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 trichloro (π-cis-but-2-en- 1,4-diammonium) platinum(II) chloride and trichloro(π-cis-pent-2-enylammonium) platinum(II)

The structures of the olefinic complexes of platinum(II) withcis-but-2-en-1,4-diammonium, [PtCl₃(C₄H₁₂N₂)]⁺, and withcis-pent-2-enylammonium, [PtCl₃(C₅H₁₂N)], the first one as its chloride, have been determined by single-crystal X-ray methods. The compounds form yellow monoclinic crystals, witha=11.238(3),b=12.234(4),c=7.769(1) Å, = 112.99(2) ° anda= 11.530(3),b=9.037(3),c= 10.067(3) Å, =105.50(2) °, respectively; both crystallize in the space groupP2₁/c withZ=4. The structures, solved by standard methods, have been refined anisotropically by full-matrix least-squares methods, both toR=0.040, on, respectively, 1808 and 1849 independent reflections collected by counter methods.In both complexes, platinum is four-coordinate to the three chlorine atoms and the double bond of the olefinic ligand. The structures are discussed, and comparison with the analogous platinum(II)-olefin complexes with the trans isomers of the olefinic ligands is made.     

Crystal and molecular structures of dimethyl 4-phenylthiosemicarbazidediacetate and its adduct with rhodium(II) acetate

The crystal structures of dimethyl 4-phenylthiosemicarbazidediacetate C₁₃H₁₇N₃O₄S (I) and its adduct [C₈H₁₂O₈Rh₂ (C₁₃H₁₇N₃O₄S)₂] (II) with rhodium(II) acetate are determined by X-ray diffraction analysis. The unit cell parameters of crystals I are as follows: a = 8.066(6) Å, b = 15.812(6) Å, c = 24.977(8) Å, β = 94.88(3)°, space group P2₁/n, and Z = 8. The unit cell parameters of crystals II are a = 8.513(1) Å, b = 16.055(1) Å, c = 16.071(3) Å, β = 104.99(1)°, space group P2₁/c, and Z = 2. In structure I, two crystallographically independent molecules considerably differ from each other in the mutual orientation of the structural fragments containing the ester groups. In the centrosymmetric dimeric complex II, the organic molecule I acts as a monodentate thio ligand and adopts only one conformation.     

Crystal and molecular structure of tetrakis(N,N′-dimethylthiourea)platinum(II)chloride

The crystal and molecular structure of tetrakis(N,N-dimethylthiourea) platinum(II) chloride has been solved and refined by least-squares methods to a finalR of 0.052 from 4145 reflections measured by counter techniques. The crystals are triclinic:P¯1,a = 10.06(1),b = 10.19(2),c = 14.06(2) Å, = 89.7(1), = 101.4(1), = 90.1(1) °,Z = 2,D _m = 1.76,D _c = 1.605 g cm^–3. The structure consists of discrete Pt[SC(NHCH₃)₂] ₄ ²⁺ and Cl^– ions, linked by a network of NH^...Cl hydrogen bonds. The dimethylthiourea groups are bonded to the metal through sulfur with Pt-S bonds of 2.305(2) and 2.321(2) Å. The PtS₄ is almost square planar with 0.24 Å displacement of Pt from the best plane of the sulfur atoms. The entire cation has an approximateC ₄ symmetry. The shortest Pt^...Cl distance is 3.677(2) Å.     

Crystal and molecular structure ofpp-diphenyl-p-tetrakis (perfluoromethyl)ethylene glycol phosphinate

The title compound crystallizes in space groupP¯1 (No. 2) witha=8.796(6),b=10.754(3),c=12.271(2) Å,=68.56(2),=67.68(3),=78.87(4)°, andZ=2. The structure was solved by direct methods and refined by full-matrix least squares toR=0.048. In the tetrahedral geometry around phosphorus, the P-O(22) bond of 1.464(2) Å is shorter than expected. The OO hydrogen bond results in dimer formation, and the substituted glycol shows staggered conformation along the C(12)-C(3) vector.     

