Crystal and molecular structure of (2-amino-4-methyl-1-pyridinio) cyanoborane

The crystal structure of the title compound, C₇H₁₀N₃B, has been determined by X-ray diffraction using CuK radiation. The crystals are monoclinic,P2₁/c witha=6.941(2),b=15.961(3),c=7.739(2) Å,=90.5(2)° andZ=4. The structure was solved by direct methods, and refined by full matrix least squares to a finalR-value of 056 with 833 observed reflections. The molecule is in the elongated form, but is not planar; the torsion angle C(2)-N(1)-B-C(8) is 82.9(4)°. The bond distances N(1)-B=1.587(5) Å; B-C(8)=1.586(6) Å; C(8)N(3)=1.134(5) Å. The B-C-N moiety is slightly [176.9(4)°] nonlinear. The molecules are linked by weak hydrogen bonds N(2)-H(1N)N(3), N(2)-N(3)=3.055(5) Å and N(2)-H(2N)N(3), N(2)-N(3)=3.165 Å.     

Molecular and crystal structure of 2-amino-6-dimethylamino-4-(tricyclo[3.3.1.13, 7]dec-1-yl) methyl-1,3,5-triazine

The crystal and molecular structure of the title compound has been determined by X-ray crystallographic studies. The compound crystallizes in the triclinic space groupP¯1 witha=10.777(8) Å,b=13.003(9) Å,c=13.045(8) Å, =72.26°(4),=104.25°(5), =108.87°(5) andZ=4. The structure was solved by direct methods and full-matrix least-squares refinement converged to a finalR=0.083 for 2656 observed reflections. The two independent molecules differ only in orientation of the adamantyl moiety. Both of them utilize the two hydrogens of the amine nitrogen N(7) to make hydrogen bonds linking the molecules into infinite chains which are held together by van der Waals interactions. The conformation of the substituents at position 6 of the triazine ring is such that the torsion angle is close to 0° for both independent molecules of the asymmetric unit.     

Studies of substituted quinoxaline-di-N-oxides. Part 1. Crystal structure and molecular conformation of 2-[N-(2-hydroxyethyl)carboxamide]-3-methylquinoxaline 1,4-dioxide

A single crystal X-ray investigation of the yellow 2-[N-(2-hydroxyethyl) carboxamide]-3-methylquinoxaline 1,4-dioxide, a commercially available growth promoter used in agricultural stock farming, shows that the molecule is planar. The dihedral angle between the benzene and heterocyclic rings is 0.5°. The N(1)-O(1) and N(2)-O(2) distances are: 1.286(1) and 1.304(1) Å. The C(1)-C(2) bond of the pyrazine ring is not lengthened by substitution at the C(1) and C(2) atoms and is 1.421(2) Å. The atoms O(1) and O(2) deviate by 0.036(2) and 0.123(2) Å from the least-squares plane through the heterocyclic ring. The deviation of the C(12) atom is –0.012(2) Å. The plane through the atoms C(1), C(9), N(3), and O(3) makes an angle of 100.5(2)° with the heterocyclic ring plane. Intermolecular hydrogen bonds O(4)-HO(4)O(3) between the hydroxyl and carbonyl groups generated alternating, antiparalled chains extending in thea direction. The crystals are triclinic,P¯1 (No. 2), witha=7.469(2),b=8.111(2),c=10.357(3) Å,=80.11(2),=88.90(2), =67.73(2)°, andV=571.3(2) ų. The structure was solved by direct phase determination guided by negative quartets and refined by full-matrix least squares to anR value of 0.041 for 2159 observed reflections.Commercially known asOlaquindox.     

