Crystal and molecular structure of 5-ethoxy-4-methylene-exo-10-oxatricyclo[5.2.1.02,6]-deca-8-ene-3-ol,C12H16O3

The structure of the title compound, C₁₂H₁₆O₃, was determined by X-rays.M _r =208.26, triclinic, space groupP¯1,a=7.802(2),b=8.449(2),c=9.069(1) Å,=90.79(1)°,=105.57(1)°, =106.07(1)°,Z=2,D _x =1.26 Mg m^–3; MoK radiation (graphite crystal monochromator, =0.71069 Å),(MoK)=0.96 cm^–1,T=290 K. Final conventionalR-factor=0.046,R _w =0.067 for 3009 observed reflections and 184 variables. The structure was solved using Patterson methods andDirdif, and the resulting all cis-endo configuration of the alcohol group on C(3) and the ethoxy group on C(5) shows that the stereochemistry of the metal-mediated addition reaction involved is solely determined by steric factors.     

Crystal and molecular structure of OC(CoC5H5)3(CF3CCCF3)

The structure of the title compound has been confirmed by an X-ray diffraction analysis, and refined by full-matrix least squares. The crystals are mono-clinic:a=9.171(3),b=25.176(15)c=9.192(3) Å,=117.08(3)°,Z=4,D _x =1.976g cm^–3,=2.66mm^¯1, space groupP2₁/n (No. 14). The finalR value is 5.7%. Interatomic distances and bond angles are compared with those reported in related molecules.The preferred name of this compound according to the IUPAC rules is ₃-[11–2-bis(trifluoromethyl)vinylene]- ₃-carbonyl-tris (-cyclopentadienyl)-triangulo-tricobalt.     

Structure of (Z)-1-p-methoxyphenyltelluro-1,4-diphenyl but-1-en-3-yne

C₂₃H₁₈TeO,M _r=437.97, ,a=9.940(2),b=13.664(3),c=7.895(2) Å, =80.60(1), =69.71(2), =75.95(1)°,V=972.0(4) ų,Z=2,R=0.041 for 2668 observed reflections. The Te–C bond distances are 2.109(5)Å and the C–Te–C angle is 96.0(2)°. The phenyl rings are planar to within experimental accuracy, making dihedral angles of 64.6(2), 65.3(2) and 31.1(3)°.     

Synthesis,characterization and crystal structure of oxovanadium(IV) complex with tridentate o-van-gly and bidentate phenanthroline

A novel oxovanadium(IV) complex with tridentate schiff base and bidentate phenanthroline ligands, VO(o-van)(phen) 2H₂O[o-van-gly: o-vanillin-glycine; phen: phenanthroline], was synthesized and characterized by elemental analysis, IR and UV-vis spectra. The crystal structure was determined by X-ray single crystal diffraction analysis. The crystal of title complex (C₂₂H₂₁N₃O₇V, M_w = 490.36) belongs to triclinic, space group P-1 with the following crystallographic parameters: a = 9.247(3) Å, b = 10.125(4) Å, c = 13.100(5) Å, = 106.343(6), = 96.042(7), = 101.726(7), V = 1135.0(7) ų, Z = 2, D_c = 1.435 Mg m^–3, (MoK = 0.485 mm^–1, F(000) = 506, and final R₁ = 0.0779, wR₂ = 0.1598 for observed reflections 1606 (I > 2(I)). V(IV) is six-coordinate with three oxygen atoms and three nitrogen atoms in a distorted octahedral geometry. The complex forms a 3-D network via – stacking and hydrogen bonds.     

On the organoaluminum chemistry of multidentate phosphine ligands. Reaction of trimethylaluminum with bis(diphenylphosphino)methane: Synthesis and molecular structure of [Al(CH3)3]2[(C6H5)2PCH2P(C6H5)2]

Reaction of an excess of trimethylaluminum with bis(diphenylphosphino)-methane in heptane affords the crystalline complex [A1(CH₃)₃]₂[(C₆H₅)₂PCH₂P(C₆H₅)₂]. The title compound crystallizes in the triclinic space group P¯1 with unit cell parametersa=10.053(6),b=11.017(6),c=15.908(8) Å,=85.58(4),=71.80(4), =77.49(4)°,V=1634(1) ų, andD _c=1.07 g cm^–3 forZ=2. Least-squares refinement based on 2924 observed reflection with intensitiesI3I) in the range 2.00245.0° converged atR=0.050 (R _w=0.067). The Al-P distances are 2.585(2) and 2.521(2) Å, and the P-C-P angle is 121.4(2)°.     

