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.     

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.     

Crystal structure of 751-1751-1751-1751-2751-2751-2

The title compound crystallizes in the centrosymmetric triclinic space group (No. 2) witha=10.818(1)Å,b=10.876(1)Å,c=11.072(2)Å, =98.74(1)°, =98.83(1)°, =96.61(1)°,V=125906(3)ų andZ=2. Interatomic distances include Fe–P=2.243(2)Å, Fe–CO=1.771(6)–1.781(5)Å, Fe–C(C₅H₅)=2.074(6)–2.103(5)Å and P–F=1.511(6)–1.571(4)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.     

X-ray crystal structures ofcis-bis(diphenylphosphinamide)tetracarbonylmolybdenum(0) andtrans-bis(N-methyl diphenylphosphinamide)tetracarbonylmolybdenum(0)

The X-ray crystal structures ofcis-Mo(CO)₄(Ph₂PNH₂)₂,I, andtrans-Mo(CO)₄(Ph₂PNHMe)₂,II, are presented. ComplexI crystallizes in the monoclinic space groupP2₁/c(a=13.433(1),b=12.2719(8),c=17.318(2)Å;=109.79(1)°;V=2686.1(8)ų;Z=4). ComplexII crystallizes in the triclinic space groupP¯1 (a=6.9986(8),b=10.328(1),c=11.241(2)Å,=107.58(1)°,=91.76(1)°, =101.28(1)°,V=756.1(4)ų,Z=1). The molybdenum coordination geometry in each complex is a slightly distorted octahedron. The molybdenum-carbon bond lengths for the carbonyls trans to phosphorus in complexI are shorter than those the carbonyls trans to other carbonyls. The average molybdenum-phosphorus distance inI (2.525(5)Å) is similar to those in other diphenylphosphinamide complexes and longer than the molybdenum-phosphorus distance inII in 2.4585(7)Å). The distance between two nitrogen atoms incis Mo(CO)₄(Ph₂PNH₂)₂ (3.74(3)Å) is significantly larger than the sum of their van der Waals radii (3.10 Å) indicating that the two nitrogens are not hydrogen bonded.     

Structure oftrans-dichlorotetrakis(thiazole)Rh(III) perchlorate·acetonitrile solvate

The title compound [RhCl₂(SNC₃H₃)₄] [ClO₄]·CH₃CN is monoclinic, witha=23.791(4),b=7.253(2),c=14.498(2)Å,=105.24(1)°,V=2414(1)ų,Z=4,D _x =1.802,(MoK)=13.95 cm^–1,F(000)=1304,T=298K in space group Cc. The structure was solved by heavy atom and Fourier methods and refined toR=0.047 for 4742 unique observed reflections. The cation is nearly octahedral, with thecis andtrans angles about the Rh in the range from 89.2(2) to 90.8(2)° and 179.4(2) to 180.0(2)°, respectively. Average Rh-Cl and Rh-N bond lengths are 2.337(2) and 2.036(6)Å. One of the thiazole ligands showed disorder between the S and one of the C atoms in the ring.     

Structure of dichloro[(2,4-dimethyl-5-oxo-2,3,4,5-tetrahydro-2-furyl)methyl]-(4-methoxyphenyl)tellurium(IV)

The crystal structure of TeCl₂(C₇H₇O)(C₇H₁₁O₂) has been determined from three dimensional, single crystal X-ray diffraction data. It crystallizes in the monoclinic space group C2/c with the lattice constantsa=24.551(5),b=11.435(2),c=12.368(2)Å,=97.33(1)° andZ=8,D _X=1.67 g cm^–3. Final least-squares refinement based on 3023 independent observed reflections yieldedR=0.026. The Te^iv ion is in a trigonal bipyramidal configuration with its lone pair of electrons at one of the equatorial positions. Distances and angles are: Te-Cl=2.495(1), 2.517(1); Te-C=2.134(3), 2.106(3)(aryl)Å; Cl-Te-Cl=173.45(4), Cl-Te-C=88.11(9), 88.60(9), 88.72(9), 86.06(9); C-Te-C=96.5(1)°. There are two secondary bonds to the tellurium: TeCl=3.824(1) and TeO(2)=3.006(1)Å. The methyl group to the carbonyl oxygen and the aryltelluro moiety exhibit atrans 2,4 relationship.     