X-ray structure and UV spectroscopic studies of (adenmato-N9)triethylphosphinegold(I)

The preparation, characterization, and X-ray structure analysis of (adeninatoN9)triethylphosphinegold(I) is reported. The crystal structure consists of discrete molecules, the adeninate anion coordinates via the N(9) atom with a Au-N(9) bond distance of 2.057(5) Å and the linear geometry about the Au atom is completed by the P atom of a disordered Et₃P ligand; the Au-P(1) bond distance is 2.238(2) Å and the N(9)-Au-P(1) bond angle is 178.8(2)°. The crystals are orthorhombic, space groupPbca, with unit cell dimensionsa=8.528(1),b=17.797(3),c=18.526(2) Å andZ=8. The structure was refined by a full-matrix least-squares procedure to finalR=0.030 andR _w =0.033 for 1749 reflections withI>2.5a(I). The electronic spectrum of the complex dissolved in water in the near ultraviolet is consistent with essentially separate -electron systems of the adenine and phosphinegold moieties; a conclusion which corroborates the X-ray structural results.     

Structure and conformation of 6,8-dinitro-2,4-bis(trichloromethyl)-1,3-benzdioxin: X-ray crystallographic determination

6,8-dinitro-2,4-bis(trichloromethyl)-1,3-benzdioxin is monoclinic,P2₁/c,Z=4,a=12.348(2),b=11.575(3),c=12.183(4) Å,=107.48(2)°. The structure was solved by direct methods, from data collected at room temperature on an Enraf-Nonius CAD4 diffractometer, and refined by least-squares to a finalR value of 0.032 using 2192 reflections. The heterocyclic ring is an envelope structure, the dihedral angle between the plane of the aromatic ring and that containing five of the atoms of the heterocycle being 4.98(6)°. One -CCl₃ group is pseudoequatorial while the (Ar-C)CCl₃ group is pseudoaxial. C-C_eq 1.526(3) Å; C-C_ax 1.537(3) Å; C-C(C_ax)-O 112.4(2)°; C(C_ax)-O-C(C_eq) 115.2(2)°.     

Crystal and molecular structure of bis(tetrathiafulvalene) bis(maleonitrile-1,2-dithiolato)nickelate(II)

The crystal and molecular structure of the title compound, C₂₀H₈N₄S₁₂Ni, is reported. Crystals are triclinic, space groupP¯1 (No. 2) withz=1 in a cell of dimensionsa=8;482(2),b=7.950(2),c=9.976(2) Å,=95.64(2),=98.60(2), and =87.65(2)°. The structure was solved by Fourier methods and refined by the method of least squares toR=0.033 for 2027 unique reflections. The Ni atom has an approximate square-planar configuration with Ni-S(1)=2.179(1), Ni-S(2)=2.175(1) Å, and the S(1)-Ni-S(2) bite angle of 91.89(4)°. The anions and the cations form a mixed stack (DAD-DAD-) along the diagonal of theab plane, showing the possibility of unusual electrical behavior.     

The crystal and molecular structure of bis(melamine)silver(I) perchlorate, Ag(C3H6N6)2ClO4

The crystal structure of the title compound, Ag(mela)₂ClO₄ (mela = melamine), has been investigated by X-ray diffraction techniques, the crystals are triclinic, space group P1¯, with a = 5.236(2), b = 7.5385(9) c = 19.063(3) Å, = 99.91(1), = 90.53(2), = 108.32(2)° and Z = 2. The Ag atom has a coordination geometry with two strong bonds (2.162(2) and 2.179(4) Å) to the nitrogen of the melamines and two weak bonds (2.776(4) and 2.785(4) Å) to oxygen atoms of the ClO^– ₄anions. The N—Ag—N vector is markedly nonlinear (angle at Ag 167.7(2)°).     

Structure and characterization of bis(N-p-chloro-phenyl-salicylideneaminate) Schiff base copper(II) complex: Cu[N-p-Cl-Ph-Sal]2

The crystal and molecular structure of the title compound has been determined by X-ray crystallography. It crystallizes in the monoclinic system, space group P2₁/c, with lattice parameters a = 13.678(3), b = 10.729(2), c = 8.1996(2) Å, = 98.96°, V = 1188.7(4) ų, and Z = 4. The crystal structure contains two centrosymmetric molecules of bis (N-p-chloro-phenyl-salicylideneaminate) Schiff base copper(II). Copper(II) ion is coordinated in a slightly distorted trans square-planar configuration, the distortion consisting of a reduction of the N–Cu–O angle with the chelate rings from the ideal value of 90°. The p-chlorophenyl rings with salicylidene moieties form a dihedral angle of 38.96°.     

