Crystal structure of bis(2,4-pentanedionato)copper(II)

The structure of bis(acetylacetonato)copper(II) has been redetermined from single crystal X-ray diffraction data. The unit cell parameters area=11.331(9),b=4.697(3),c=10.290(9) Å, and=91.84(7)dg. A finalR=0.056 for 727 observed reflections was obtained. The O-Cu-O chelate (bite) angle is 93.2(2)°. The two Cu-O bond lengths are 1.914(4) and 1.912(4) Å. The complex has a slight chair structure and a step angle of 7.05°.     

Crystal structure ofcis-diaqua bis(2,2′-bipyridyl)chromium(III) nitrate, [Cr(bipy)2(H2O)2] (NO3)3

cis-Diaquabis(2,2-bipyridyl)chromium(III) nitrate crystallizes in the mono-clinic system, space groupP2₁/c, witha=16.102(6),b=10.792(5),c=15.076(6) Å,=112.90(5)°, andZ=4. The saltlike structure was determined from X-ray crystallography and refined toR=7.5% for 3342 observed reflections. The Cr atom is octahedrally surrounded by twocis water molecules and by two chelated 2,2-bypiridyl ligands forming two nearly orthogonal planes. Selected bond distances are: Cr-O, 2.00(1) and 1.98(1) Å, Cr-N, 2.04 Å (mean).     

X-ray crystal structure oftrans-dichlorobis(2,4,6-collidine)-copper(II)

The X-ray crystal structure oftrans-dichlorobis(2,4,6-collidine)copper(II) has been determined. Dark blue crystals of the complex crystallize in the monoclinic space group P2₁/c, with cell dimensionsa=7.527(3),b=14.732(4),c=7.951(4)Å and=92.79(9)°;V=880.6(6)ų andZ=2. 949 unique reflections withI _net>3(I) on refinement afforded values ofR=0.041 andR _w =0.048.     

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 structure of hexa(3,5-dicarboxypyridine)potassium tetrabromoaurate(III)

The title complex has been prepared, and characterized by X-ray crystallography. The crystals are rhombohedral, space groupR32, witha=20.954(5),c=9.753(1) Å,Z=3, andR _F =0.070 for 680 observed MoK reflections. The structure consists of a packing of hexa(3,5-dicarboxypyridine) potassium cations and tetrabromoaurate(III) anions. The potassium atom is surrounded by equivalent oxygen atoms to form a KO₆ octahedron with a very short K-O distance of 2.56(1) Å. The AuBr ₄ ^– group exhibits orientational disorder with a mean bond length of 2.38(1) Å. Two symmetric strong hydrogen bonds (linear OHO and bent NHN) are found in the crystal structure. The nearly planar organic ligands are interlinked by hydrogen bonds to form parallel sheets which approximately correspond to the (003) family of planes. The potassium atoms lying in between these sheets connect them into a three-dimensional network.On leave from Central Laboratory, Nankai University, Tianjin, China.     

Structural confirmation of a template reaction mechanism: Structure of dichloro (2,9-dimethyl-3,10-diphenyl-1,4,8,11-tetraazacyclotetradeca-1,3,8,10-tetraene)cobalt(III) hexafluorophosphate

The structure of the title compound has been investigated by X-ray diffraction methods. The crystals are monoclinic, space groupP2₁/c, with unit cell parameters:a=11.394(3),b=6.381(2),c=17.413(4)Å, and=95.72(2)°. The structure was refined with 2369 unique reflections by a full-matrix least squares procedure givingR andR _w of 3.2 and 4.2%, respectively. The cobalt complex forms a six coordinate distorted octahedral structure with the cobalt atom at a center of symmetry. The macrocyclic ligand presents eighteen of its 28 nonhydrogen atoms in a planar array about the cobalt atom. Only the two central trimethylene carbon atoms and four carbon atoms of each phenyl ring deviate by more than ±0.05 Å from this plane. Thetrans arrangement of substituents on the ligand of the complex confirms the structural assignment previously made based on NMR data and lends support to the proposed template reaction mechanism by which these complexes form.     

