Crystal and molecular structures oftrans-dichloro-(ethylene) (4-methylpyridine)platinum(II) andtrans-dichloro(ethylene) (2,4,6-trimethylpyridine)platinum(II)

The crystal and molecular structures oftrans-[PtCl₂(C₂H₄)(4-MeC₅H₄N)] (I) andtrans-[PtCl₂(C₂H₄)(2,4,6-Me₃C₅H₂N)] (II) have been determined by single-crystal x-ray methods.I crystallizes in space groupP2₁/c witha= 4.991(1), b=21.658(3), c=10.675(3) Å, =110.17(2) °,Z=4;II is orthorhombic (Pbca) witha=10.295(6),b=12.393(8),c=20.370(10) Å,Z=8.Full-matrix least-squares refinements have given finalR factors of 0.053 (1520 reflections) forI and 0.042. (1412 reflections) forII. The intensities were recorded by counter methods, and only those reflections havingI>3(I) were used in the analyses.In both complexes, platinum is four-coordinate with the two chlorine atoms, the double bond of the ethylene, and the nitrogen atom of the substituted pyridine. The two structures are discussed in terms of the arrangement of the pyridine ligand with respect to the PtCl₂(C₂H₄) moiety.     

Crystal and molecular structure of trichloro(1-methylpent-4-enylammonium)platinum(II)

The crystal structure of the olefinic complex of platinum(II) with 1-methylpent-4-enylammonium has been determined from single crystal X-ray data and refined by least-squares methods toR=0.049. The monoclinic crystals have unit cell dimensionsa=11.500(4),b=6.088(4),c=18.961(5) Å,=116.92(4)°, space groupP2₁/c, andZ=4. In the zwitterionic complex the platinum atom is square-planar coordinated by the three chlorine atoms and by the double bond of the unsaturated ammonium cation.Deceased.     

Crystal and molecular structures of two polymorphs of 4-methyl-2-nitroacetanilide (MNA)

Journal of Chemical Crystallography - The crystal and molecular structure of white (MNA-1) and yellow (MNA-3) forms of 4-methyl-2-nitroacetanilide have been determined by X-ray diffraction...     

Crystal structures of copper(II) compounds with racemic threonine

Crystals structures of two modifications of the copper(II) compound with racemic threonine Cu(D-Tre)(L-Tre) are determined by the electron diffraction technique. The unit cell parameters, space group, and number of formula units per unit cell for the crystals of two modifications are as follows: a = 11.10(3) Å b = 9.56(2) Å, c = 5.11(2) Å, γ = 92.6(2)°, space group P2₁/b, and Z = 2 (I); and a = 22.20(3) Å, b = 9.56(2) Å, c = 5.11(2) Å, γ = 92.6(2)°, space group C2₁/b, and Z = 4 (II). The structures are polytypic modifications of the same compound.     

Crystal and molecular structure of the ethanol adduct of tris(oxinato)indium(III)

The ethanol adduct of tris(oxinato)indium(III), prepared in aqueous ethanol, crystallizes in the monoclinic space groupP2₁/n (Nr.14) witha=11.343(2),b=13.477(3),c=16.845(2)Å, -94.71(1)°,V=2566.4(8)ų andZ=4. The structure was solved by direct methods and refined by full-matrix least-squares methods toR=0.032 for 3374 observed reflections withI>2 (I). Three bidentate oxinato ligands (or 8-quinolinolato) coordinate to indium atom leading to an approximately octahedral coordination of the metal(III) ion. One ethanol molecule per mole of metal complex is occluded in the crystal lattice and forms a hydrogen bond with the O(3) oxygen atom of one oxinato ligand [O(3) ... O(4) =2.715(3) Å]. The two other oxinato ligands of the same unit are not involved in hydrogen bonding.     

