Crystal structure of [Cu2(II)(dmpa)2(p-Cl-C6H5COO)2] (Hdmpa = N,N-dimethyl-3-amino-1-propanol)

The copper complex, [Cu₂(II)(dmpa)₂(p-Cl-C₆H₅COO)₂], has been prepared and its structure determined using X-ray crystallography. The dimer is a di-₂-alkoxo complex which is a five-coordinate copper dimer with unsupported alkoxo bridges. The complex crystallizes in the triclinic space group P-1 with a = 11.384(2), b = 14.636(5), c = 9.609(2) Å, = 100.07(2), = 104.33(3), = 72.79(2)°, V = 1471.8(7) ų, and Z = 2. The structure is comprised of discrete binuclear clusters in which the metal atoms are bridged by two alkoxo oxygens of the dmpa^– ligands. The Cu-O and Cu-N distances are in good agreement with those found for other copper(II) aminoalcoholato complexes. The Cu···Cu distance is 2.9765(6) Å. In the crystal, every two dimeric coordination molecules are combined together by the recognition through intermolecular hydrogen-bonding interactions between the apical water molecule and the non-coordinated O atom from the p-chlorobenzoato ligand, forminga tetramer.     

Crystal structure of [Mn2(III)(salpa)2Cl2(H2O)2] (H2salpa = 1-(salicylaldeneamino)-3-hydroxypropane)

The manganese complex, (Mn₂(III)(salpa)₂Cl₂(H₂O)₂], has been prepared and its structure determined using x-ray crystallography. The dimer is a di-₂-alkoxo complex which is a six-coordinate manganese dimer with unsupported alkoxide bridges and a rare example of a chloride- and water-containing manganese dimer. The complex crystallizes in the monoclinic space group P2₁/c with a = 9.315(5), b = 11.130(4), c = 11.637(5) Å, = 104.33(3)°, V = 1169.0(9) ų, and Z = 2. The structure comprises discrete binuclear clusters in which the metal atoms are bridged by two alkoxo oxygens of the salpa^2– ligands. The Mn—O and Mn—N distances are in good agreement with those found for other manganese(III) Schiff base complexes. The Mn—Cl and Mn—O3 distances are 2.585(2) and 2.371(2) Å, respectively, and the Mn ··· Mn distance is 3.001(1) Å. In the crystal, there are two types of hydrogen bonding between the H₂O molecule and the Cl atom with Cl ··· H(H₂O) distance of 2.33(6) (intramolecule: –1 + x, y, –1 + z) and 2.68(6) Å (intermolecule: –1 + x, 0.5–y, –0.5 + z).     

Hydrothermal synthesis of [Mn(HTPO)(BIPY)] (H3TPO = tris-(4-carboxylphenyl)phosphine oxide): a crosslinked coordination polymer

The hydrothermal synthesis and crystal structure of the title compound is reported. The structure consists of 1-D looped chains with the HTPO ligand binding through the phosphoryl and two carboxylate oxygens to manganese atoms. The carboxylic acid group is hydrogen bonded to adjacent chains forming a 2-D hydrogen bonded network. The crystals are triclinic and the space group isP-1 with a = 11.6767(8) Å, b = 10.8680(8) Å and c = 11.4232(87rpar; Å = 92.301(2)°, = 106.932(2)° and = 103.2390(10)° V = 1341.02(16) ų; Z = 2.     

Molecular complexes of 3-amino-1,2,4-triazole: The crystal structure of 3-amino-1,2,4-triazolium 5-nitrofuran-d2-carboxylate

3-Amino-1,2,4-triazolium (3-AT) 5-nitrofuran-2-carboxylate has been prepared and its x-ray crystal structure reported (a = 12.363(3) Å, b = 12.5720(10) Å, c = 12.8550(10) Å, Pbca, orthorhombic, Z = 8, and D _c = 1.604 mg m^–3). The solid-state packing of this organic acid-base salt consists of a three-dimensional hydrogen-bonded network which exhibits a cage-like repeat unit involving both the N(2)–H and N(4)–H sites of 3-AT. A review of five such structures reveals that in all cases the carboxylate groups interact with either of these sites [and the N(31)H₂] and form a R ² ₂(8) graph set interaction. Analysis of all 3-AT complexes which form this interaction reveals that the hydrogen-bonding distances between the non-hydrogen atoms are not equal [av. 2.712(5) Å and 2.897(5) Å], with the shorter distance being the interaction between the heterocyclic nitrogen and the corresponding carboxylate oxygen. Furthermore, a review of the interactive modes of all 3-AT adducts has been undertaken.     