Structure and spectral properties of (O-Cyclohexyldithiocarbonatio-S,S′) bis(triphesnylphosphine) copper(I) complex

The complex [(C₆H₁₁OCS₂)(PPh₃)₂Cu], was synthesized and characterized using IR, UV, and ¹H NMR. The crystal and molecular structure has been determined by X-ray diffraction. The yellow crystal of the complex is triclinic of space group , with parameters a=10.370(2)Å, b=13.530(3)Å, c=14.640(3)Å, =92.60(3)°, =108.00(3)°, =97.70(3)°, and Z=2. In the complex, the central Cu atom is in a distorted tetrahedral environment and chelated by two phosphorus atoms of the TRIPHOS and two sulfur atoms from the O-cyclohexyldithiocarbonate. The cyclohexane ring adopts a chair conformation. The thermal analytical data indicate that the complex begins to decompose at 101°C and stop at 360°C , leaving CuS. IR, UV, and NMR results supported the crystal structure.     

A new monoclinic crystal phase of [Bu4N][Ni(dmit)2]

The crystal structure of the title compound, tetrabutylammonium bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III), [N(C₄H₉)₄][Ni(C₃S₅)₂], is the fourth known phase of this polymorphous compound. It is monoclinic space group P2₁/c, with a = 20.040(2) Å, b = 13.1151(17) Å, c = 12.1093(15) Å, = 105.456(15)°, and V = 3067.5(6) ų with Z = 4, for D _calc = 1.503 g cm^–3. The [Ni(dmit)₂] anion packing arrangement consists of arrays of side-on touching anions and these arrays are connected via head-to-tail close S S contacts.     

Pentacoordination in dibromo-N-2-methylthiophenyl-2′-pyridylmethyleneiminezinc

The crystal structure of dibromo-N-2-methylthiophenyl-2-pyridylmethyleneiminezinc has been determined and refined by Fourier and least-squares methods toR = 0·058 using three-dimensional X-ray data collected at room-temperature on a single-crystal automated diffractometer. The crystals are triclinic (space groupP¯i), with two molecules in the unit cell of dimensions:a = 9·384(6),b = 11·587(7),c = 7·962(7) Å, = 113·3(1), = 104·3(1), = 92·7(1) °. The zinc atom is five-coordinated through two bromine atoms (Zn-Br=2.366, 2.398 Å), one sulphur atom (Zn-S=2.645 Å) and two nitrogen atoms (Zn-N=2.121, 2.150 Å) from the organic molecule, which behaves as a tridentate ligand. Packing is determined by normal van der Waals interactions.     

Crystal structure of 10-oxa-3,4 benzobicyclo [5.3.0] deca-1 (7) ene-8,9 dione,C13H10O3

The crystal and molecular structure of the title compound, C₁₃H₁₀O₃, determined by single crystal X-ray diffraction is reported. Crystals are triclinic, space groupP¯1,a=9.251(1),b=8.837(1),c=7.091(1)Å;=85.6(1)°,=108.2(1)°, =110.1(1)°;V=517(3)ų;Dx=1.38 mg m^–3, (MoK)=0.7107 Å;=0.91 mm^–1;F(000)=224. The structure was solved by direct methods and the finalR value is 0.059 (R=0.078) for 1393 independent observed relfections. In the crystal the cycloheptadienic moiety adopts an approximate twist chair conformation with a pseudo-twofold axis and presents disorder.     

Crystal structure of μ-adeninatobis (methylmercury (II)) perchlorate monohydrate

The title compound belongs to the triclinic space groupP¯1,a= 8.189 Å,b = 9.863 Å,c = 10.726 Å, = 69.93 °, = 68.62 °, = 73.66 °, andZ = 2. The structure was refined on 1337 observed reflections to anR factor of 0.042. The crystals contain [adeninato(CH₃Hg)₂]⁺ complex cations in which mercury is linearly bonded to N(7) and N(9) of a deprotonated adenine ring. Centrosymmetrically related complex cations are paired via two N(6)-H(6) N(l) hydrogen bonds. Those planar units are stacked in the crystal with a distance of 3.4 Å between rings. The water molecule and the ClO₄ ^-ion are involved in hydrogen bonding and HgO contacts. This structure identifies N(7) as the best residual coordination site after H(9) has been substituted by CH₃Hg.     

Synthesis and structural studies of <Emphasis Type="Italic">tris</Emphasis>-2-chlorobenzylamine and <Emphasis Type="Italic">tris</Emphasis>-2-bromobenzylamine

The tris-2-chloro and 2-bromotribenzylamines are prepared from aqueous ammonia and 2-chlorobenzyl chloride and 2-bromobenzyl bromide, respectively, in ethanol. Recrystallization yielded colorless cubes of each product. The crystal structures are each solved in space group P , and are isostructural. The tris-2-chloro compound, 1, has a = 7.4226(5) Å, b = 9.0825(7) Å, c = 14.529(1) Å, = 78.279(1), = 82.389(1), = 84.661(1), and V = 948.41(12) ų with Z = 2, and d_calc = 1.368 Mg/m³. The tris-2-bromo analog, 2, has a = 7.6569(11) Å, b = 9.0922(13) Å, c = 14.614(2) Å, = 79.286(2), = 81.777(2), = 85.401(2), and V = 987.9(2) ų with Z = 2, and d_calc = 1.762 Mg/m³. Lithium–halogen exchange experiments conducted in tetrahydrofuran at –78C using n-butyl lithium revealed that no exchange occurred for the tris-2-chloro compound, but did occur for the tris-2-bromo analog to yield tribenzylamine upon quench and work-up.     