Crystal and molecular structure of [CpRu(PPh3)2(t-C4H9SH)]BF4

The structure of the [CpRu(PPh₃)₂(t-C₄H₉SH)]BF₄ complex was determined by X-ray diffraction techniques: monoclinic space groupP2₁/c,a=14.662(9),b=18.515(7),c=15.368(6)Å,=101.88(5)°,V=4082(6)ų,Z=4,R=0.049,R _w=0.057. The Ru is attached to two triphenylphosphine ligands, a cyclopentadienyl and thet-butylmercaptan. The Ru-S distance is 2.396(2)Å and the S-H distance is 1.289(2)Å.     

Study on the crystal and molecular structure of triphenyl tin methacrylate: (C6H5)3SnOCOCCH2CH3

The crystal and molecular structure of (C₆H₅)₃SnOCOCCH₂CH₃ has been determined by a single crystal X-ray diffraction study. The crystal is monoclinic with space group P2₁/c,a=11.902(3),b=10.104(4),c=16.721(2) Å,=97.56(1)°,V=1930.4 ų,Z=4 andD _c =1.495 g/ cm³,F(0,0,0)=872,(CuK)=1.5418 Å. The structure was solved by the heavy-atom method and refined by full-matrix least-squares procedures to anR factor of 0.060 based on 2157 independent reflections. The results showed that the Sn-O bond distance is 2.064(4) Å. The average Sn-C bond distance is 2.126 Å. There is a weak coordination through the O of the CO group of the methacrylate residue (Sn-O(2) 2.774(5) Å) except for four normal coordinations. The coordination number at the Sn⁴⁺ is 5.     

The crystal and molecular structure of [K·DB-18-C-6][AlMe3NO3]·0.5C6H6

The use of dibenzo-18-crown-6 in the synthesis of trimethylaluminum adducts of KNO₃ results in the formation of a 1/1 adduct, [K·DB-18-C-6]-[AIMe₃NO₃]. The crystal structure of [K·DB-18-C-6][AlMe₃NO₃]-has been determined from single-crystal X-ray diffraction data collected by counter methods. The title compound crystallizes in the monoclinic space groupP2₁/c (No. 14) with unit cell parametersa=11.804(3),b=28.828(4),c=9.118(3) Å, =96.61(3)°, andD _calc=1.23 forZ=4. Least-squares refinement gave a final conventionalR value of 0.045 for 983 independent observed reflactions. The potassium atom is centered among the six oxygen atoms of the crown at an average KO contact of 2.74(2) Å. Its environment is completed by an oxygen atom of a nitrate anion (2.88 Å) and a benzo group (>3.44 Å) of a neighboring crown ether. The trimethylaluminum moeity is coordinated to the nitrate anion by an oxygen atom at an Al-O bond distance of 1.92(1) Å.     

Crystal and molecular structure of tris-(O-isopropylxanthato)-chromium(III)

The title compound has been synthesized by the reaction of CrCl₃6H₂O with K{S₂COCH(CH₃)₂} in a 13 molar ratio in an aqueous medium. It has been characterized by elemental analysis and IR spectral studies. Crystals of Cr{S₂COCH(CH₃)₂}₃ are monoclinic, space group P2₁/n witha=10.002(2),b=10.973(1),c=18.961(6) Å,=91.78(2)°,V=2079.9 ų,Z=4,D _calc=1.46 g cm^–3, monochromatic radiation (Mo-K), =0.71069 Å,=11.2 cm^–1,F(0 0 0)=948,T=295K, finalR=0.0320 for 2641 reflections. The environment of the chromium atom is based on an octahedral geometry having six sulfur donor atoms from three symmetrically chelated ligands with average distances: Cr-S=2.396(9) Å, C-S=1.690(3) Å and C-O=1.315(3) Å. The bond distance between oxygen atom and the carbon atom of the isopropyl group (O-C_av=1.478(4) Å) suggests that the form –S ₂ ^(–) C=O⁽⁺⁾CH(CH₃)₂ contributes significantly to the structure of the isopropyl group.     

Crystal and molecular structure of 1-(2-isopropylcarbamoylpropan-2-ylamino) 3-(1-naphthyloxy)propan-2-ol (C20H28N2O3)

The crystal structure of the title compound has been determined with three-dimensional MoK X-ray diffraction data. The space group and unit-cell parameters are:P2₁/c,a=8.610(3) Å,b=13.516(5) Å,c=16.818(5) Å,=94.95(3)° andV=1950.0(7) ų. The structure was solved by direct methods, and refined by full-matrix least-squares techniques toR=0.0608 andR _w=0.0648. The compound is a derivative of the popular-adrenolytic propranolol, and in the propanol part of the side chain shows the typicalgauche conformation.     