Crystallographic and IR spectral study ofcis-bis(creatinine-N)dinitro platinum(II)

Acis-Pt(creat)₂(NO₂)₂ complex was synthesized stereoselectively in a high yield (65%) and characterized by IR spectral and X-ray diffraction analysis. Crystal data: Pt(C₄H₇N₃O)₂(NO₂)₂,M _r=767.55, monoclinic, space groupP2₁/n,a=9.736(1),b=13.433(1),c=12.098(1) Å,=110.55(1)°,V _c=1482(1) ų,Z=2,D _x=3.441 g cm^–3,(MoK)=0.71073 Å,=97.0 cm^–1,F(000)=1504,T=292 K,R=0.026 andR _w=0.028 for 2061 observed reflections with I>2(I). The structure consists of Pt(creat)₂(NO₂)₂ molecules disposed in general positions and joined by N-HO and N-HN hydrogen bonds. The platinum atom has square-planar PtN₄ coordination of twocis disposed pairs of nitro [Pt-N_av 2.023(7) Å] and creatinine [Pt-N(endo)_av 1.991(8) Å] ligands. The creatinine moieties are planar and tilted to the equatorial plane by ~80°.     

Crystal structure of bis-[dihydrido(3,5-dimethyl-1-pyrazolyl) (3,5-diphenyl-1-pyrazolyl)borate]zinc(II), [Zn{H2B(3,5-Me2Pz)(3,5-Ph2Pz)}2]

Crystals of the title compound are monoclinic,a=13.796(1),b=16.727(1),c=16.1937(8) Å,=102.063(5)°,V=3654.3(4) ų, space groupP2₁/c,Z=4. The crystal structure was solved by Patterson and Fourier methods and refined toR=0.033 for 3883 unique reflections withF _o>3(F _o). The metal atom is tetrahedrically coordinated to two bidentate ligands with Zn-N distances and N-Zn-N angles in the range 1.982(2)–2.019(2) Å and 100.3(1)–119.5(1)°. The boat conformations of both BN₄Zn chelate rings are unusually asymmetric (quasi-sofa), with the B atoms at 0.71 Å from the N₄ mean plane, while the Zn atoms are at only 0.07 Å. ZnB distances (3.784 and 3.794 Å) andv(B-H) stretching frequencies (2497 and 2400 cm^–1) rule out agostic bonds. Overall the molecule displays approximate C₂ symmetry. The temperature-dependent NMR spectra show no fluxional behavior in solution.Paper presented at the XV Congress of the International Union of Crystallography, Bordeaux, France, 19–28 July 1990 (abstract PS-06.03.01).     

Studies of systemic acylanilide fungicides. Part I. Crystal structure and molecular conformation ofdl-methyl-N-(2,6-dimethylphenyl)-N-(2-methoxyacetyl) alaninate

The crystal structure of metalaxyl (C₁₅H₂₁NO₄) was determined by three-dimensional X-ray analysis from diffractometer data. The crystals are monoclinic,P2₁/c,a=7.851(3) Å,b=13.119(10) Å,c=15.107(7) Å,=101.71(6)°,Z=4,D _x=1.218 g cm^–3, (MoKa)=0.095 mm^–1. FinalR=0.079 for 1203 observed reflections. The dimethylphenyl ring is almost perpendicular to the amidic plane of the molecule.     

Crystal structures of 2-pyrazinecarboxylato silver(I) and ammine 2,3-pyrazinecarboxylato disilver(I)

X-ray analysis has shown that the complexes of silver(I) with the anionic forms of 2-pyrazinecarboxylic and 2,3-pyrazinedicarboxylic acids are three-dimensional network polymers. Ag(C₅H₃O₂N₂) (1) crystallizes in space groupPna2₁ witha=7.028(2),b=11.510(3),c=6.949(2) Å andZ=4. Silver tetrahedral coordination occurs through three ligands: the first one acts as a bidentate chelator (Ag–O=2.539(4), Ag–N=2.334(4)Å), the second one involves one N pyrazine atom (Ag–N=2.196(4)Å) and the third one bonds through one O-carboxylato atom (Ag–O=2.323(4)Å). The dinuclear complex Ag₂(C₆H₂O₄N₂)(NH₃) (2) crystallizes in space groupP2₁/c witha=7.775(2),b=16.455(2),c=7.174(1) Å, -115.21(1)° andZ =4. Each of the two silver atoms shows a trigonal environment. The first silver atom involves two O carboxylic atoms (Ag–O=2.312(4), 2.374(4)Å) and one N pyrazine atom (Ag–N=2.277(3)Å) belonging to three different ligands. The second one involves one O carboxylic atom (Ag–O=2.364(3)Å) and one N pyrazine atom (Ag–N=2.304(4)Å) from the same chelating ligand and one N ammine atom (Ag–N=2.158(5)Å).     