Molecular structures of two conjugated ene-ynes derived from thiophene

The crystal structures of two conjugated ene-yne derivatives of thiophene are described, 2,5-di-(trimethylsilylethynyl)-3,4-dibromothiophene (1), is triclinic P witha=6.3281(4)Å,b=9.7421(6)Å,c=16.3669(9)Å; =80.516(5)°, =84.810(5)°, =74.072(5)°,Z=2,R=0.054; 2,3,4,5-tetra(trimethylsilylethynyl)thiophene (2), is monoclinic, P2₁/c with a=20.928(2)Å b=5.852(1)Å,c=23.907(2)Å; =100.245(6)°,Z=4,R=0.049. The ethynylic C atoms of both compounds lie near the thiophene plane, with deviations in the range 0.010(3)–0.455(4)Å. The phenyl groups of2 form a dihedral angle of 13.0(4)°.     

Synthesis and crystal structure of N-<Emphasis Type="Italic">tert-</Emphasis>butyl-N′-thio [O-(1-methylthioethylimino)-N″-methylcarbamic acid]-N,N′-dibenzoylhydrazine

The novel compound N-tert-butyl-N-thio[O-(1-methylthioethylimino)-N-methyl carbamic acid]- N,N-dibenzoylhydrazine has been synthesized by the reaction of N-tert-butyl-N,N-dibenzoylhydrazine with N-sulfenyl chloride of O-(1-methylthio ethylimino) -N-methylcarbamic acid. Its structure was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic, space group P2₍₁₎/n with the following crystallographic parameters: a = 7.569(3) Å, b = 20.585(7) Å, c = 16.347(5) Å, = 90, = 92.606(6), = 90, V = 2544.4(14) ų, z = 4, Dx = 1.276 mg/m³, F(000) = 1032, T = 293(2) K, 2.34 25.01, the final R factor: R₁ = 0.0475, wR₂ = 0.0907. The N–N bond adopts a gauche conformation with a dihedral angle() of 98.8 for C(17)=N(1)=N(2)=C(7), whereas its parent compound N-tert-butyl-N,N-dibenzoyl hydrazine has the dihedral angle of –71.8.     

Complexation with diol host compounds. Part 3. Molecular inclusion of 4-methylcyclohexanone and 2-methylcyclohexanone by the host,trans-9,10-dihydroxy-9,10-diphenyl-9,10-dihydroanthracene

The structures of the 12 molecular complexes oftrans-9,10-dihydroxy-9,10-diphenyl-9,10-dihydroanthracene with 4-methylcyclohexanone (1) and with 2-methylcyclohexanone (2) have been determined by X-ray crystallography. The crystal data are as follows: Compound (1):P2₂/c,a=8.838(2) Å,b=8.92(1) Å,c=20.879(8)=Å,=98.67(2)°,V=1627(2) ų,Z=2 andR=0.062 for 2201 unique MoK reflections; Compound (2):P¯1,a=8.917(3) Å,b=9.900(2) Å,c=11.250(4) Å,a=68.72(2)°,=64.39(3)°, =74.86(2)°,V=828.1(5) ų,Z=1 andR=0.098 for 2563 unique reflections. Both inclusion compounds exhibit O-HO=C hydrogen bonding interactions. The thermal properties of these compounds have been characterized by DTA and TGA thermograms.     

Crystal structure of dicesium thorium trisulfate dihydrate,Cs2Th(SO4)3·2H2O

Dicesium Di--sulfatosulphatobisaquothorate(IV), H₄O₁₄S₃Cs₂Th, (M _r =821.8) crystallized from water in the monoclinic space groupP2₁/c (No. 14), witha=6.415(2),b=15.95(1),c=13.078(8) Å,=90.88(4)°,V=1338(14) ų,Z=4,D _x =4.08 g cm^–3, MoK (=0.71069 Å),=195.8 cm^–1,F(000)=1407.3, room temperature, finalR=0.086 for 1699 unique observed reflexions. Two of the sulfate groups are tridentate (chelating and bridging) and the other is bidentate chelating. As the waters are both coordinated the thorium is 10-coordinate. It shows an unusual 2/4/2/2 geometry.     