X-ray crystal structure of (1-methylthyminato)triethylphosphinegold(I)

The crystal structure of the title compound reveals that the gold atom exists in a linear geometry defined by a P atom [Au-P 2.223(6) Å] and the N(3) atom of the 1-methylthyminate nucleobase [Au-N(3) 2.06(2) Å] with a P-Au-N angle of 178.4(5)°. The crystal lattice is characterized by significant hydrogen bonding contacts involving both the carbonyl oxygen atoms and the solvent water molecule of crystallization. The crystals are monoclinic, space groupP2₁ with unit cell dimensionsa 8.037(1),b=11.329(2),c09.501(1) Å,=104.08(1)°,Z=2. The structure was refined to finalR=0.047 for 2069 reflections which satisfiedI3.0(itI).     

Isomerism in some 1-oxa-3,5-dithians and the X-ray structure determination of 2,6-bis(trichloromethyl)-4-dichloromethylene-1-oxa-3,5-dithian

2,6-bis (trichloromethyl)-4-dichloromethylene-1-oxa-3,5-dithian is triclinic,P¯1,a=10.125(3),b=10.294(3),c=14.631(10) Å,=92.84(5),=96.51(5), =96.18(2)°,V=1503 ų,Z=4. The structure was solved by direct methods, from data collected at room temperature on an Enraf-Nonius CAD4 diffractometer, and refined by least squares to a finalR value of 0.035 using 3961 reflections. The conformation of the molecules is twist-boat, one molecule being almost symmetrically twisted about the O-C(Cl₂) direction. The range of endocyclic O-C-S angles is 111.8(3) to 115.1(3)° and data are given which support the possibility of there being a correlation between the endocyclic O-C(X)-S angle, the C-O-C(X)-C(Cl₃) torsion angle, and the C-S-C(X)-C(Cl₃) torsion angle. The -CCl₃ groups are in pseudoequatorial positions. Average bond lengths (Å) for the two molecules are C-O 1.405, C(sp ³)-S 1.822, C(sp ²)-S 1.759, C-C_eq 1.529 and average endocyclic angles (°) are O 117.3, C (sp ³) 113.5, S 97.4, C(sp ²) 119.3, the esds on the individual bond lengths and angles being in the ranges of 0.003–0.004 Å and 0.2–0.4° respectively.     

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 structure of bis(benzimidazolium) tetrabromocuprate(II)

Stable, dark-violet crystals of (C₇H₇N₂)₂CuBr₄ were obtained from an aqueous solution of CuBr₂, HBr, and benzimidazole. The crystal structure was determined by three-dimensional X-ray analysis. The crystals are monoclinic:C2/c, a=15.651(4),b=7.945(1),c=15.775(4) Å,=91.44(2)°,Z=4,V _c=1960.96 ų,D _x=2.105 g cm^–3. The structure was refined by full-matrix least squares to giveR=0.042 andR _w=0.048 for 1254 intensities above 3(I). The copper(II) ions are four-coordinated in the form of a distorted tetrahedron CuBr₄ ofC ₂ symmetry. Two different Cu-Br bond lengths are observed: Cu-Br(1)=2.426(2), Cu-Br(2)=2.330(2) Å. Only one flattened angle [Br(2)-Cu-Br(2)=132.71(9)°] in the CuBr₄ tetrahedron is noted. The angles Br(1)-Cu-Br(1)=108.83(7), Br(2)-Cu-Br(1)=99.92(5) and Br(2)-Cu-Br(1)=107.13(5)° have been found. Hydrogen bonds explain the deformation of the CuBr ₄ ^2– coordination polyhedron. The structure is compared with other CuX ₄ ^2– complexes.     