Crystal structure of aquo (hydroxo) (ethylenediaminetetraacetato) sodium(I) tin(IV), NaSn(OH)(edta)(H2O)

NaSn(OH)(edta)(H₂O) is monoclinic, space groupP2₁/c, witha=9.747(3)Å,b=9.121(3)Å,c=16.430(6)Å, =98.69(4)°, ų, andZ=4. The coordination environment of Sn(IV) is a capped octahedron. Sn–O distances range from 1.990(6)Å to 2.351(7)Å. Na(I) is five coordinated to three different edta molecules. Na–O distances range from 2.283(9)Å to 2.414(7)Å. The edta ligand presents the E, G/R conformation. The crystal structure is composed of sheets parallel to (001): inside a sheet Sn(OH)(edta) molecules are connected to each other by the Na(I) interactions.     

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.     

Molecular structure of ThBr4(DME)2 (DME = 1,2-dimethoxyethane)

The molecular structure of ThBr₄(DME)₂ (DME = 1,2-dimethoxyethane), the first structurally characterized thorium complex containing a simple bidentate ether ligand, is described. The eight-coordinate complex presents a distorted dodecahedral geometry, with Th—Br and Th—O bond lengths in the ranges 2.8516(13)–2.8712(13) Å and 2.564(8)–2.620(8) Å, respectively. ThBr₄(DME)₂ is monoclinic, space group P2₁/n, a = 7.672(1), b = 14.581(1), c = 15.847(2) Å, = 102.24(1)°, V = 1732.4(3) ų, and Z = 4.     

Refinements of the crystal structures of 1,4-diphenylbutadiyne and its complex with two moles of Co2(CO)6

1,4-diphenylbutadiyne, C₁₆H₁₀, crystallizes in monoclinic space group P2₁/n witha=6.6152(6),b=6.0768(7),c=14.634(1) Å, =100.981(8)⁰,V=577.5(2) ų,Z=2. The structure was refined toR=0.077 andR _w=0.069 for 1007 observed reflections with CuK radiation. The molecule lies on an inversion center. Our determination represents and increase in precision of a factor of approximately three over the original determination. The 21 cobalt complex, C₁₆H₁₀[Co₂(CO)₆]₂, also crystallizes in monoclinic space group P2₁/n witha=8.9568(12),b=17.7057(10),c=18.5671(12) Å, =90.606(12)^o,V=2944.3(5) ų,Z=4. The structure was refined toR=0.032 andR _w=0.031 for 4312 observed reflections. The diphenylbutadiyne triple bonds elongate to 1.346(3) Å and the angles at the diyne C atoms decrease to 134.1(3)–144.9(3)^o upon complexation. The Co-Co distance is 2.4580(4)Å. Our data represent an increase in precision by a factor of 2–3 over the original determination.     

The crystal structure of tris(4-methylpyridine) tricarbonylmolybdenum(0)

The title compound, Mo(4-CH₃C₅H₄N)₃(CO)₃, is monoclinic, P2₁/c, with cell dimensionsa=10.385(1),b=13.572(2),c=15.522(2) Å, =105.08(1)°,Z=4. The complex isfac-octahedral with approximate three-fold symmetry. The Mo–C bond lengths are 1.901–1.904(7) Å, distinctly shorter than in the parent Mo(CO)₆, and the Mo–N bond lengths are 2.297–2.331(5) Å.     

Schiff bases and their complexes with metal ions. Part II. Structures of N-n-butyl-2-hydroxy-1-naphthaldimine and bis[N-n-pentyl-2-hydroxy-1-naphthaldiminato]nickel(II)

The Schiff base ligand (1), [C₁₅H₁₇NO] crystallizes in the monoclinic space group P2₁/c witha=10.054(3),b=10.313(3), c=13.173(4)Å, =107.42(4)°,V=1303.2(7)ų,Z=4,Dx=1.159 g cm^–3, and (MoK)=0.674 cm^–1. The C2-O[1.23(1)Å] and C3–C4 [1.33(2)Å] bond lengths are short, due to its quinoidal structure. In the Schiff base nickel complex (2), [Ni(C₁₆H₁₈NO)₂] the asymmetric unit is comprised of two half-complexes. It crystallizes in the triclinic space group witha=5.124(3),b=16.227(3),c=16.886(4)Å, =95.47(8), =96.00(1), =90.71(4)°,V=1389.6(9) ų,Z=2,Dx=1.289 g cm^–3, and (MoK) =12.1 cm^–1. The coordination of the Ni(II) ions are square planar with bond angles between 87.9(1) and 92.1(1)°. The Ni–O and Ni–N distances are 1.819(2), 1.922(2) and 1.823(2), 1.914(3)Å in these two complexes.     