Crystal and molecular structure of triphenylphosphine (N,N-diethyldithiocarbamato)gold(I)

The crystal and molecular structure of triphenylphosphine (N,N-diethyldithio-carbamato) gold(I), (C₆H₅)₃PAuSSCN(C₂H₅)₂, has been determined by three-dimensional X-ray methods. The compound crystallizes in the monoclinic space groupP2₁/c witha = 13·547(1),b = 12·277(1),c = 14·013(1) Å, = 90·81(1) ° andZ = 4. Three-dimensional intensity data were collected on an automatic diffracto-meter. Atomic parameters were refined by full-matrix least-squares methods to a conventionalR value of 0·04 for 2318 non-zero observed reflexions.In this complex the diethyldithiocarbamate moiety acts as a monodentate ligand, the double-bond distance being 1·68(1) Å and the bond involving the sulphur atom that is coordinated to the gold atom being 1·75(1) Å. The gold atom is linearly coordinated, the angle being 175·7(1) ° and the and distances being 2·338(3) and 2·251(3) Å, respectively.     

Synthesis and structure of bisiodobis(diisopropyldithiocarbamato)tellurium(IV)

The title mixed ligand complex was synthesized by the controlled oxidative displacement reaction of TeL ₄ by iodine (L is diisopropyldithiocarbamate ion). Its crystals are monoclinic, space group P2₁ withZ=2 in a unit cell of dimensionsa=8.344(4),b=14.113(8),c=10.647(5) Å,=99.884(2)°, andV=1235.15 ų, finalR=0.043 andR _w =0.047 for 3553 unique reflections. The central tellurium atom shows a S₄I₂ six coordination with the two dithiocarbamate groups almost isobidentate, the average Te-S and the Te-I distances being 2.571(3) and 3.011(1) Å, respectively. The structure is monomeric in the solid state. No intermolecular short contacts are observed.     

Crystal and molecular structure of rubidium azidotrimethylaluminate,Rb[Al(CH3)3N3]

The crystal structure of rubidium azidotrimethylaluminate has been determined from three-dimensional counter data, and refined by full-matrix least-squares techniques. The crystals belong to the monoclinic space groupP2₁/n, witha= 10.003(5),b=7.497(4),c= 11.806(5) Å, = 108.70(3) °, andD _c= 1.58 g cm⁼³ forZ=4. The finalR factor for 922 observed reflections is 0.049. The compound is not isostructural with its cesium analog. The aluminum atom is coordinated in a tetrahedral fashion, and the Al-N bond length is 1.944(8) Å.     

Structure of dichloroethanolaminecopper(II) and dibromoethanolaminecopper(II)

CuCl₂(NH₂CH₂CH₂OH) is monoclinic, space group C2/c, witha+11.092(2),b+10.012(2),c+6.401(1) Å, =121.71(1)°, andV=604.8(2)ų withZ+4. The structure was refined to a final value ofR+0.27 for 518 unique observed reflections with |F|>3. The ethanolamine and halide ions coordinate to the copper(II) ion forming a pseudoplanar four-coordinate monomeric CuCl₂L² complex (L²+bidentate ligand). The copper ion also interacts with the halides of neighboring complexes through the formation of semi-coordinate Cu-Cl linkages (2.926(1) Å) between oligomers. The copper thus attains a 4+2 elongated octahedral coordination geometry. In this space group, the ligand is statisticallydisordered The Cu-Cl distance is 2.267(1)Å while the Cu-N/O distances are 2.025(2)Å. The dibromide structure is isomorphous with the dichloride structure, with space group C2/c, anda+11.285(2),b+10.218(2),c+6.715(1) Å, =121.65(1)°, andV=659.2(2)ų.     

Structural studies on molecular complexes,I: Crystal and molecular structure of 9-aminoacridine-sulfamethoxypyridazine (1∶1), C13H10N2·C11H12N4O3S

The crystal structure of the molecular complex of the antiseptic 9-aminoacridme and the sulfa drug sulfamethoxypyridazine (11), C₁₃H₁₀N₂·C₁₁H₁₂N₄O₃S, has been determined by X-ray diffraction methods. The crystals are orthorhombic: Pbca (No. 61),a=16.321(1),b=16.951(1),c=16.331(1) Å,Z=8,F(000)=1984, andV _c =4518.1(5) ų. The structural parameters have been refined to a finalR value of 0.046 for 3134 observed reflections. The results of X-ray analysis show that the structure contains an acridinium-sulfanilamidate ion pair. A hydrogen atom is transferred from the sulfonamide nitrogen atom to the nitrogen atom of the acridine ring, and an N(acridinium)-HN(sulfonamide) hydrogen bond is formed. A slight folding of the acridine moiety is observed.     

