The crystal structure of a magnesium(II) ethyl diglyme complex

Dibromo[1,1-oxybix[2-ethoxyethane]-O,O,O]-(tetrahydrofuran-O) magnesium, C₁₂H₂₆O₄MgBr₂, crystallizes in space group Pbca witha=7.402(1),b=16.726(2),c=29.248(3) Å,V=3620.9(12) ų,Z=8. The structure was refined toR=0.083 andR _w =0.055 for 1880 observed reflections. Magnesium is octahedrally coordinated by twocis bromine atoms and four oxygen atoms, three from the meridional ethyl diglyme and one from tetrahydrofuran. The Mg–Br distances are 2.614(3)trans to thf and 2.529(3) Åtrans to the central O of the diglyme. The Br–Mg–Br angle is 97.9(1)° and the Mg–O(thf) distance is 2.196(6) Å. The O–Mg–O bite angles subtended by the diglyme are 75.3(2) and 75.7(2)°. The Mg–O(ethyl diglyme) distances are 2.127(6), 2.136(6), and 2.090(6) Å.     

Crystal structures of 1-(2-hydroxyphenyl)-3-phenyl-1,3-propanedione and 1-(1,3-benzodioxol-5-yl)-3-(2,4-dimethoxyphenyl)-1,3-propanedione

1-(2-Hydroxyphenyl)-3-phenyl-1,3-propanedione crystallizes in the triclinic space group (a=5.4233(5),b=13.910(1),c=17.036(1) Å, =68.311(6), =80.854(7), =78.760(8)°) as two independent enolic tautomers in which the hydroxyl and phenolic protons are hydrogen bonded to the ketonic oxygen atom. The structure was refined toR=0.039 for 2085I3(I) reflections. 1-(1,3-Benzodioxol-5-yl)-3-(2,4-dimethoxyphenyl)-1,3-propanedione, which belongs to the triclinic space group (a=7.3990(7),b=8.1239(5),c=14.004(1) Å, =86.673(6). =88.574(7), =64.885(7)°) also exists in the enolic form. The structure was refined toR=0.040 for 1564I3(I) reflections.     

Crystal structure of 4,6-dinitro-1-(5-tetrazolyl)-1H-indazole trihydrate

The title compound, C₈H₄N₈O₄·3H₂O, crystallizes in space groupP¯1 with cell constantsa=7.022(1),b=9.507(2),c=10.906(2) Å,=84.99(1),=71.89(1),=72.56(1)°,Z=2, andV _c =660.2 ų. The structure was solved by direct methods using diffractometer data and was refined by full-matrix least-squares methods to anR value of 0.060 for 2112 observed reflections. The molecule, consisting of a phenyl ring fused to a pyrazole ring with a tetrazole ring connected to it equatorially, is planar except for the N(7) nitro-group oxygen atoms. The structure is stabilized by a three-dimensional network of O-HO, O-HN, and N-HO hydrogen bonds through the water molecules.     

Conformational study on aryl ketones: The structure of 2,6-dimethyl-1,5-di-(2-methyl)-propanoylnaphthalene

C₂₀H₂₄O₂ (M _r =296.4) crystallizes in the monoclinic system, space groupC2/c witha=24.154(4),b=8.001(2),c=12.751(3) Å;=136.8(1)°;V=1686.9 ų,Z=4,D _c =1.17 g cm^–3,(Cu-)=5.4 cm^–1,=1.5418 Å,F(000)=640. The molecule in the solid state adopts a centrosymmetric geometry with the molecular center of symmetry coincident with a crystallographic center of symmetry. This fact forces the molecule to themeso conformation.     

Studies of systemic acylanilide fungicides. Part IV. Crystal structure and molecular conformation ofN-(2-methoxyacetyl)-N-(2,6-xylyl)-α-amino-γ-butyrolactone

The crystal structure of the title compound (C₁₅H₁₉NO₄, MW 277.3 amu) was determined by three-dimensional X-ray analysis from diffractometer data. Crystal data are: monoclinic,P2₁/n,a=9.600(3) Å,b=11.964(6) Å,c=12.802(4) Å,=101.25(3)°,V=1442.1(16) ų,Z=4;D _x =1.277 Mg m^–3;(MoK)=0.10 mm^–1. FinalR=0.055 for 1686 observed reflections having 2 (MoK)<50° andI>2.5 (I). The compound is isostructural withN-(2-methoxyacetyl)-N-(2,6-xylyl)-3-amino-1,3-oxazolidin-2-one. The dimethylphenyl ring is almost perpendicular to the amidic plane of the molecule (dihedral angle 81.9°); the butyrolactone ring is in the typical envelope conformation.     