The crystal and molecular structure of bis(melamine)silver(I) perchlorate, Ag(C3H6N6)2ClO4

The crystal structure of the title compound, Ag(mela)₂ClO₄ (mela = melamine), has been investigated by X-ray diffraction techniques, the crystals are triclinic, space group P1¯, with a = 5.236(2), b = 7.5385(9) c = 19.063(3) Å, = 99.91(1), = 90.53(2), = 108.32(2)° and Z = 2. The Ag atom has a coordination geometry with two strong bonds (2.162(2) and 2.179(4) Å) to the nitrogen of the melamines and two weak bonds (2.776(4) and 2.785(4) Å) to oxygen atoms of the ClO^– ₄anions. The N—Ag—N vector is markedly nonlinear (angle at Ag 167.7(2)°).     

Synthesis and the crystal structure of aqua-dioxo-nitrato-(2,2′,6′,2″-terpyridine)-neptunium(V) [NpO2(NO3)(terpy)(H2O)]

The crystal structure of the [NpO₂(NO₃)(Terpy)(H₂O)] complex between pentavalent neptunium and 2,2′,6′,2″-terpyridine is determined. The crystal data are as follows: a = 11.130(3) Å, b = 7.916(2) Å, c = 18.324(5) Å, β = 100.873(6)°, V = 1585.5(8) ų, Z = 4, space group is P2₁/n, R = 0.044, and wR(F ²) = 0.092. The coordination polyhedron of the Np atom is a pentagonal bipyramid whose equatorial plane includes three nitrogen atoms of the Terpy molecule and two oxygen atoms of the nitrate ion and the water molecule.     

Synthesis and crystal structure of N-benzylmethy- lammonium pentachlorothallate (III), [C6H5CH2NH2CH3]2TlCl5

N-Benzylmethylammonium pentachlorothallate (III) salt crystallizes in the monoclinic system P2₁/c with the following unit cell dimensions: a = 10.9540 (8), b = 12.559(1), c = 18.099(2)Å, = 112.1(3)° and Z = 4. The examination of the structure shows an alternate stacking of inorganic layers of pentachlorothallate (III) anions and organic layers of [C₆H₅CH₂NH₂CH₃]⁺ cations parallel to the c axis. The cohesion forces of the packing of N-benzylmethylammonium units in the layer and between two adjacent layers are provided by hydrogen bonds (N—HsCl) and van der Waals contacts.     

Ether cleavage of [2.2.2]cryptand: synthesis and X-ray crystal structure of [NH(CH2CH2I)3][I5]

Treatment of [2.2.2]cryptand1 in toluene with HI(g) has resulted in the formation of a twophase liquid clathrate solution from which the complex [NH(CH₂CH₂I)₃][I₅]2 has been isolated and crystallographically characterized. Crystal data for2: triclinic, space group $P\bar 1$ ,a=9.301(3) Å,b=10.419(3) Å,c=11.078(3) Å, α=90.20(2)^o, β=103.28(2)^o γ=96.50(2)^o,D _c =3.57g/cm³,Z=2,R _f =0.054,R _w =0.054. The salt is a product of an ether cleavage of the macrobicycle. The crystal structure of2 contains [NH(CH₂CH₂I)₃]⁺ ions and zigzag chains of [I₅]^? ions which self-assemble to form alternating layers, of cations and anions.     

Crystal structure of mixed-ligand copper(II) complexes. Bis(2,2′-bipyridyl)monophenylphos-phatocopper(II)monophenylphosphate monohydrate, [Cu(C10H8N2)2(C6H5OPO3)]-(C6H5OPO3H2)(H2O)

The title mixed-ligand copper(II) complex has been synthesized and its crystal structure at room temperature solved. The crystals are monoclinic:P2₁/c,a=12.004(3),b=19.402(5),c=14.192(4) Å,=108.80(3)°,Z=4. The structure was solved by direct methods, and refined to anR value of 0.041 for 4457 nonzero independent reflections. The crystal structure consists of discrete [Cu(bipy) (MPhP)] units, noncoordinated MPhPH₂, and H₂O molecules. Each [Cu(bipy)₂(MPhP)] unit involves a five coordinate CuN₄O chromophore with a distorted trigonal-bipyramidal stereochemistry. The phosphate groups are linked together by short hydrogen bonds of (P)-O-H--O-P type.     

A novel vanadyl selenite templated by organic salt: [(VO)(H2O)2(SeO3)]2[(H2pipe)SO4]

The title compound [(VO)(H₂O)₂(SeO₃)]₂[(H₂pipe)SO₄] was synthesized under hydrothermal condition with VOSO₄, piperazidine (pipe), and SeO₂, and its crystal structure was established using single-crystal X-ray diffraction method. The title compound was characterized with IRFluorescence. The crystal data: P-1 (No. 2), a = 8.633(2) Å, b= 9.223(2) Å, c= 12.508(3) Å, =109.28(3)°, =90.42(3)°, = 107.79(3)°, Mr = 644.08, V=888.5(3) ų, Z=2, Dc = 2.407 g cm^–3, =5.350 mm^–1, F(000)=632. The structure of the title compound consists of an infinite neutral ladder chain, which is built up from VO₆ octahedral and SeO₃ pyramidal units sharing vertices, and organic salt. The biprotonized pipe (piperazidine) and SO₄ ^2– interact with one another and the inorganic chain through strong hydrogen bonds N–H···O or O–H···O to give a 3D structure. Hydrogen bonds play a role of stabilization structure.     