Crystal and molecular structure of the rutheniumcarbene-tetraborohydrate complex [Ru(BH4)(LAr)(PPh3)2]; (LAr=CN(C6H4Me-4)CH2CH2NC6H3Me-4)

The structure of the title compound has been determined by single crystal X-ray diffraction analysis:P2₁/c,M _r=889.9,a=15.940(1),b=23.357(2),c=18.767(2) Å,=132.62(1)°,V _c=5141.6 ų,Z=4,D _x=1.150 mg m^–3,F(000)=1848; finalR _f=0.074 (R _w=0.085). The BH ₄ ^– ligand in the complex is bidentate. A comparative study indicates that the lengths of the Ru-carbene carbon bond and other bonds to the Ru atom are determined by a combination of several factors, and not just by a purely - or -bonding interaction.     

Structures of Z-(nitrostilbene)chromium tricarbonyl complexes: The effect of metal coordination on the nonplanarity of the stilbene system

The structures of the nitrostilbene complexes Z-(4-R–C₆H₄–CH=CH–C₆H₄-4-NO₂)Cr(CO)₃ (R=Me₂N,1; H,2; F₃C,3), are reported. The copounds were prepared as part of a study of the synthesis of organometallic complexes with potential nonlinear optics applications. For Z-(4-Me₂N–C₆H₄–CH=CH–C₆H₄-4-NO₂)Cr(CO)₃,1, triclinic, ,a=7.214 (3) Å,b=7.340 (3) Å,c=17.238 (9)Å, =88.23 (5)°, =88.76 (4)°, =87.66 (3) °,Z=2. For Z-(C₆H₅–CH=CH–C₆H₄-4-NO₂)Cr(CO)₃,2, monoclinic, P2₁/C,a=12.255 (3) Å,b=9.415 (1) Å,c=13.579 (4) Å, =105.60 (2)°,Z=4. For Z-(4-F₃C–C₆H₄–CH=CH–C₆H₄-4-NO₂)Cr(CO)₃,3, triclinic, ,a=7.094 (2) Å,b=8.057 (5) Å,c=17.295 (9) Å, =87.95 (5)° =85.94 (4)°, =64.24 (5)°,Z=2. The structural data show that the Z isomers exhibit bond lengths and angles similar to those observed in the E isomers, but the stilbene fragment is considerably more nonplanar. As a consequence, these molecules are unlikely to behave as NLO materials.     

Crystal and molecular structure of 1,6-dimethyl-3,6-dimethoxy-3-[(N-methylindol-3-yl)methyl] piperazine-2,5-dione,C18H23N3O4

The structure of the title compound, C₁₈H₂₃N₃O₄, was determined by X-rays.M _r =344.40, triclinic, space groupP¯1,a=8.163(4),b=9.230(2),c=13.297(2) Å,=102.70(2),=103.58(3)°,=102.50(3)°,V=911.3 ų,Z=2,D _c =1.26 Mg m^–3. CuK radiation (graphite crystal monochromator,=1.54178 Å),(CuK)=7.50 cm^–1,T=290 K. Final conventionalR-factor=0.068,R _w =0.079 for 1912 unique reflections and 295 variables. The structure was solved usingMultan andDirdif. The title compound is the first example of a 3,6-tetrasubstituted dioxopiperazine adopting a folded conformation, owing to a direct interaction between the dioxopiperazine ring and the aromatic side chain.     

Mercury(II) complex with terpyridine: structure of the 2∶1 solvate of [Hg(terpy)2](CF3SO3)2 with acetone

[Hg(terpy)₂](CF₃SO₃)₂·0.5(CH₃)₂CO crystallizes in the triclinic space group witha=14.631(6),b=15.258(4),c=18.785(7) Å, =69.66(2), =70.72(1), =88.55(1)°. The crystal structure consists of two independent [Hg(terpy)₂]²⁺ cations, four trifluoromethanesulfonate anions and an acetone molecule in the asymmetric unit. Each mercury atom is coordinated by two tridentate terpyridine ligands forming an irregular six-coordination polyhedron. The Hg–N bond lengths range from 2.27(2) to 2.53(2) Å.     

Crystal and molecular structure of 3-(4-chlorobenzoylimino)-5,6-dihydro-3H-imidazo[2,1-c]-1,2,4-dithiazole

Crystal structure of the title compound belonging to the group of-acylimino derivatives of sulfur(II) compounds has been determined by X-ray structure analysis. The crystals are monoclinic, P2₁/c,a=11.210(2),b=8.197(1),c=13.659(2) Å,=102.36(2)°,V=1226.0(3) ų,Z=4,D _x =1.61 g cm^–3, (MoK)=0.71069 Å,=6.3 cm^–1. The structure has been refined to a finalR value of 0.035 for 1401 observed reflexions.The molecule is nearly planar with symmetrym. The title compound contains a very short intramolecular C=OS contact of 2.328(3) Å, suggesting a bond-non-bond resonance interaction.