Structural Determination And Analysis Of Some New Schiff Base And Triangulo-Triruthenium Compounds

Eight Schiff base compounds were studied in this research. They crystallized out in the common space groups, i.e. four compounds are in monoclinic C2/c, and one each in monoclinic Cc, P21 and Pn and triclinic1P. One Schiff base compound exists in a zwitterion form. The structures of two Schiff base compounds are disordered. One Schiff base compound is a racemic twin crystal. Water solvent exists in the asymmetric unit of two Schiff base compounds. The Schiff base compounds all exist in an E configuration with respect to the N=C. The average N=C double bond value is 1.282 Å

5,5′-Dimeth­oxy-2,2′-[2,2-dimethyl­propane-1,3-diylbis(nitrilo­methyl­idyne)]diphenol

The asymmetric unit of the title Schiff base compound, C21H26N2O4, consists of four crystallographically independent mol­ecules, viz. A, B, C and D. The A and D, and the B and C mol­ecules are related by a pseudo-inversion centre, and the remaining pairs of mol­ecules differ in the orientations of one of the meth­oxy groups. In each independent mol­ecule, intra­molecular O—H⋯N hydrogen bonds generate two S(6) ring motifs. The dihedral angles between the benzene rings in mol­ecules A, B, C and D are 65.86 (19), 50.41 (19), 68.59 (19) and 50.85 (19)°, respectively. In the crystal structure, mol­ecules are linked by C—H⋯O hydrogen bonds, forming R 2 2(8) dimers. In addition, weak C—H⋯π inter­actions are observed

Ethyl 4-(2,4-difluoro­phen­yl)-6-methyl-2-oxo-1,2,3,4-tetra­hydro­pyrimidine-5-carboxyl­ate

In the title compound, C14H14F2N2O3, the dihydro­pyrimidin­one ring adopts a flattened boat conformation. The difluoro­phenyl group is disordered over two orientations with occupancies of 0.544 (3) and 0.456 (3). The methoxy­carbonyl group is disordered over two positions with occupancies of 0.580 (8) and 0.420 (8). In the crystal, mol­ecules are linked into centrosymmetric dimers by paired N—H⋯O hydrogen bonds and the dimers are linked into a ribbon-like structure along [100] by further N—H⋯O hydrogen bonds

N′-[(E)-4-Chloro­benzyl­idene]-2-(4-isobutyl­phen­yl)propanohydrazide

The asymmetric unit of title compound, C20H23ClN2O, consists of two crystallographically independent mol­ecules (A and B) in which the orientations of the 4-isobutyl­phenyl units are different. The isobutyl group of mol­ecule B is disordered over two positions with occupancies of 0.850 (5) and 0.150 (5). The dihedral angle between the two benzene rings is 88.70 (9)° in mol­ecule A and 89.38 (9)° in mol­ecule B. The independent mol­ecules are linked together into chains along [100] by N—H⋯O and C—H⋯O hydrogen bonds, and by C—H⋯π inter­actions. In the chain, N—H⋯O and C—H⋯O hydrogen bonds generate R 2 1(6) ring motifs. In addition, C—H⋯N hydrogen bonds are observed. The presence of pseudosymmetry in the structure suggests the higher symmetry space group Pbca but attempts to refine the structure in this space group resulted in high R (0.119) and wR (0.296) values

Ferrocene-1-carbaldehyde 4-ethyl­thio­semi­carbazone

The asymmetric unit of title compound, [Fe(C5H5)(C9H12N3S)], contains two crystallographically independent mol­ecules, A and B. The two cyclo­penta­dienyl (Cp) rings are parallel to each other in both mol­ecules, forming dihedral angles of 2.3 (3) and 1.0 (3)°, respectively, and adopt an eclipsed conformation. The mean plane of the semicarbazone group is twisted slightly away from the attached Cp ring in both mol­ecules, the dihedral angles between the mean plane and the Cp ring being 15.3 (2) and 10.8 (2)°. The ethyl group in mol­ecule A is coplanar with the mean plane of the semicarbazone group [C—N—C—C torsion angle = −175.2 (4)°], whereas it is nearly perpendicular in mol­ecule B [C—N—C—C torsion angle = 84.8 (6)°]. In the crystal structure, inter­molecular N—H⋯S hydrogen bonds link the mol­ecules into dimers. These dimers are further linked into chains via inter­molecular C—H⋯S hydrogen bonds. The crystal studied was a non-merohedral twin with a refined ratio of the twin components of 0.265 (2):0.735 (2)

Undeca­carbonyl-1κ3 C,2κ4 C,3κ4 C-[tris­(4-methyl­phen­yl)arsine-1κAs]-triangulo-triruthenium(0)