Crystal and molecular structure of 2-(p-tolyl)-2-dehydrosparteine

The formula of the title compound is C₂₂H₃₀N₂,M _T =322.5; monoclinic:P2₁,a=7.569(3),b=9.381(1),c=13.684(4) Å,=105.81(2)°,Z=2,V _c =933.7 ų,D _x =1.15 g cm^–3,(CuK)=5.1 cm^–1. The sparteine skeleton (bis-quinolizidine system) has atrans-trans configuration. RingA has an intermediate form between the sofa and half-chair conformations, ringsB andD-chair, and ringC-boat conformations, respectively. The double bond C(2)=C(3) is equal to 1.343(9) Å. The phenyl ring is planar and makes an angle with a plane through N(1), C(2), C(3), and C(4) atoms equal to 43.9°.     

Low-temperature,high-resolution crystal structure study of tricyclo[3.3.1.13,7]decan-2-ol (adamantanol-2)

The structure of the title compound (C₁₀H₁₅OH) was determined by X-ray diffraction at liquid nitrogen temperature. The crystals are triclinic, spacegroupP¯1 witha=11.3686(5),b=11.3990(5),c=11.4353(6) Å,=82.193(4),=70.211(4) and =62.279(4)°,V _c =1233.9(1) ų,Z=6,F(000)=504,D _x =1.229 g cm^–3; MoK radiation, =0.71073 Å,(MoK)=0.7 cm^–1. FinalR factor=0.046 andwR=0.062 for 8162 reflections withI>2.5(I). The asymmetric unit consists of three independent adamantanol-2 molecules which together with the three symmetry-related molecules form a cluster having pseudo ¯3 symmetry. The six molecules in the cluster are connected by six O-HO hydrogen bonds, the oxygens of which constitute an almost ideal chair conformation.     

Crystal structures of difluoro[2-(4-methoxyphenyl)-3-oxo-3-phenylpropanalato]boron(III), [BF2(C16H13O3)], and bis[2-(4-methoxyphenyl)-3-oxo-3-phenylpropanalato]copper(II), [Cu(C16H13O3)2]

The crystal structures of difluoro[2-(4-methoxyphenyl)-3-oxo-3-phenylpropanalato]boron(III), [BF₂(C₁₆H₁₃O₃)], and bis[2-(4-methoxyphenyl)-3-oxo-3-phenylpropanalato]copper(II), [Cu(C₁₆H₁₃O₃)₂], have been determined by single-crystal X-ray diffraction methods. The structures were solved by direct methods and electron density calculations and were refined by the full-matrix least-squares method. Difluoro[2-(4-methoxyphenyl)-3-oxo-3-phenylpropanalato]-boron(III) crystallizes as yellow rhombs in the monoclinic space groupP2₁/c witha=11.429(3),b=11.364(4),c=11.412(4) Å,=92.19(2)°,V=1481.0(8) ų andZ=4. A total of 2754 unique reflections were collected. Of these 1342 were considered observed [I>3(I)] leading to a finalR-value of 0.045. Boron is tetrahedrally coordinated to the two fluorine atoms and to two oxygen atoms of the bidentate 2-(4-methoxyphenyl)-3-oxo-3-phenylpropanalato ligand, C₁₆H₁₃O ₃ ^– . Average bond distances: C-C (aromatic) 1.378(10) Å, B-O 1.473(7) Å and B-F 1.343(4) Å. bis[2-(4-Methoxyphenyl)-3-oxo-3-phenylpropanalato]copper(II) crystallizes as dark yellow-green plates in the monoclinic space groupC2/c witha=23.410(7),b=13.856(3),c=8.039(3) Å,=101.79(2)°,V=2553(1) ų andZ=4. Of the unique set of 3076 scanned reflections 2401 hadI>3(I) for whichR became 0.040. Copper is coordinated to four oxygen atoms, two from each of the two bidentate 2-(4-methoxyphenyl)-3-oxo-3-phenylpropanalato ligands, in a distorted square planar manner. The molecule hasC ₂ symmetry. Average bond distances: C-C (aromatic) 1.383(6) Å and Cu-O 1.896(8) Å. The crystals of both compounds consist of monomeric molecular complexes held together by van der Waals forces.