X-ray crystal structure oftrans-dichlorobis(2,6-lutidine)palladium(II)

The X-ray structure oftrans-(2,6-lutidine)₂PdCl₂ has been determined. Golden orange crystals of the complex crystallize in the triclinic space group , with cell dimensionsa=7.6950(8),b=7.9705(10),c=8.0485(8)Å, =116.967(9), =113.343(8), and =93.836(9)°;V=385.18(7)ų andZ=2. 1336 unique reflections withI _net>3 (I) on refinement afforded values ofR=0.018 andR _w=0.023.     

Crystal structure oftrans-tetrachlorobis[2-(2-1H-imidazolyl)-1H-imidazolium]cadmium(II), [Cd(H3biim)2Cl4]

The reaction between cadmium(II) chloride and 2,2'-bi-1H-imidazole (H₂biim) in an acidic solution affords [Cd(H₃biim)₂Cl₄] (H₃biim=2-(2-1H-imidazolyl)-1H-imidazolium) in 63% yield. The compound crystallizes in the triclinic space groupP1, wherea=8.072(2),b=8.100(2),c=8.593(2) Å, =75.89(2), =62.94(2), =63.29(1)°,V=446.4(2) ų, andZ=1. The central Cd atom exhibits an octahedral geometry composed of a Cl₄N₂ core. The Cd-N bond distance is 2.392(2) Å. Cd–Cl distances are 2.5919(9) and 2.671(1) Å.     

Synthesis and molecular structure of {[Se(CH3)3][(CH3)AlCl3]}n: A novel two-dimensional layered organoaluminum-selenium polymer

The crystalline product {[Se(CH₃)₃][(CH₃)AlCl₃]}_n was prepared from reaction of SeCl₄ with A1(CH₃)₃ in heptane. The organo-main group polymer crystallizes in the monoclinic space group P2₁/c with unit cell parametersa=11.218(3) Å,b=11.119(3) Å,c=9.915(2) Å,=107.82(2)°,V=1177.4(5) ų, andD ^calcd=1.54 g cm^–3 forZ=4. Least-squares refinement based on 1195 observed reflections I>3(I) in the range 3.50°<2<45.0° led to a finalR factor of 0.036 (R ^w=0.047). The asymmetric unit contains one selenonium ion, Se(CH₃) ₃ ⁺ , and one organoaluminum anionic species, (CH₃)AlCl ₃ ^– . Secondary interactions (SeCl) serve to link the ions along two dimensions to form infinite layers. Thus, {[Se(CH₃)₃] [(CH₃)A1C1₃]}_n may be regarded as a layered organoaluminum-selenium polymer. The mean Se-C bond distance is 1.921(5) Å while the mean C-Se-C bond angle is 99.1(4)°. The independent Al-C bond distance is 1.927(8) Å while the mean Al-Cl bond distance is 2.166(7) Å.     

Crystal and molecular structure ofmer-trichlorotris(pyridme)chromium(III), CrCl3(C5H5N)3

The crystal and molecular structure of 1,2,6-trichlorotris(pyridine)chromium(III) is discussed. Monoclinic crystals were indexed in the nonstandard space group, P2₁/n (No. 14). The unit cell contains four molecules:a=9.088(1) Å,b=12.442(1) Å,c=15.557(1) Å, and=91.33°;d _x=1.49 g cm^–3,d _m=1.49 g cm^–3. A total of 4056 unique reflections was recorded on a Syntex automated four-circle diffractometer usingMo K radiation. After the appropriate Lorentz and polarization corrections were made, the structure was solved by standard Patterson techniques. Least-squares refinement and difference Fourier analysis revealed all other atoms. The final agreement factors areR=0.062 andR _w=0.052. The nearly planar pyridine ring systems were found to pivot in a fan-blade arrangement about the plane described by the three nitrogen atoms and one chlorine atom. The geometry about the central chromium atom agrees with the expected octahedral configuration.