Polymeric and mixed carboxylate compounds: Crystal structures of [Zn(tiglate)2]x and [Zn2(tiglate)3(crotonate)]x

The crystal structures of [Zn(O₂CC(CH₃)CHCH₃)₂]_x and [Zn₂(O₂CC(CH₃)CHCH₃)₃-(O₂CCHCHCH₃)]_x have been determined by single crystal X-ray diffraction. Both structures consist of chain polymers, in which pairs of zinc atoms are bridged alternately by three syn-syn carboxylates and by one syn-anti carboxylate. In the mixed carboxylate structure, the crotonate takes up preferentially the syn-anti bridge position. Vibrational and elemental analysis data indicate that the spontaneous solid-state reaction of zinc tiglate in air, accelerated for the tiglate and observable also for the mixed carboxylate compound by -ray or X-ray irradiation, gives an oxocentered tetranuclear complex [Zn₄O(O₂CR)₆] rather than a polymerization through cross-linking of the unsaturated carboxylates.     

Coordination properties of sulfonyl-N-aminoacids: Crystal and molecular structure of the [Zn(II) (N-(p-toluenesulfonyl)-L-glutaminate)2(H2O)2] complex

The coordination behavior of N-tosyl-L-glutamine (hereafter abbreviated as tsglnH, tosyl =toluenesulfonyl group) toward the Zn(II) ion is investigated by means of structural and spectroscopic techniques. From aqueous solution, at acidic pH the Zn(II) ion separates a compound of empirical formula Zn(tsgln)₂·2H₂O whose crystal structure is determined. The crystal is monoclinic, space group C2, with cell dimensions:a=19.775(5),b=5.3146(3),c=16.543(8) Å, =119.93(3)°,Z=2. The Zn(II) is tetrahedrally coordinated by two symmetry-related tsgln monoanions acting as monodentate carboxylate ligands and two symmetry related water molecules. The Zn–O bond distances are similar while the angles at Zn(II) ion differ significantly from those of regular tetrahedron. The side chain amide group does not participate in metal coordination and forms intermolecular hydrogen bonds.     

Crystal structure of 2,3-dihydronaphto[2,3-b) [1,5] dioxepin

The X-ray single crystal structure of C₁₃H₁₂O₂ compound was determined. It crystallizes in the orthorombic space group P2₁2₁2₁ with a = 7.8847(7), b = 9.639(1), c = 13.432(2) Å, Z = 4 and V = 1020.8(3) ų. The final R converged to 0.037 for 1763 independent reflexions. The title compound forms layers parallel to (1 0 0) planes and the three dimensional cohesion of the crystal is assumed by Van der Waals interactions. The molecule consists of two six-membered rings (A and B) and a seven-membered ring (C). A and B rings are planar, whereas the C ring has a chair conformation     

Crystal and molecular structure of [Cu(pyrimidine)4]2BF4

The crystal structure of [Cu(pyrimidine)₄]2BF₄ was determined using single crystal X-ray diffraction. The compound crystallizes in the monoclinic space groupP2₁/n, with lattice parametersa=9.9736(8),b=13.872(1),c=16.568(1) Å. β=98.002(1), andZ=8, yielding a calculated density of 1.857 g/cm³. The Jahn-Teller distorted copper coordination sphere is composed of the four pyrimidine ligands in the equatorial positions (ave. Cu?N=2.02 Å) and the longer axial bonds from the copper to one fluorine (ave Cu?F=2.39 Å) on each of the BF ₄ ^? anions. The crystal structure features layers of molecules having interleaved pyrimidine rings: the layers are connected through intermolecular H … F hydrogen bonds.     

Crystal and molecular structure of triphenyl[2-(p-tolylthio)ethyl]tin

The crystal and molecular structure of Ph₃SnCH₂CH₂SC₆H₄Me-p has been determined by X-ray crystallography. In each of the two independent molecules in the asymmetric unit the tin atom has an irregular tetrahedral geometry, with C–Sn–C valency angles ranging from 104.1(5) to 114.7(5)° in molecule (1) and from 104.6 to 112.7(6)° in molecule (2). The bond lengths, C_alkyl–Sn are 2.18(1) and 2.17(2)Å (in molecules (1) and (2), respectively) while the C_aryl–Sn bond lengths range from 2.11(1) to 2.13(1)Å in molecule (1) and from 2.09(1) to 2.14(1)Å in molecule (2). The Sn–C–C–S torsion angle, 172(1)° is the same for both molecules. NMR spectral data are presented; the¹H NMR spectrum in solution of the central-CH₂–CH₂-unit suggests that each of the protons on each of the CH₂ groups is magnetically distinct and that rotations about the C–C bond are slow on the NMR time scale. Comparisons with similar molecules are made and conformations discussed in terms of steric effects.     