Crystal and molecular structures of trans-bis(acetonitrile)bis(bipyridine)ruthenium(II) perchlorate and trans-diamminebis(bipyridine)ruthenium(II) perchlorate

The structures of trans-[(MeCN)₂(bpy)₂Ru](ClO₄)₂(I) andtrans-[(NH₃)₂(bpy)₂Ru](ClO₄)₂(II) have been determined by single crystal X-ray diffraction methods. (I) forms monoclinic crystals in the space groupP2₁/c witha=8.399(2),b=10.406(2),c=15.590(3) Å,=93.78(2)° andZ=2 atT=293 K. The final refinement gaveR=0.040 for 2448 reflections withF _o ² >3(F _o ² ). (II) crystallizes in the triclinic space groupP¯1 witha=1.702(1),b=8.439(2),c=10.525(2) Å,=107.56(2),=104.63(1), =100.89(2)° andZ=1 atT=293 K. Refinement using 1878 reflections withF _o ² >3(F _o ² ) produced a finalR value of 0.036. Both of these structures have the ruthenium atom located on a crystallographic inversion center. The bipyridine ligands in both structures are in the bowed conformation as a means of circumventing the steric problems associated with the trans arrangement of the bipyridine ligands. The Ru-N(monodentate) distance is longer for the ammonia complex (2.106(3) Å) than for the acetonitrile complex (2.008(4) Å); there are no significant differences in the distances and angles of the two Ru(bpy)₂ frameworks.     

Crystal and molecular structures of the orthorhombic and monoclinic isomers of catena-di-μ-chloro-semicarbazidecopper(II)

The crystal structures of two isomeric complex compounds of formula [Cu(Cl)₂(NH₂NHCONH₂)] have been determined by X-ray diffraction methods. The orthorhombic isomer has space groupPna2₁ and unit cell constants:a = 6·91(1),b = 8·30(1),c = 10·24(1) Å;Z = 4. The monoclinic isomer has space groupP2₁/c and unit cell constants:a = 6·91(1),b = 8·30(1),c = 11·32(1) Å, = 117·1(2)°;Z = 4. In both complexes coordination around copper is octahedral, with chains of coordination polyhedra along [100]. In the monoclinic compound, the two semicarbazide molecules, which are present in two adjacent octahedra along the chain, have the oxygen and nitrogen atoms in thetrans configuration, one with respect to the other, and are correlated by a centre of symmetry. In the orthorhombic compound, the two semicarbazide molecules are in thecis configuration and there is no centre of symmetry. In both compounds packing is determined by the NH···Cl and NH···O hydrogen bonds which join the chains together.The authors are indebted to Mr M. Lanfranchi who prepared the compounds and to Dr A. Immirzi who made abailable his computer programs.     

Crystal structures of isomorphous cadmium(II) and lead(II) oxalate trihydrates

The isomorphous cadmium(II) oxalate trihydrate (I) and lead(II) oxalate trihydrate (II) crystals belong to space groupP¯1 withZ=2. The crystallographic parameters for compoundI are:a=6.006(1),b=6.663(1),c=8.497(1)Å,a=74.76(1),=74.39(1), =80.94(1)°, andR=0.028 for 2643 observed MoK reflections; forII:a=6.008(1),b=6.671(1),c=8.493(1)Å,a=74.70(1),=74.33(1), =80.98(1)°, andR=0.065 for 4536 reflections. In the crystal structure, the metal atom is surrounded by seven oxygen atoms (including two aqua ligands) in the form of a distorted pentagonal bipyramid. The coordination polyhedra are interconnected through bridging oxalate groups to form a thick layer matching the (020) plane. Adjacent layers are further linked by hydrogen bonds involving both ligand and lattice water molecules to generate a three-dimensional network.On leave from Central Laboratory, Nankai University, Tianjin, China.     

Crystal structures of salicylideneguanylhydrazinium chloride and its copper(II) and cobalt(III) chloride complexes

The crystal structures of salicylideneguanylhydrazinium chloride hydrate hemiethanol solvate (I), salicylideneguanylhydrazinium trichloroaquacuprate(II) (II), and bis(salicylideneguanylhydrazino)cobalt(III) chloride trihydrate (III) are determined using X-ray diffraction. The structures of compounds I, II, and III are solved by direct methods and refined using the least-squares procedure in the anisotropic approximation for the non-hydrogen atoms to the final factors R = 0.0597, 0.0212, and 0.0283, respectively. In the structure of compound I, the monoprotonated molecules and chlorine ions linked by hydrogen bonds form layers aligned parallel to the (010) plane. In the structure of compound II, the salicylaldehyde guanylhydrazone cations and polymer chains consisting of trichloroaquacuprate(II) anions are joined by an extended three-dimensional network of hydrogen bonds. In the structure of compound III, the [Co(LH)₂]⁺ cations, chloride ions, and molecules of crystallization water are linked together by a similar network.     

