]- 1-diazenyl}-5,5-dimethylhexahydro-1-pyrimidinyl)methyl]-5,5-dimethylhexahydro-1-pyrimidinyl-1-diazenyl) benzoate. X-ray crystal structure

Methyl 4-((E)-2-{3-[(3-{(E)-2-[4-(methoxycarbonyl)phenyl]-1-diazenyl}-5, 5-dimethyl hexahydro-1-pyrimidinyl)methyl]-5, 5- dimethylhexahydro-1- pyrimidinyl}-1- diazenyl) benzoate (1) has been synthesized by reaction of a mixture of formaldehyde and 2,2-dimethyl-1,3-propanediamine with p-methoxycarbonylbenzenediazonium chloride. The crystal structure of 1 has been determined by single crystal X-ray diffraction analysis. The crystals of 1 displayed problems of disorder; the asymmetric unit is built up by two independent molecules, which display disorder within a methoxycarbonyl group. The two independent molecules in the asymmetric unit are very similar, differing only slightly about the mutual orientation of the aryltriazenyl groups. With respect to the N–C–N bridge between the hexahydropyrimidinyl rings, the two equivalent fragments containing the triazene moieties are in a cis orientation. The N–N single bonds, in the range 1.319(4)–1.348(4) Å, and the N=N double bonds, in the range 1.255(5)–1.275(4) Å, indicate significant conjugations within the triazene moieties. All the hexahydropyrimidine six-membered rings adopt a chair conformation as shown by their puckering parameters. The crystal packing is determined only by simple van der Waals interactions. The crystal structure of 1 is compared with the previously reported structure of the unbranched hexahydropyrimidine analogue 2. Crystal data: 1 C29H40N8O4, triclinic, space group P-1, a = 13.9652(2), b = 14.2908(3), c = 16.6129(4) Å, = 97.279(1), = 90.872(1), = 107.385(1), V = 3133.6(1) ų, for Z = 4.     

Synthesis,characterization and crystal structure of a mononuclear iron(III) complex derived from 4-bromo-2-[(pyridin-2-ylmethylimino)methyl]phenol

A nitrate salt of bis[4-bromo-2-(pyridin-2-ylmethyliminomethyl)phenolato]iron(III), [Fe(C₁₃H₁₀BrN₂O)₂].NO₃, has been obtained and characterized by elemental analysis and X-ray single crystal determination. The complex crystallizes in the tetragonal space group P4₂/n with unit cell dimensions a = b = 17.608(3) ?, c = 17.199(3) ?, V = 5332.4(15) ?³, Z = 8, R ₁ = 0.0444 and wR2 = 0.0902. The complex consists of a [Fe(C₁₃H₁₀BrN₂O)₂]⁺ cation and a nitrate anion. The Fe atom in the cation is six-coordinated in an octahedral geometry. In the crystal structure, molecules are linked through weak C–H⋯O intermolecular hydrogen bonds, forming chains running along the c axis. Supplementary material CCDC-607149 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdccam.ac.uk/const/retrieving.html or from the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033 or e-mail: deposit@ccdc.cam.ac.uk.     

Synthesis and crystal structure of [Nd(H2O)2]2(C2O4)3

Some crystals of [Nd(H₂O)₂]₂(C₂O₄)₃ were synthesized hydrothermally by heating at 200°C for 8 days an aqueous suspension of neodymium oxalate decahydrate in presence of terephthallic acid and guanidinium carbonate. They crystallize in the orthorhombic system, space group P2₁2₁2₁, with a = 8.6702(7) Å, b = 9.558(2) Å, and c = 17.009(2) Å. The structure of this complex is built up by two independent neodymium atoms, three bischelating oxalate ligands, and four water molecules forming a rectangle building unit of 6-membered ring, [Ln(H₂O)₂(C₂O₄)]₆. The packing of these units leads to a layer parallel to the plane (001). However, the neodymium atoms of two neighbor layers share an edge of oxalato oxygen atoms thus giving a double-layer. The three dimensionality between these double-layers is insured by hydrogen bonds of water molecules which are bound to the neodymium atoms. There is no zeolitic water molecule. The two neodymium atoms are nine-coordinated. In both cases, the coordination polyhedron can be described as a distorted tricapped trigonal prism.     