Crystal structure of 2-mercaptobenzimidazole and bis[2-mercaptobenzimidazole]dichlorocobalt(II)

Delocalization of the imidazole electron density is observed in both structures. In the dichlorocobalt complex structure, the two crystallographically independent mercaptobenzimidazole molecules are attached together through the direct bonding of the Co(II) ion with two S atoms. The cohesion of the molecules in the crystals is due to intermolecular N–H...S, and; intra and intermolecular N–H...Cl hydrogen bonds, respectively.     

Crystal and molecular structure ofo-aminobenzoato (o-(p-dimethylaminobenzalidine)benzoato)(o-ammoniobenzoate)dimethyltin(IV), an example of a mixed carboxylate complex of tin

The structure of the title compound, [Me₂Sn(O₂CC₆H₄NH₂-o)(O₂CC₆H₄(N=C(H)C₆H₄NMe₂-p)-o)(^–O₂CC₆H₄NH₃-o)], has been determined at room temperature. The structure features a distorted trigonal bipyramidal coordination geometry for Sn, defined by three O atoms derived from chemically different, monodentate carboxylate ligands and two methyl groups. Crystals are monoclinic, space groupP2₁/n witha=14.718(5),b=10.981(4),c=20.321(3) Å, =110.74(2)°,Z=4; refinement on 2480 reflections gaveR=0.046.     

(Aroxymethyl)triphenyltin compounds: Crystal and molecular structure of triphenyl(p-toloxymethyl)tin

Compounds, Ph₃SnCH₂OAr, are available from Ph₃SnCH₂I and NaOAr in EtOH. The crystal and molecular structure of Ph₃SnCH₂OC₆H₄Me-p (II) has been determined by X-ray crystallography. The molecule in the crystal contains a slightly distorted tetrahedral tin atom [C-Sn-C valency angles varying from 106.9(5) to 114.1(6)°] with an intramolecular Sn---O distance of 2.900(11) Å. NMR spectral data for (II) and for Ph₃SnCH₂OC₆H₃Br₂-2,4 are reported.     

Crystal structure of Zn[Cl2Ti(C5H5)2]2·2C6H6

The structure of crystals of the composition Zn[Cl₂Ti(C₅H₅)₂]₂·2C₆H₆ has been determined from Patterson and Fourier syntheses of two projections, and refined toR = 0·117 by full-matrix three-dimensional least-squares methods. The crystals are orthorhombic:Pbcn,a = 18·45(5),b = 15·40(6),c = 11·35(3) Å,Z= 4. The complex consists of a central distorted ZnCl ₄ ^2– tetrahedron linked along the Cl—Cl edges to two distorted TiCl₂(C₅H₅)₂ ⁺ tetrahedra in such a way that their centres are nearly collinear The two C₆H₆ molecules in the formulae unit may be regarded as benzene of crystallization.     

Crystal structure of bis[dihydrobis(3,5-dimethy-1-pyrazolyl)borato]cadmium(II)

The structure of [H₂B(3,5-Me₂pz)₂]₂Cd shows the four nitrogen donor atoms form a pseudotetrahedral arrangement about the cadmium(II). The intraligand N—Cd—N angles are restricted to an average of 91.4° by the chelate rings forcing the interligand N—Cd—N bond angles to average 119.4°. The Cd—N bond distances average 2.21 Å with a range of 0.04 Å. The crystal is in the triclinic space group, P with a = 7.6793(2) Å, b = 8.5992(2) Å, c = 25.0874(4) Å, = 91.0791(2)°, = 97.9769(4)°, = 110.2344(6)°, and Z = 2.     

Crystal structure of potassium tris[3-(2-pyridyl)pyrazolyl]hydroborate

The crystal structure of the potassium tris[3-(2-pyridyl)pyrazolyl]hydroborate has been determined. Potassium tris[3-(2-pyridyl)pyrazolyl]hydroborate crystallizes in the orthorhombic space group Pca2₁ with the parameters a=30.7323(5) ?, b=8.3083(1) ? and c=9.2173(2) ?, V=2353.48(7) ?³ with Z=4. The crystal structure reveals the formation of continuous chains where two bidentate arms of the hydroborate ligand are coordinated to one potassium and the third to another cation. The structures of numerous transition metal and actinide salts have been reported during the last decades but no alkali metal complexes were available.     