In the title triangulo-triruthenium compound, [Ru3(C21H21As)(CO)11], one equatorial carbonyl group has been substituted by the monodentate arsine ligand, leaving one equatorial and two axial carbonyl substituents on the Ru atom. The remaining two Ru atoms each carry two equatorial and two axial terminal carbonyl ligands. The three arsine-substituted phenyl rings make dihedral angles of 73.2 (2), 71.0 (2) and 75.3 (2)° with each other. In the crystal packing, mol­ecules are stacked down the b axis and each mol­ecule is stabilized by an intra­molecular C—H⋯O hydrogen bond

6-Chloro-3-[5-(3-meth­oxy-8-methyl-4-quinol­yl)-1-phenyl-4,5-dihydro-1H-pyrazol-3-yl]-2-methyl-4-phenyl­quinoline

In the title compound, C36H29ClN4O, the dihydro­pyrazole ring adopts an envelope conformation. The two quinoline ring systems (r.m.s. deviations = 0.029 and 0.018 Å) are oriented at a dihedral angle of 71.43 (4)°. One of the quinoline rings makes a dihedral angle of 65.40 (7)° with the phenyl substituent. In the crystal, mol­ecules are linked into chains along the b axis by inter­molecular C—H⋯N hydrogen bonds. In addition, C—H⋯π and π–π [centroid–centroid distance = 3.7325 (8) Å] inter­actions are observed

(Benzyl­diphenyl­phosphine-3κP)[μ-bis(diphenyl­arsino)methane-1:2κ2 As:As′]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-triangulo-triruthenium(0)

The asymmetric unit of the title triangulo-triruthenium compound, [Ru3(C25H22As2)(C19H17P)(CO)9], consists of two crystallographically independent mol­ecules of the triangulo-triruthenium complex, A and B. The bis­(diphenyl­arsino)methane ligand bridges an Ru—Ru bond and the monodentate phosphine ligand bonds to the third Ru atom. Both the phosphine and arsine ligands are equatorial with respect to the Ru3 triangle. In addition, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. With regard to the three phosphine-substituted rings, the benzyl ring makes dihedral angles of 41.0 (3) and 43.9 (3)° with the other two benzene rings in mol­ecule A; these angles are 49.8 (3) and 56.8 (3)° in mol­ecule B. The dihedral angles between the two benzene rings are 76.1 (3) and 88.2 (3)° for the two diphenyl­arsino groups in mol­ecule A and 71.3 (3) and 78.1 (3)° in mol­ecule B. In the crystal packing, mol­ecules are linked into chains via inter­molecular C—H⋯O hydrogen bonds. Weak inter­molecular C—H⋯π inter­actions further stabilize the crystal structure

μ-Bis(diphenyl­arsino)methane-1:2κ2 As:As-nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-[(2-methoxy­phen­yl)diphenyl­phosphino-3κP]-triangulo-triruthenium(0)

In the title triangulo-triruthenium compound, [Ru3(C25H22As2)(C19H17OP)(CO)9], the bis­(diphenyl­arsino)methane ligand bridges a Ru—Ru bond and the monodentate phosphine ligand bonds to the third Ru atom. Both the phosphine and arsine ligands are equatorial with respect to the Ru3 triangle. Additionally, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three phosphine substituted phenyl rings make dihedral angles of 74.34 (12), 68.34 (12) and 85.45 (11)° with each other. The dihedral angles between the two phenyl rings are 87.56 (11) and 60.56 (11)° for the two diphenyl­arsino groups. In the crystal packing, the mol­ecules are linked together into chains via inter­molecular C—H⋯O hydrogen bonds down the a axis. Weak inter­molecular C—H⋯π inter­actions further stabilize the crystal structure

Bis(1-ferrocenylmethyl­idene-4-phenyl­thiosemicarbazidato-κ2 N 1,S)zinc(II) monohydrate

In the title compound, [Fe2Zn(C5H5)2(C13H11N3S)2]·H2O, the ZnII ion is in a distorted tetra­hedral geometry being coordinated by two thio­semicarbazone ligands via N and S atoms. One of the Cp rings is disordered over two positions with occupancies of 0.55 and 0.45. The dihedral angle between the substituted Cp rings is 56.1 (5)° and the two phenyl rings are orientated at a dihedral angle of 41.7 (4)°. In the crystal structure, inter­molecular O—H⋯S, N—H⋯O and C—H⋯N hydrogen bonds link the mol­ecules into chains along the b axis. The structure is further consolidated by O—H⋯π inter­actions