Crystal structures of [WI2(CO)3{Ph2P(CH2) n PPh2}] (n = 2 or 3)

[WI₂(CO)₃{Ph₂P(CH₂)₂PPh₂}] (1) crystallizes out in the monoclinic space group P2₁/n, with a = 13.852(7) Å, b = 14.789(19) Å, c = 14.915(19) Å, = 102.86(1)°, Z = 4. [WI₂(CO)₃{Ph₂P(CH₂)₃PPh₂}] (2) crystallizes out in the monoclinic space group P2₁/n, with a = 10.499(15) Å, b = 14.58(2) Å, c = 20.75(3) Å, = 103.59(1)°, Z = 4. Both structures show the metal in a seven-coordinate environment with a carbonyl in the unique capping position, two further carbonyls and a phosphorus in the capped face, and two iodides and the second phosphorus in the uncapped face.     

Synthesis,characterization and crystal structure of bis{2-methoxy-6-[(2-diethylaminoethylimino)methyl]phenolato}thiocyanatocobalt(III) perchlorate

Brown block-shaped crystals of bis{2-methoxy-6-[(2-diethylaminoethylimino)methyl]phenolato}thiocyanatocobalt(III) perchlorate, the first cobalt(III) complex derived from the Schiff base ligand HL, [Co^III(L)(HL)(NCS)].ClO₄ (HL=2-methoxy-6-[(2-diethylaminoethylimino)methyl]phenol) have been obtained and characterized by elemental analysis and X-ray single crystal determination. The complex crystallizes in the monoclinic space group P2₁/c with unit cell dimensions a=16.087(3) ?, b=12.354(3) ?, c=16.762(3) ?, β=93.77(3)°, V=3324.1(12) ?³, Z=4, R ₁=0.0741 and wR2=0.1366. X-ray structure determination revealed that the complex consists of a [Co^III(L)(HL)(NCS)]⁺ cation and a disordered perchlorate anion. The Co atom in the cation is six-coordinate in an octahedral coordination. In the crystal structure, the perchlorate anions are linked to the cations through intermolecular C–H⋯O hydrogen bonds, forming zigzag chains running along the caxis. It is the first cobalt(III) complex derived from the Schiff base ligand HL.     

Synthesis and crystal structure of a terephthalato-bridged copper(II) complex [Cu2(tpt)(bpy)2(H2O)4] [Cu2(tpt)3 (bpy)2(H2O)2]

A terephthalato-bridged copper(II) complex [Cu₂(tpt)(bpy)₂(H₂O)₄][Cu₂(tpt)₃(bpy)₂ (H₂O)₂] (1) (tpt = terephthalate, bpy =; 2,2'-bipyridine) was synthesized by the reaction of Cu(ClO₄)₂ 6H₂O and terephthalic acid in the presence of 2,2'-bipyridine in H₂O solution. Crystal structure of 1 was determined by X-ray diffraction analysis in the triclinic space group P , with a = 10.7327(10) Å, b = 11.1658(11) Å, c = 17.3768(16) Å, = 108.063(2), = 91.064(2), = 116.721(2), V = 1737.5(3) ų, and Z = 2. Both the anion and the countercation in 1 are copper(II) complexes linked by terephthalate bridges in the bis(monodentate) (syn–anti) mode. The anion and the countercation are also linked by two hydrogen bonds between coordinating water molecules and terephthalate ligand.     

A new monoclinic crystal phase of [Bu4N][Ni(dmit)2]

The crystal structure of the title compound, tetrabutylammonium bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III), [N(C₄H₉)₄][Ni(C₃S₅)₂], is the fourth known phase of this polymorphous compound. It is monoclinic space group P2₁/c, with a = 20.040(2) Å, b = 13.1151(17) Å, c = 12.1093(15) Å, = 105.456(15)°, and V = 3067.5(6) ų with Z = 4, for D _calc = 1.503 g cm^–3. The [Ni(dmit)₂] anion packing arrangement consists of arrays of side-on touching anions and these arrays are connected via head-to-tail close S S contacts.     

Structure of 4,6-dimethylisothiazolo[5,4-b]pyridin-3(2H)-one and its 2-[4-(2-methylphenyl) piperazin-1-ylmethyl] derivative

The crystal and molecular structures of 4,6-dimethylisothiazolo[5,4-b]pyridin-3(2H)-one, C₈H₈N₂OS, 1, and its 2-[4-(2-methylphenyl)piperazin-1-ylmethyl] derivative, C₂₀H₂₄N₄OS, 2c, are described. These compounds crystallize in the monoclinic system in the space group P2 ₁/c. The cell constants for compound 1 are a = 5.049(1), b = 14.897(1), c = 11.330(1) Å, = 98.07(1)°, Z = 4, T = 293 K, and D _cal = 1.419 g cm^–3, and for compound 2c are a = 15.525(1), b = 12.021(1), c = 10.911(1) Å, = 106.42(1)°, Z = 4, T = 293 K, and D _cal = 1.253 g cm^–3 The structures were solved by direct methods and refined to R values of 0.0411 and 0.0380 for 1640 and 3504 reflections for 1 and 2c, respectively. The analysis of the geometry and difference electron density map reveal that the dimethylisothiazolopyridine 1 exists in the amino tautomeric form in the crystalline state. The conformation of the o-methylphenylpiperazine part of the molecule 2c strongly depends on the substituents effect in the phenyl ring and is very similar to those observed in crystals for other investigated arylopiperazine derivatives of the isothiazolopyridine.     