Crystal structure ofcis-bis[1-(2-thienyl)-4, 4,4-trifluoro-1,3-butanedionato]-bis (4-methylpyridine)nickel(II)

The crystal structure of the 4-methylpyridine adduct of bis[1-(2-thienyl)-4, 4,4-trifluoro-1,3-butanedionatolnickel(II) was determined by a three-dimensional x-ray analysis using counter data. The crystals are monoclinic,C2/c, witha = 9.330,b = 18.278,c = 17.855 Å, and = 95.1°. The structure was refined by full-matrix least squares toR = 0.10. The molecule has a two-fold axis, and both enantiomers withcis configuration occur in the crystal. The solvation by 4-methylpyridine is shown to weaken the chelate bonds in the same way as doestrans hydration.     

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 structure of bis(2,3,5-trimethylpyridine N-oxide) 2,4,6-trinitrophenolate: Cation complex tied by the extremely strong OHO hydrogen bonding

The salt of bis(2,3,5-trimethylpyridine N-oxide) 2,4,6-trinitrophenolate, C₂₂H₂₅N₅O₉, crystallizes in monoclinic space group C2/c with a=12.411(2)Å, b=15.326(3)Å, c=13.559(3)Å, =113.13(1)°, V=2371.8(8)ų, Z=4, D _c=1.410 mg/m³, F(000)=1056. The molecule of 2,3,5-trimethylpyridine N-oxide is protonated. Two pyridine N-oxide molecules are linked by extremely strong OHO hydrogen bonding (2.378(4)Å) to form a cation complex. CHO hydrogen bonding and – interactions also play important role in stablizing the structure of the salt.     

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 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 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 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 structure of di-μ-methoxo-bis(chloro-2-methylpyridine copper(II))

The crystal structure of di--methoxo-bis(chloro-2-methylpyridine copper(II)), [CuCl(OCH₃)-(2-mepy)]₂, has been determined from three-dimensional, photographically recorded X-ray data. The unit cell is monoclinic, space groupP2₁/c, with dimensionsa = 8·79,b = 6·01,c = 17·59 Å, = 104·4° and contains two centrosymmetric dimeric units [CuCl(OCH₃). (2-mepy)]₂, in which the copper atoms are linked by methoxide oxygen bridges, the dimers being joined into infinite chains through long copper-chlorine bonds. The environment of each copper atom may be described as a distorted tetragonal pyramid with one chlorine, one nitrogen and two oxygen atoms in the base and a chlorine atom from an adjacent dimer at the apex.     

Crystal and molecular structure oftrans-ammonium-tetrachlorobis(4-methylpyridine) tungstate(III) tetrahydrate,NH4[WC14(C6H7N)2] ·4H2O

Trans-NH₄[WCl₄(C₆H₇N)₂]·4H₂O crystallizes from a solution oftrans-(C₆H₇NH) [WC1₄(C₆H₇N)₂] in aqueous ammonia. The compound is air sensitive and thermally unstable; space groupI4₁/amd (No. 141),a=18.215(5),c=14.160(3) Å, andZ=8. The structure was solved by the heavy-atom method and refined by least squares toR andR _w of 0.052 and 0.053, respectively. The unit cell contains two almost unrelated parts: the NH ₄ ⁺ and WC1₄(C₆H₇N) ₂ ^– are linked by electrostatic and hydrogen bonds, and the rest of the unit cell is filled with the four isolated (H₂O)₈ clusters ofD _2d symmetry. The O-O distances within the cluster are 2.72(2) and 2.86(2) Å; the anion is located on a symmetry center (C _2h symmetry). The W-C1 and W-N(4-methylpyridine) bonds are 2.427(6), 2.446(6), and 2.168(15) Å.     

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 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.