A comparison of the coordination preferences of Zn, Co, and Cd(II) with the heteroscorpionate ligand (2-hydroxy-3-t-butyl-methylphenyl)bis (3,5-dimethylpyrazolyl)methane

Reaction of the Zn, Cd, or Co nitrate salts with the deprotonated ligand (2-hydroxy-3-t-butyl-methylphenyl)bis(3,5-dimethylpyrazolyl)methane (L1O^–) in methanol produced the following complexes: [(L1OH)Zn(NO₃)₂] in two isomorphs, a = 40.983(8) Å, b = 9.571(2) Å, c = 15.667(8) Å, = 90, = 106.38(1), = 90, C2/c, and a = 13.027(3) Å, b = 14.781(4) Å, c = 16.107(3) Å, = 90, = 105.30(1), = 90, P2₁/n; [(L1OH)Cd(pz)(NO₃)₂] a = 14.7476(2) Å, b = 13.5411(2) Å, c = 16.7223(2) Å, = 90, = 110.3840(10), = 90, P2₁/c; and [(L1O)Co(pz)(NO₃)] a = 11.4240(2) Å, b = 13.4498(2) Å, c = 13.8056(2) Å, = 105.2080(10), = 105.8130(10), = 112.7470(10), P . The Zn adopts a pseudotetrahedral four-coordinate geometry where the potentially tridentate ligand is actually bidentate with a protonated and uncoordinated phenoxy arm. The Co complex is pseudooctahedral six-coordinate where the phenoxy arm is deprotonated and coordinated. Finally the Cd complex is seven-coordinate but the metal is not coordinated through the phenoxy group that is again protonated.     

Pentacoordinated tin(II); crystal structure of dichloro-[2,2′∶6′,2″-terpyridyl]-tin(II)

The crystal structure of a well-defined 5-coordinate complex, dichloro-(2,26, 2-terpyridyl)-tin(II), is described. The stereochemistry of this complex is strongly influenced by the stereochemically active pair of electrons, illustrating clearly the potential donor capabilities of this molecule. The complex (C₁₅H₁₁Cl₂N₃Sn) crystallizes in the monoclinic space groupC2/c (No. 15) witha=15.770(5),b=9.450(2),c=10.482(2) Å,=97.53(2)°,Z=4. The finalR value is 0.029 for 1085 observed reflections.     

Syntheses and structures of N-phenylmaleimidetriazoles and by-products

The syntheses, properties, and structures of N-phenylmaleimidetriazole derivatives are described. Intermediates and by-products are also discussed. 1b. a = 43.997(7) Å, 5.7610(9) Å, 8.245(1) Å, = 99.339(4), C₂/c; 2a. a = 13.646(4) Å, b = 7.744(2) Å, c = 10.612(3) Å, = 91.979(6), P2₁/c. 3a. a = 22.245(1) Å, b = 22.245(1) Å, 10.010(1) Å, P42/n. 3a. a = 11.727(2) Å, b = 14.075(3) Å, c = 16.080(3) Å, = 105.859(3), = 105.331(3), = 98.187(3), P-1. 3b. a = 8.561(3) Å, b = 14.755(5) Å, c = 22.771(7) Å, = 97.006(5), P2₁/c. 3c. a = 10.500(2) Å, b = 12.189(2) Å, c = 13.040(2) Å, = 109.091(3), = 106.089(3), = 101.022(3), P-1. 8a. a = 16.389(8) Å, b = 5.749(3) Å, c = 19.316(3) Å, = 97.467(9), P2₁/n. 8b. a = 5.822(2) Å, b = 10.114(3) Å, c = 16.705(4) Å, = 84.681(5), = 82.840(5), = 75.769(4), P-1. 9b. a = 11.251(1) Å, 13.335(3) Å, 13.376(3) Å, = 102.456(4), P2₁/n. 9c. a = 15.836(3) Å, b = 8.236(2) Å, c = 5.447(3) Å, = 92.551(3), P2₁/c. 10a. a = 13.177(2) Å, b = 14.597(2) Å, c = 5.5505(8) Å, = 110.979(2), Cc. 11a. a = 14.720(2) Å, b = 13.995(2) Å, c = 38.245(6) Å, = 94.430(3), P2₁/n. 12b. a = 15.067(5) Å, b = 20.378(6) Å, c = 8.669(5) Å, = 99.16(4), = 99.32(3), = 105.23(3), P-1. 13b. a = 8.2824(6) Å, b = 10.5245(7) Å, c = 15.518(1) Å, = 92.305(1), = 100.473(1), = 100.124(1), P-1. 15a. a = 15.357(3) Å, b = 7.778(2) Å, c = 22.957(2) Å, Pbca. 16b. a = 18.0384(4) Å, b = 12.474(3) Å, c = 20.078(5) Å, Pbca.     