Crystal structure of 4-methyl-2-phenylbenzo[de]cyclobut[i] isoquinoline-3,5(2H)-dione

4-Methyl-2-phenylbenzo[de]cyclobut[i]isoquinoline-3,5(2H)-dione, C₂₁H₁₅NO₂, resulted from the photochemical reaction of N-methyl-1,8-naphthalenedicarboximide with phenylacetylene, has been characterized by ¹H NMR, IR, and MS spectra and established by single-crystal X-ray crystallography. The crystal structure belongs to the monoclinic space group P2₁/n with cell parameters a = 12.530(2) Å, b = 9.324(2) Å, c = 13.296(2) Å, = 96.85(1), V = 1542.3(4) ų, and Z = 4.     

Crystal and molecular structure of [5,10,15,20-tetrakisphenyl-2-ethoxy-3-oxa-chlorinato]Ag(II)

The silver(II) complex of the chlorin-like derivativev [5,10,15,20-tetrakisphenyl-2-ethoxy-3-oxa-chlorinato]Ag(II) (1Ag), formally formed by substitution of one pyrrolic subunit in silvermeso-tetraphenylporphyrin by one ethoxy-substituted hydrooxazole moiety, crystallizes in the tetragonal space groupI4/m witha = 13.4811(10) Å,c = 9.7361(13) Å, andZ = 2. The molecule, which is asymmetric, accommodates the high-symmetry space group by rotational disorder with the silver atom located on the four-fold axis.     

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).     

Crystal and molecular structures of 1-isoquinolyl(phenyl)methyl benzoate and 1-isoquinolylisopropyl benzoate

Both of the title compounds crystallize in the monoclinic system: C₂₃H₁₇NO₂ (Ib),P2₁/c,a = 8.970(1),b = 22.629(5),c = 9.101(1) Å, = 106.08(1) °,Z = 4,D _x = 1.27 Mg m^–3; C₁₉H₁₇NO₂ (Ic),P2₁/a,a = 15.225(2),b = 6.429(1),c = 17.190(1) Å, = 112.99(1) °,Z = 4,D _x = 1.25 Mg m^–3. The structures were solved and refined by standard methods, both toR 0.04. In compound Ib, a weak intramolecular interaction is observed between the nitrogen atom from the isoquinoline ring and the carbon atom from the carbonyl group, with the N(2) . C(18)distance being 2.98 Å. In compound Ic, the PhCO₂ -fragment is twisted in the opposite direction to that in compound Ib, without hydrogen bonding. The pK _a and IR data were considered in the light of the results of the X-ray investigation.     

Crystal structure of 2,8,14,20-tetranaphthylpyrogallol[4]arene

The aromatic derivative 2,8,14,20-tetranaphthylpyrogallol[4]arene was synthesized by the acid catalyzed condensation of 2-naphthaldehyde and pyrogallol in refluxing aqueous ethanol. Single crystal X-ray analysis revealed that the molecule crystallizes in a triclinic space group P1(bar) No. 2, with a = 11.3396(7) Å, b = 15.9942(10) Å, c = 26.3653(17) Å, α = 94.309(2)°, β = 91.765(2)°, γ = 93.892(2)°, D _calc = 1.298 g/m³ for Z = 1. Within the unit cell, six methanol molecules of crystallization plus one molecule of pyrazine were found to accompany the pyrogallol macrocycle. In the solid state, the macrocycle is found to adopt the chair conformation.     

Crystal structure of [bis 1,2-(diphenylphosphino)ethane]-bis(pyridine-2-thiolato)ruthenium(II)

The Ru atom in the title compound, [Ru(dppe)(2-pyS)₂] exists in a distorted octahedral geometry defined by a dppe ligand and two 2-pyS anions which function as bidentate ligands via their N- and S-atoms. Important interatomic parameters are Ru-P2.240(3), 2.256(3); Ru-N 2.131(8), 2.136(8); Ru-S 2.413(3), 2.428(3) Å; P-Ru-P 84.1(1), S-Ru-S 155.0(1) and N-Ru-N 87.5(3)°. Crystals are monoclinic, space groupP2₁/c, with unit cell dimensionsa=10.342(1),b=31.145(6),c=11.107(2) Å,=113.80(1)° andZ=4. The structure was refined to finalR=0.064 for 3057 reflections withI2.5(I).