Synthesis of homoleptic lanthanide amides and the crystal structure of [Li(THF)4][Y(NPh2)4]

Anhydrous LnCl₃ reacted with three equivalents of LiNPh₂ in THF to give the unexpected homoleptic lanthanide amides [Li(THF)₄][Ln(NPh₂)₄] (Ln = Sm (1), Y (2)) in high yield. The crystal structure of complex 2 has been determined by X-ray diffraction methods. It crystallizes in the orthorhombic space group Pbcn with a = 17.522(3) Å, b = 16.321(3) Å, c = 19.947(3) Å, V = 5704.4(17) ų, and D _calc = 1.231 mg/m³ for Z = 4. Complex 2 is composed of discrete [Li(THF)₄]⁺ cations and [Y(NPh₂)₄]^– anions, both of which have crystallographically imposed two-fold symmetry. To achieve steric saturation of the metal center, there are interactions between the yttrium atom and one -carbon atom of each amide ligand. The yttrium and lithium atoms both exhibit distorted tetrahedral coordination geometry.     

Synthesis and structure of the first water-soluble chiral monomeric MnIV complex: [Δ-MnIV(biguanide)3] (ClO4)4·H2O

The reaction of KMnO₄ with alkaline biguanide sulfate solution, followed by acidification of the resulting stable filtrate with concentrated HClO₄, led to the title complex, 1. The crystal structure of the [Δ-Mn^IV(bigH)₃](ClO₄)₄·H₂O (1, bigH: biguanide, C₂H₇N₅) has a tetragonal chiral P4 ₁ 2 ₁ 2 space group with a = b = 11.416(3) ?, c = 20.742(7) ?, Z = 4. The complex consists of one chiral [Δ-Mn^IV(bigH)₃] tetracation, four ClO₄ ⁻ anions, and one water molecule. In the tetracation, six N atoms from three neutral biguanide chelate coordinate to the Mn^IV cation, forming an octahedron with Δ-optical activity. The [Δ-Mn^IV(bigH)₃] tetracation interconnects each other by numerous hydrogen bonds with N–H···O and O–H···O between biguanide moieties of the [Δ-Mn^IV(bigH)₃] tetracations and counter-anions as well as water molecules, to construct a three-dimensional network.     

Synthesis and crystal structure of the copper(II) complex with novel Schiff base ligand: Cu(C8H7O2N)2(OH2)

The title complex Cu(C₈H₇O₂N)₂(OH₂) crystallized in the orthorhombic space group, Pbca with unit cell parameters: a = 15.242(2), b = 11.782(4), c = 17.946(4) Å, and Z = 8. Two nitrogen atoms, two phenolic oxygen atoms of the ligand, and one water molecule are coordinated with copper to form a distorted tetragonal pyramidal polyhedron.     

Synthesis and crystal structure of 3-[2-oxo-2-(4-methyloxyphenylsulfonamidophenyl)ethylidene]-3,4-dihydro-1H-quinoxalin-2-one

3-[2-Oxo-2-(4-methyloxyphenylsulfonamidophenyl)ethylidene]-3,4-dihydro-1H-quinox-alin-2-one (4) was synthesized and characterized by ¹H NMR,¹³C NMR, IR, and single-crystal X-ray diffraction techniques. The crystallographic results show that the composition of the title compound is C₂₃H₁₉N₃O₅S. It belongs to triclinic crystal system and P-1 space group, with a=7.273(6) ?, b=9.092(7) ?, c=15.928(13) ?; α=85.135(11)°, β=78.297(10)°, γ=84.619(11)°, V=1024.4(14) ?³, Z=2, D _c=1.457 mg/m³, μ = 0.201 mm⁻¹, F(000)=468, R=0.0597, wR=0.1438. Supplementary material CCDC-281953 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at www.ccdc.cam.ac.uk/retrieving.html or from the Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44-1223-336033; e-mail: deposit@ccdc.cam.ac.uk.