Crystal and molecular structure of tetrapyridyl-copper(II)-bis-nitrato-bis-pyridine

The crystal and molecular structure of a pyridine complex of anhydrous copper(II)nitrate is described. The structure has been solved by vector search methods and refined by least-squares methods to R₁=0.049 [I>2(I)]. The complex lies on a twofold axis parallel toa, and two solvent pyridine molecules lie on twofold axes parallel toc. The copper atom is coordinated by four pyridyl groups and two monodentate NO₃ groups. Crystal data: C₃₀H₃₀N₈O₆Cu, orthorhombic, space group Pnna(52),a=14.446(7),b=12.154(5),c=16.881(4) Å,V=2964(2) ų,Z=4.     

Crystal and molecular structure oftrans-dichlorobis(oxazole)palladium(II)

The crystal and molecular structure oftrans-dichlorobis(oxazole)palladium-(II), Pd(C₃H₃ON)₂Cl₂, has been determined by single-crystal X-ray diffraction techniques using counter methods and has been refined by full-matrix least-squares procedures to a finalR index of 0.022. The complex crystallizes in the triclinic space groupP¯1 with unit cell dimensions ofa = 6.957(1),b = 7.506(1),c = 5.538(1) Å, = 109.22(1), = 91.37(1), and = 115.09(1) °, withZ = 1. The palladium(II) ion, located at an inversion center, is coordinated in a regular square-planar manner to two chloride ions at 2.293(1) Å and, at 2.016(2) Å, to the nitrogen atoms of two oxazole ligands. The planar oxazole rings are tilted 33 ° with respect to the PdN₂Cl₂ plane. Further verification of the presence of oxazole in the complex was obtained by high-resolution mass spectrometry. Crystals of Pd(C₃H₃ON)₂Cl₂ resulted irreproducibly from attempts to prepare single crystals of a previously reported dimeric palladium(II) disulfide complex by treating Pd(CH₃CN)₂Cl₂ with a slight excess of diphenyl disulfide in benzene in the atmosphere. The source of the oxazole is not understood.     

Crystal and molecular structure oftrans-dichlorobis(N-propylimidazole)palladium(II)

The crystal structure of Pd(N-PropIm)₂Cl₂ has been determined from X-ray data collected by counter methods. The compound crystallizes in the monoclinic space groupP2₁/n with four molecules per unit cell, the dimensions of which area=14.554(5),b=8.204(2),c=14.860(3) Å,=115.63(2)°. Full-matrix least-squares refinement gave a final R value of 0.0263 for 1913 independent observed reflections. The Pd atom is four-coordinated and is surrounded in atrans square planar fashion by two N atoms of the imidazole groups and by two Cl ions.     

Crystal structures of bis(4-dimethylaminopyridinium) tetrachlorocobaltate(II) and bis-[1,3-di (ammoniummethyl)benzene]tetrachlorocobaltate(II)

The crystal structures consist of organoammonium cations hydrogen bonded to tetrahedral CoCl₄ ^2– anions. In the 4-dimethylaminopyridinium salt, [(CH₃)₂NC₅H₅NH]₂CoCl₄, pairs of cations hydrogen bond in an asymmetric fashion to two of the chlorines in each anion. The planar cations form two sets of – stacks, first parallel to the a axis and the second parallel to the b axis. The anions lie between these two nonintersecting sets of stacks. In contrast, for the second compound, [C₆H₄(CH₂NH₃)₂]CoCl₄, the tetrahedral CoCl₄ ^2– anions form layers lying parallel to the bc plane. The 1,3-di(ammoniummethyl)benzene cations crosslink adjacent anionic layers, forming a lamellar structure of alternating organic and inorganic layers.     

Crystal and molecular structure of bis(aminomethylphosphonate)copper(II)

The crystal and molecular structure of bis(aminomethylphosphonate)-copper(II), C₂H₁₀N₂O₆P₂Cu, has been determined from MoK diffractometer data. The compound crystallizes in the monoclinic space groupP2₁/n witha =7.571(2),b = 4.943(1),c = 11.212(3) Å, = 105.84(2) °, andZ = 2. The structure was solved by the heavy-atom technique and refined by full-matrix least-squares methods toR = 0.041, using 1084 reflections for which ¦F _o¦ > 3.92 (¦F _o¦). In this complex, the Cu atom is square-planar coordinated by four O atoms from four phosphonic groups, and not by the amino group. The Cu-O bond lengths are 1.928(3) and 1.937(3) Å, and the phosphonic groups bridge adjacent Cu atoms in polymeric chains. The infrared spectrum of this complex is reported.     