Synthesis and structure of tris(N-methylaminoethanoldithiocarbamato)arsenic(III)

The title compound was synthesized by the interaction of arsenic(III)chloride with freshly prepared N-methylaminoethanoldithiocarbamic acid in methanol. The compound crystallized in the triclinic system, space groupP with two molecules per unit cell, the dimensions area=6.509(10)Å,b=14.077(3)Å,c=14.195(3)Å, =64.16(2)^o, =84.67(2)^o and =84.00(2)^o. The molecule is monomeric with three short (mean 2.320(3)Å) and three long (mean 2.927(2)Å) As-S bonds. Asymmetry in the As-S bonds is due to the presence of stereochemically active lone pair on arsenic and the coordination polyhedron deviates from the usual D₃ symmetry to C₃ symmetry. Disorder exists in one of the dithiocarbamate ligands probably due to the O...O interaction arising from the water molecule. The anisobidenticity of the As-S bond distances is as a consequence of stereochemical requirement of the ligand and the lone pair of electrons on arsenic.     

Diammonium μ-oxobis[trichloroferrate(III)] salts. Crystal and molecular structure of bis(benzyldimethylphenylammonium) μ-oxobis(trichloroferrate)

Several alkyl-, aralkyl-, and aryl-substituted diammonium-oxobis[trichloroferrate(III)] salts, of potential interest as model compounds for the study of certain electrophysical and biological processes, are synthesized via the corresponding tetrachloroferrate(III) salts and are characterized by IR and Raman spectroscopy. A structure analysis is performed on the representative bis(benzyldimethylphenylammonium)-oxobis(trichloroferrate). The (tetracoordinate) iron atoms in the oxo-bridged dinuclear anion of the salt each possess an ever so slightly distorted tetrahedral ligand environment; the bridge geometry [Fe-O distances 1.757(5) and 1.775(5) Å, Fe-O-Fe angle 147.7(3)°] compares well with that of other salts containing the [Cl₃Fe-O-FeCl₃]^2- anion. Crystallographic Data:a=26.392(5) Å,b=14.015(3) Å,c=9.638(2) Å,=92.65(2)°, andZ=4; space groupP2₁/n.R(F)=0.070,R _W (F)=0.078 for 4447 observed reflections.     

Synthesis and structural characterization of the bitopic ferrocene-based tris(pyrazolyl)methane ligand Fe[C5H4CH2OCH2C(pz)3]2 (pz = pyrazolyl ring)

The structure of Fe[C₅H₄CH₂OCH₂C(pz)₃]₂ (pz = pyrazolyl ring) contains 1.5 independent molecules in the asymmetric unit. One molecule has no imposed symmetry with the iron atom located on a general position while in the other the iron atom is located on an inversion center. The two independent molecules are arranged into a three-dimensional supramolecular structure by a series of C—H s N and C—H s O weak hydrogen bonding interactions and C—H s interactions. The crystals are triclinic, space group, P , with a = 8.1202(4) Å, b = 16.7209(9) Å, c = 18.6540(10) Å = 85.8270(10), = 85.4740(10), = 81.5910(10), and Z = 3     

Crystal and molecular structure of (exo)-2-methoxycarbonyl-5-ethoxycarbonyl-4,5,6,11b-tetrahydroisoxazolidino-[2,3-a]-β-carboline,C18H20N2O5

The structure of the title compound, C₁₈H₂₀N₂O₅, was determined by X-rays atT=290 K.M _r =344.366, monoclinic, space groupP2₁/c,a=13.7850(8),b=8.8951(7),c=15.1603(11) Å, =111.410(6)°,V _c =1730.7 ų,Z=4,D _x =1.322 Mgm^–3. Cu K radiation (graphite crystal monochromator, =1.54178 Å),(Cu K)=7.69 cm^–1. Final conventionalR-factor=0.057,R _w =0.076 for 2160 observed reflections and 271 variables. The structure was solved usingMultan.     

Crystal structure of 5α-bromo-8β,9α-dimethyl-hydrindane-1,4-dione

The molecular structure of 5-bromo-8,9-dimethylhydrindane-1,4-dione (C₁₁H₁₅BrO₂) has been confirmed using three-dimensional X-ray data collected by means of a Picker FACS-1 four-circle diffractometer. The compound crystallized in the space groupC2/c with unit cell constantsa = 26.56(5),b = 6.68(1),c = 12.32(2) Å and = 90.6(1) °; the density was 1.55 g cm^–3 andZ = 8. Least-squares refinement of the positional and anistropic thermal parameters gave a finalR ₁ value of 0.083 for 793 significant reflections.     

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.     

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.     