Intra- vs intermolecular hydrogen bonding. The crystal structure of 5-methyl-2-hydroxyacetophenone thiosemicarbazone monohydrate and salicylaldehyde-2-methylthiosemicarbazone monohydrate

The crystal structure of 5-methyl-acetophenonethiosemicarbazone monohydrate,A, and salicylaldehyde-2-methylthiosemicarbazone monohydrate,B, were determined using single crystal X-ray diffraction.A crystallizes in the monoclinic space groupC2/c, with lattice parametersa=14.161(2),b=15.753(1) ?,c=11.084(1) ?, β=112.59(1)° andZ=4, yielding a calculated density ofD _calc=1.352 mg/m³.B crystallizes in the triclinic space groupP1, witha=7.233(2) ?,b=7.371(2) ?,c=11.841(2) ?, α=82.77(2)°, β=78.33(2)°, γ=63.06(2)° andD _calc=1.371 mg/m³ forZ=2,. In bothA andB the immine nitrogen and the sulfur atom areanti with respect to N2-C8. WhileA presents the usual intramolecular six membered hydrogen bond ring,B has instead an intermolecular hydrogen bond between the hydroxy moiety of the salicyladehyde and a water molecule. AM1 calculations agree with the experimental conformations observed in both compounds. Contribution No. 1619 of the Instituto de Química, UNAM.     

Crystal structures of 3-[1-Benzenesulfonyl-3-phenylsulfanyl-1H-indol-2-yl]-1-[4-(methyl (I)/methoxy (II) phenyl)]-2-phenyl-propane-1-one

The compounds 3-(1-Benzenesulfonyl-3-phenylsulfanyl-1H-indol-2-yl)-1-[4-methyl (I)/methoxy (II)phenyl)]-2-phenyl-propane-1-one crystallize in triclinic space group P . The details are: compound I a = 11.941(6) ?, b = 12.154(7) ?, c = 13.006(7) ?, α = 63.124(8)°, β = 84.464(9)°, γ = 64.810(8)°, V = 1519.7(14) ?³, Z = 2, D _cal = 1.284 Mg m⁻³, and R = 0.0382 (wR = 0.0978); compound II a = 11.897(6) ?, b = 12.268(6) ?, c = 13.001(7) ?, α = 61.919(8)°, β = 83.480(8)°, γ = 64.676(7)°, V = 1504.0(14) ?³, Z = 2, D _cal = 1.333 Mg m⁻³, and R = 0.0422 (wR = 0.1049). The indole ring system in both the molecules I and II are not strictly planar and the dihedral angles formed by the pyrrole and benzo planes are 4.0(7)° and 3.5(8)°, respectively. The C–HO, C–Hπ and ππ types of interactions stabilize the molecules in the unit cell in addition to van der Waal's forces in I and II.     

Synthesis and crystal structure of catena-poly[aqua(cis-syn-cis-dicyclohexyl-18-crown-6) tetra(thiocyanato)barium(II) platinum(II)]: [BaPt(NCS)4(C20H36O6)(H2O)] n

An organic–inorganic hybrid polymeric complex, [BaPt(NCS)₄(C₂₀H₃₆O₆)(H₂O)] _n or [[Ba(DC18C6-A)(H₂O)][Pt(SCN)₄]] _n (1) (DC18C6-A = cis-syn-cis-dicyclohexyl-18-crown-6) has been synthesized by the reaction of cis-syn-cis-dicyclohexyl-18-crown-6 with Ba(SCN)₂, BaCO₃ and H₂PtCl₄, and characterized by elementary analysis, FT-IR spectra and X-ray single-crystal diffraction. It crystallizes as monoclinic, space group P 2₁/n with crystallographic data: a = 14.275(6) ?, b = 13.165(5) ?, c = 18.971(8) ?, β = 106.294(6)°, V = 3422(2) ?³, Z = 4, D _calcd = 1.854 g/cm³, F(000) = 1856, R ₁ = 0.0491, wR ₂ = 0.0709. The asymmetric unit of complex 1 contains one [Ba(DC18C6-A)(H₂O)]²⁺ complex cation and one [Pt(SCN)₄]²⁻ complex anion, which are assembled into an infinite polymeric chain via the bridging SCN groups. The coordinated water molecule gives two different intrachain and interchain hydrogen bonds.     