Crystal and molecular structure of dibromobis(benzimidazole)copper(II)

The reaction of CuBr₂ with benzimidazole and HBr in aqueous solution leads to the formation of Cu(C₇H₆N₂)₂Br₂ as dark-brown, stable monoclinic crystals. Space groupP2₁/c witha=13.794(5),b=7.875(2),c=14.510(6) Å;=105.82(5)°;V _c =1516(5) ų;D _x =2.010(3) Mg m^–3. The structure was refined by a full-matrix least-squares procedure to giveR=R _w =0.045 for 1932 intensities above 3(I). The copper (II) ions are four coordinates in the form of a distorted flattened tetrahedron CuN₂Br₂, with the bond lengths Cu-Br(1)=2.402(1), Cu-Br(2)=2.446(1), Cu-N(1)=1.976(7), and Cu-N(11)=1.946(7) Å. The flattened angles are Br-Cu-Br=139.0(1) and N-Cu-N=154.6(3)°. The geometry of intermolecular and intramolecular hydrogen bonds is discussed.     

Crystal structures of three methylmercury(II) complexes with thiazolidine-2-thione

The crystal structures of three CH₃Hg⁺ complexes with 1,3-thiazolidine-2-thione (HT) are reported. The cationic [(CH₃Hg)HT]NO₃ complex is monoclinic, space group P2₁/c,a=7.158(14),b=10.156(7),c=13.472(12) Å,=108.21(4)°,Z=4. The structure was refined toR=0.045. The [(CH₃Hg)HT]⁺ cation contains a CH₃Hg⁺ group bonded to the exocyclic S atom of the ligand retaining its N-H proton. This proton is lost and the CH₃Hg⁺ group remains bonded to sulfur in the neutral [(CH₃Hg)T] compound (hexagonal, P6₃,a=13.502(8),c=6.984(7) Å,Z=6,R=0.027). The [(CH₃Hg)₂T]NO₃ compound (monoclinic, C2/c,a=25.200(10),b=7.029(6),c=17.946(8),=128.99(3)°,Z=8,R=0.047) contains complex cations in which the CH3Hg⁺ groups are bonded to N and the exocyclic S atom. This series of compounds shows that the exocyclic S atom is always the first target for the CH₃Hg⁺ group, which is also found to bind to nitrogen in the 2:1 compound. No coordination is observed with the endocyclic S site, which does not even participate in intermolecular H-bonding or HgS contacts in the solids.     

Crystal and molecular structures of several tetrakis (nitrile)copper(I) complexes

The crystal structures of several [Cu(RCN)₄]X salts (R = Me, X = SO₃CF₃ ^–; R = Ph, X = BF₄ ^–, ClO₄ ^–, and PF₆ ^–) were determined using single crystal X-ray diffraction. All of the compounds contain distorted tetrahedral Cu(I) centers and noncoordinating anions, with the acetonitrile and benzonitrile structures containing three and one unique CuL₄ ⁺ complex in their respective asymmetric units. One important distortion is observed in the benzonitrile-Cu bonds, which are bent up to 23° away from linearity. The result is a flattened complex that maximizes the – tacking of the aromatic rings and is the dominant packing interactions between the complexes.     

Crystal and molecular structure of nickel(II) dicyanothiosemicarbazide monohydrate

The structure of the title compound (Ni(CN)₂(CH₅N₃S)·H₂O) has been determined, from X-ray diffractometer data, by the heavy-atom method and refined by least-squares. The finalR-values, based on 3109 observed reflections, areR=0.035 andR _w =0.039. The complex has square-planar geometry with two adjacent cyano carbon atoms (Ni-C, 1.838(2) Å and 1.862(2) Å)and thiosemicarbazide sulfur and nitrogen atoms (Ni-S, 2.169(1) Å and Ni-N, 1.923(2) Å). The water molecule does not enter the inner coordination sphere of the nickel atom; however, it plays a very important role in the crystal structure. Water is coordinated by hydrogen bonds to four adjacent complex units.