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.     

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)°.     

Gold(I)-selenium bond: synthesis and x-ray structure of chloro(triphenylphosphine selenide)gold(I)

The crystal and molecular structures of chloro(triphenylphosphineselenide)gold(I), [(C₆H₅)₃PSe]AuCl, have been determined from three-dimensional X-ray intensity data collected on a CAD4 diffractometer. The compound crystallizes in the triclinic space groupPl witha=9.322(3),b=10.639(5),c=9.252(3) Å, =104.74(4), =99.52(3), =76.97(3)°, andZ=2. Atomic parameters were refined by full-matrix least-squares to anR value of 5.7% for 2591 observed reflections. This is one of the few known examples of linear gold(I) complexes having an Au-Se linkage. The Se-Au-Cl angle is 178.6(1)°, and the Au-Se and Au-Cl distances are 2.371(2) and 2.277(6) Å, respectively. As expected, the Au-Se bond length is 0.10–0.18 Å longer than the Au-S bond length observed in similar two-coordinate linear gold(I) complexes.     

Molecular structure of an extremely crowded iron(II) dihydride complex: FeH2(PMePh2)4

The crystal structure of FeH₂(PMePh₂)₄ shows this to exist as thecis isomer in the solid state with major distortions of the FeP₄ skeleton:cis P-Fe-P angles 98.1(1)–107.2(1)° andtrans P-Fe-P angle 143.3(1)°. All hydrogen atoms were refined, and the mean Fe-H separation is 1.59 Å. Long Fe-P distances, 2.187(3)–2.251(3) Å, emphasize the crowding in this molecule. Crystallographic data:a=11.684(4) Å,b=37.793(17),c=9.765(3),=90.81(1)°, andZ=4 in space groupP2₁/n (No. 14).R(F)=6.3% andR _w (F)=6.0% for 2585 observed reflections collected at —162°C.     

Crystal and molecular structures of two polymorphic forms of dimethyl-N-(2-ethylphenyl)-phosphoramidate (I) and dimethyl-N-(2,6-dimethylphenyl)-phosphoramidate (II)

The crystal structures of the phosphoric amides dimethyl-N-(2-ethylphenyl)-phosphoramidate (I) and dimethyl-N-(2,6-dimethylphenyl)-phosphoramidate (II) have been determined by direct methods and refined by full-matrix least squares. Compound (I) crystallizes in two polymorphic forms, both monoclinicP2₁/c, but with different cell parameters. Parameters for compound (I) are: FormA:a=10.878(5),b=8.890(4),c=25.11(1) Å,=92.18(2)°; FormB:a=7.071(4),b=17.059(9),c=10.221(5) Å,=97.07(2)°. Compound (II) is also monoclinicP2₁/c witha=8.453(4),b=14.231(7),c=10.283(5) Å,=108.95(2)°. Compound (I) exists as a hydrogen-bonded dimer, whereas compound (II) exists as a hydrogen-bonded polymeric species.     

The molecular structure of acetato[2-(pyridin-2′-yl)phenyl]mercury(II)

The crystal structure of the title compound was determined by X-ray crystallography. The compound crystallizes in the monoclinic crystal system witha=8.152(4),b=17.994(7),c=8.634(9) Å, =108.92(5)°, space group P2₁/c (N:14),V=1198.02 ų,Z=4. The mercuryl(II) atom forms two strong, almost colinear bonds (bond angle 176.1(4)°) with a carbon of the phenyl ring (Hg–C=1.99(1) Å) and one of the acetate oxygen atoms (Hg–O(1)=2.005(7) Å). These primary bonds are supplemented by secondary intramolecular interactions with the pyridine nitrogen (Hg...N=2.727(9) Å) and the other acetate oxygen (Hg...O(2)=2.925(8) Å), although the latter is very weak and the acetate anion therefore practically monodentate. Weak additional intermolecular Hg–C and Hg–O(1)interactions contribute to the lattice structure.     

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.     

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.