The molecular structure of dibutylbis(2-pyridinethiolato-5-ethyl ester)tin(IV), [SnBu2(TNEE)2]

The crystal structure of [SnBu₂(TNEE)₂], (HTNEE=5-ethyl ester of 2-mercaptopyridine-5-carboxylic acid) has been determined by X-ray single crystal diffraction study. The crystal is triclinic, space groupP,a=10.042(1),b=18.421(2),c=7.979(1) Å, =98.7(1), =107.3(1), =87.7(1)^o,V=1393(1) ų, and Z=2 The tin center is coordinated to two butyl groups and to the nitrogen and the sulfur atoms of two ligand molecules in a very distorted trapezoidal bipyramid.     

Crystal structure of osmocene,Os(η-C5H5)2

Crystals of osmocene, Os(-C₅H₅)₂, are orthohombic:Pnma,M _r =321.3,a=7.079(2),b=8.908(1),c=12.771(2),V _c =806 ų,Z=4,D _x =2.640 g cm^–3, MoK (=0.71069 Å),=151 cm^–1,F(000)=584,T=293 K,R=0.04 for 730 observed reflections. Osmocene is isomorphous with ruthenocene and the molecules have averageD _5h symmetry with a mean Os-C distance of 2.19(1) Å (compared with 2.186 Å forRu-C).Part 26 of the series Cyclopentadienyl-ruthenium and -osmium chemisty. For Part 25, see Bruce, etal. (1985).     

Structural characterization and excited-state properties of luminescent <Emphasis Type="Italic">Tris</Emphasis>-(μ -3-methyl-5- trifluoromethylpyrazolato)trigold(I)

Tris-(-(3-methyl-5-trifluoromethylpyrazolato)-N:N)triangulo-trigold(I), (3,5-tfmpz)₃ Au₃, has been synthesized and exhibits a planar nine-member ring containing a central gold triangle with an average intramolecular Au–Au distance of 3.3455(8) Å. The complex crystallizes in the monoclinic space group Cc with a = 12.998(2) Å, b = 22.910 (3) Å, c = 7.217(1) Å, and = 104.781(1). The solid-state structure consists of sheets of (3,5-tfmpz)₃Au₃ units stacked in an offset fashion along the c axis such that one gold atom in each Au₃ unit (Au1) lies approximately over the midpoint of the Au1–Au3 edge of the triangle in the layer below it. The intermolecular Au–Au distances are between 3.880(1) and 4.023(1) Å, which are too long for there to be significant intertrimer bonding interaction suggesting that any supramolecular organization may be due to hydrogen-fluorine and fluorine-fluorine interactions between the molecules. The complex exhibits excitation-dependent emission at room temperature in the solid state. The structured higher energy emission (_em = 468, 517, and 556(sh) nm) is believed to be a ligand-centered ^* transition with a lower energy unstructured emission (_em = 658 nm) assigned to the classical Au–Au excited state transition.     

Crystal and molecular structure of [(C6H5)3Sb]3CuCl·CHC13

The X-ray crystallographic structure determination of [(C₆H₅)₃Sb]₃ Cu(I)Cl·CHC1₃ reveals that the compound crystallizes in the triclinic space groupP¯1 witha=18.827(3),b=14.279(3),c=14.399(3) Å,=84.43,=87.39(2), and=75.18(1)°,V=2734.7(9) ų,Z=2. Least-squares refinement based on 4689 independent observed data [(F _obs)²3(F _obs)²], resulted in a finalR value of 0.064. The cocrystallized solvent molecules were highly disordered. The coordination about Cu(I) of three Sb(C₆H₅)₃ molecules and one Cl ligand is approximately tetrahedral. The Cu-Cl distance, 2.235(5) Å, is extremely short in comparison to previously reported Cu-Cl distances in four-coordinate Cu(I) complexes. In keeping with the short Cu-Cl distance are very long Cu-Sb distances, av. 2.554(5) Å.     

The crystal structure of 5-methyl-1-(octahydro-1-iodo-1H-1-inden-4-yl)-1H-tetrazole

The title compound is C₁₁H₁₇N₄I, F.W.=330.20, monoclinic, space groupP2₁/a,a=11.586(2),b=10.617(1),c=10.417(1) Å, =94.567(2)°,Z=4,F(000)=652, (MoK)=0.7107 Å, (MoK)=2.31 mm^–1,V=1277.31 Å₃,D _C=1.71 gcm^–3,D _m=1.70 gcm^–3. The structurewassolved by Patterson and Fourier methods and refined to anR value 0.031 for 1620 observed reflections. The connectivity and conformation of the addition product ofcis-1,5-cyclononadiene and iodine azide was determined by X-ray analysis. The reaction product contains a chair-conformation cyclohexane ring that iscis fused to a cyclopentane ring. The cyclopentane ring has an envelope conformation and an equatorially oriented iodine substituent. A planar tetrazole ring is axially substituted on the cyclohexane ring. The plane of the tetrazole ring makes a dihedral angle of 69.6° with the average plane of the carbon atoms of the cyclohexane ring.