Yan-Jun Hou

4-Meth-oxy-2-nitro-4'-(trifluoro-meth-yl)biphen-yl.

The title compound, C14H10F3NO3, was prepared by a palladium-catalysed Suzuki–Miyaura coupling reaction. The dihedral angle between the nitro group and its parent benzene ring is 66.85 (19)° while the dihedral angle between the two benzene rings is 49.98 (9)°. The CF3 group is disordered over two sets of sites with occupancies of 0.457 (8) and 0.543 (8).

1,4-Bis[(1H-pyrazol-1-yl)meth-yl]benzene dihydrate.

The asymmetric unit of the title compound, C14H14N4·2H2O consists of two half-molecules of the main molecule, each situated on an inversion center, and two molecules of water. One-dimensional chains of water molecules are built up by O—H⋯O hydrogen bonds which are then linked with the main molecule via O—H⋯N hydrogen bonds, forming a two-dimensional supramolecular network in the ac plane.

3,4-Dimeth-oxy-4'-nitro-1,1'-biphen-yl.

The title compound, C14H13NO4, was prepared through a palladium-catalysed Suzuki–Miyaura coupling reaction. The asymmetric unit comprises two molecules related by pseudo-inversion symmetry. The dihedral angles between the benzene rings in the two molecules are 44.30 (6) and 48.50 (6)° while those between the benzene ring and the nitro group are 6.54 (13) and 5.73 (10)°. The crystal packing is defined only by Van der Waals interactions.

3a,11b-Dihy­droxy-3a,11b-dihydro-1H-imidazo[4,5-f][1,10]phenanthroline-2(3H)-thione

The title compound, C13H10N4O2S, was prepared through a cyclization reaction of 1,10-phenanthroline-5,6-dione and thiourea. The dihedral angle between the pyridine rings is 8.22 (2)°. In the crystal, molecules are connected by N—H⋯O, O—H⋯N, N—H⋯S and O—H⋯S hydrogen bonds, forming a three-dimensional network.

2,9,10-Trimeth-oxy-dibenzo[b,d]oxepin-7(6H)-one.

The title compound, C17H16O5, was prepared through a cyclization reaction of 2-(3′,4′,5-trimethoxybiphenyl-2-yloxy)acetyl chloride. The two benzene rings form a dihedral angle of 34.55 (5)°. The crystal structure does not feature any hydrogen bonds.

Crystal structure of 3-hydroxy-2-(4-(methylsulfonyl)-2- nitrobenzoyl)cyclohex-2-enone, C14H13NO7S

C14H13NO7S, monoclinic, P121/c1 (no. 14), a = 10.440(1) Å, b = 11.537(1) Å, c = 12.346(1) Å, ) = 95.115(1)°, V = 1481.1 Å, Z = 4, Rgt(F) = 0.046, wRref(F ) = 0.138, T = 273 K. Source of material To a solution of cyclohexane-1,3-dione (10 mmol) and anhydrous ZnCl2 (12 mmol) in anhydrous toluene (50 ml) was added 4methylsulfonyl-2-nitrobenzoyl cyanide (12 mmol). After stirring the reaction mixture for 5 h at room temperature, the solvent was poured into 2 N HCl. The organic phase was washed with 5 % Na2CO3 and acidified with HCl, extracted with methylene chloride, concentrated and the residue was recrystallized from methanol to give the title compound in a yield of 60 % [1]. Crystals suitable for single crystal X-ray diffraction were obtained by slow evaporation of a solution in methanol at room temperature in a yield of 43 %. Experimental details All H atoms were placed in idealized positions [d(C—H) = 0.96 (methyl), 0.97 (methylene) and 0.93 Å (aromatic)] and included in the refinement in the riding model approximation, with Uiso(H) = 1.5 Ueq(Cmethyl) and 1.2 Ueq(Cmethylene,aromatic). Discussion The title compound is used as herbicide with a trade name ‘mesotrione’. The herbicide mesotrione inhibits a critical enzyme, phytoene desaturase, in plant carotenoid biosynthesis [2]. All bond lengths and angles in the title molecule are normal. The cyclohexene ring has the twist conformation. The dihedral angle between C1/C2/C3/C5/C6 plane and C3/C4/C5 plane is 42.9(3)°. The dihedral angle between the nitro group and benzene ring is 15.6(3)°. The crystal structure features intramolecular O–H···O and intermolecular O–H···O, C–H···O hydrogen bonds, leading to the formation of a 3D framework. Z. Kristallogr. NCS 225 (2010) 465-466 / DOI 10.1524/ncrs.2010.0204 465

Methyl 4-methyl­sulfonyl-2-nitro­benzoate

The title compound, C9H9NO6S, was prepared by the reaction of methanol and thionyl chloride with 4-methylsulfonyl-2-nitrobenzoic acid under mild conditions. The dihedral angle between the nitro group and benzene ring is 21.33 (19)° and that between the carboxylate group and the benzene ring is 72.09 (17)°. The crystal structure is stabilized by weak intermolecular bifurcated C—H⋯O interactions occurring in the (100) plane.

Ethyl N-[3-(N,N-dimethyl­carbamo­yl)pyridin-2-ylsulfon­yl]carbamate

In the molecular structure of the title compound, C11H15N3O5S, the amide group is nearly perpendicular to the pyridine ring, making a dihedral angle of 86.30 (13)°. The terminal ethyl group is disordered over two sites of equal occupancy. Intermolecular N—H⋯O hydrogen bonding is present in the crystal structure.

Poly[[[diaqua­cobalt(II)]-bis­[μ2-1,1′-(butane-1,4-di­yl)diimidazole-κ2N3:N3′]] dichloride tetra­hydrate]

In the title compound, {[Co(C10H14N4)2(H2O)2]Cl2·4H2O}n, the CoII atom and the mid-point of the 1,1′-butane-1,4-diyldiimidazole ligands lie on inversion centers. The CoII atom is six-coordinated in a slightly distorted octahedral environment by four N atoms from four different ligands and by two O atoms from the water molecules. The CoII atoms are bridged by the ligands into a (4,4) net. Adjacent nets are linked to the chloride anions and uncoordinated water molecules via O—H⋯Cl and O—H⋯O hydrogen bonds, generating a three-dimensional supramolecular structure.

CCDC 624206: Experimental Crystal Structure Determination

Related Article: Jin-Sheng Gao, Guang-Feng Hou, Ying-Hui Yu, Yan-Jun Hou, Guang-Ming Li|2006|Acta Crystallogr.,Sect.E:Struct.Rep.Online|62|m2685|doi:10.1107/S1600536806037767