Crystal and molecular structure of di(1-pyrazolyl)methane,CH2(C3N2H3)2

The title compound consists of two planar pyrazolyl fragments oriented at 73.0° to each other and linked to a common carbon atom. All hydrogen atoms were located unambiguously and their positions were refined.     

Investigations of dehydroepiandrosterone. Part I: crystal structure of sublimed DHEA

The crystal structure of an orthorhombic polymorph of the title compound, crystallized by sublimation, has been determined. Dehydroepiandrosterone, C₁₉H₂₈O₂, space groupP2₁2₁2₁ witha=6.6408(4)b=11.4423(11)c=22.085(2)Å,V=1678.2(4)ų,Z=4. The structure was refined toR=0.051 for 2645 observed reflections. The conformation of the molecule is similar to that found in other polymorphs and solvates, with a chair A ring, an 8, 9 half-chair B ring, a chair C ring, and a 14 envelope D ring. Molecules are linked in chains by OH...O hydrogen bonds involving the carbonyl oxygen atom. The O...O distance is 2.855(3) Å, and the angle about H is 171(2)^o.     

X-ray crystal structure of (6-n-propyl-2-thiouracilato)(triethylphosphine)gold(I)

The crystal structure of the title compound [Et₃PAu(PTU)] is reported. There are two molecules in the asymmetric unit and each of the independent Au atoms exists in a linear geometry defined by a P atom of the phosphine ligand and a thiolate S atom derived from the thionucleobase; molecule 1: Au-P 2.255(5), Au-S 2.314(5)Å, P-Au-S 176.9(2)° and molecule 2: Au-P 2.249(5), Au-S 2.328(4)Å and P-Au-S 175.0(2)°. The lattice features weak AuAu contacts of 3.486(1)Å and hydrogen bonding interactions involving theOxo and N-H groups. Crystals are monoclinic, space groupP2₁/c with unit cell dimensions:a=21.445(2),b=8.931(2),c=17.956(3)Å;=96.09(1)° andZ=8. The structure was refined by a full-matrix least-squares procedure to finalR=0.053 using 2875 reflections withI3.0(I).     

Synthesis and crystal structure of bis(2-methylbenzimidazolium) tetrahalocuprate(II)

The crystal structures of 2-methylbenzimidazolium tetrahalocuprates (H2-mebz)₂[CuX₄] (X = Cl and Br) have been detemined. The chloride salt is monoclinic, P2₁/c, with a = 8.540(2) Å, b = 16.591(2) Å, c = 14.303(3) Å, and = 98.69(2)°. The bromide salt is also monoclinic, P2₁/c, with a = 8.316(3) Å, b = 17.436(3) Å, c = 14.747(3) Å, and = 98.82(3)°. Both the compounds contain discrete distorted tetrahedral CuX₄ ^2– anions and almost planar 2-methylbenzimidazolium cations. In the chloride salt, three chloride ions are involved in hydrogen bonding instead of two bromide ions in the bromide salt.     

Synthesis and structure of the three‐dimensional coordination polymer [Ag3hmt3(μ3 ‐btc)]·5H2O

A new coordination polymer, [Ag₃hmt₃(μ₃ ‐btc)]·5H₂O (1) (hmt = hexamethylenetetramine, btc=1,3,5‐benzenetricarboxlic), has been successfully synthesized. Crystal data: P2₁/a, a = 11.9906(2) Å, b = 17.3689(2) Å, c = 16.96100(10) Å, β = 101.9820(14)°, V = 3455.40(7) ų, Z = 4, Dc = 2.002 Mg/m³. In the hexagonal structure of Ag‐hmt unit, each Ag‐hmt unit comprises three Ag atoms and three hmt ligands. The μ₃ ‐btc ligands bridge adjacent two‐dimensional honeycomb‐like Ag‐hmt layers to form three‐dimensional networks. Structure analysis show that hydrogen bonds play a key role for the stable structure in the compounds. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of the bidentate ligand 2,2-di(1-pyrazolyl)propane,CH3C(C3N2H3)2CH3

The title compound lies on a site of C₂ symmetry, with the two planar pyrazolyl moieties oriented at 86.1° to one another. The hydrogen atoms were located and refined.     

The X-ray crystal structure of Hg(p-MeC6H4)(O2CC6F5) from synchrotron radiation

The X-ray crystal structure of Hg(p-MeC₆H₄)(O₂CC₆F₅) reveals near linear C—Hg—O units stacked into columns with intermolecular Hg–O bonding and overall distorted square-planar stereochemistry for mercury. Hg(p-MeC₆H₄)(O₂CC₆F₅) crystallizes in triclinic space group with a = 6.405(4), b = 7.285(3), c = 14.630(9) Å, = 84.07(3), = 81.21(3), = 86.87(3)° with calculated density 2.490 g cm^–3 for Z = 2.