Crystal and molecular structure of chloro(tri-t-butylphosphino-C,P)triphenylarsinepalladium(II)

(SP-4-4)-chloro[2-(di-tert-butylphosphino)-2-methylpropyl-C,P] (triphenylarsine)palladium(II), C₃₀H₄₁ClPAsPd, has been characterized by single-crystal X-ray diffraction data. It crystallizes in the monoclinic space groupP2₁ witha=9.611(2),b=14.335(2),C=11.953(1) Å,=111.97(1)° andZ=2. The phasing model was determined by direct methods and the full-matrix least-squares refinement of 302 structural parameters yielded a reliability factor of 0.039 for 2269 unique reflections withI> 3(I). The square planar geometry about the Pd atom is angularly distorted due to the steric bulk of the ligands and the formation of the four-membered ring, Pd-P-C(2)-C(1), which is severely distorted. The arsine and phosphine ligands are orientedtrans across the square-planar geometry with an As-Pd-P angle of 163.5(1)°. Details of the structural content and selected bond lengths and angles are discussed. The phenyl rings are planar and in a staggered orientation. Steric bulk illustrations from ligand profile calculations (/2 vs ) about the arsine and phosphine ligands are presented.     

Synthesis,spectroscopic studies,and crystal structure of the first monopyridinium salt of 1,1′-bis-(2-naphthol) sulfone,C25H19NO4S

The crystal and molecular structure of 1,1-bis-(2-naphthol) sulfone monopyridine (3) determined by single-crystal X-ray diffraction is reported. C₂₅H₁₉NO₄S crystallizes in the monoclinic space groupC2/c (No. 15) witha=17.095(4),b=14.574(2),c=18.731(2) Å,=116.29(2)°,Z=8,D _x =1.364 Mg m^–3,D _m =1.353(8) Mg m^–3. The phase problem was solved by direct methods and the final reliability factor obtained from full-matrix least-squares refinement of 2306 independent reflections is 0.067. The unit cell contains eight molecules with intramolecular hydrogen bonding and the molecules in the crystal lattice are held together by van der Waals forces. Conoscopic, infrared, and¹H and C¹³ NMR analyses have been performed. Details of the structural content and selected bond lengths and angles are discussed.     

Characterization and structural analyses of trimethoxy and triethoxybenzo[b]thiophene

The crystal and molecular structures of two methoxybenzo [b] thiophenes have been determined by three-dimensional, single-crystal X-ray diffractometry. Both 3-(3,4,5-trimethoxybenzoyl)-2-(4-methoxyphenyl)-6-methoxybenzo[b]thiophene and 3-(3,4,5-triethoxybenzoyl)-2-(4-methoxyphenyl)-6-methoxybenzo[b]thiophene (hereafter referred to as I and II, respectively) crystallize in the triclinic centrosymmetric space group (No. 2, C¹) with two formula units per cell with a = 6.842(1) Å, b = 12.602(2) Å, c = 13.815(2) Å, = 94.80(1)°, = 98.27(2)°, and = 100.59(2)° and a = 10.600(1), b = 11.415(2), c = 12.137(2) Å, = 94.57(1)°, = 101.18(1)°, and = 110.45(1)°, respectively. The phase problems were solved by direct methods and the respective final full-matrix least-squares refinements converged to R = 0.039 and 0.068. The structures differ in the orientation of the trimethoxy and triethoxy groups of the benzoyl ligands. The molecules in the crystal lattice are held together by van der Waals forces. Selected bond distances, angles, and torsion angles are tabularized as well as reference to the synthesis of the title compounds and peripheral studies.     

Synthesis, characterization, peripheral studies, and structural analysis of E-4-(N-methylanilino)-3-pentene-2-one, C12H15NO

Crystallographic structural refinement of E-4-(N-methylanilino)-3-pentene-2-one (I) has been carried out by means of three-dimensional single-crystal X-ray diffractometry. The title compound crystallizes in space group C2 (No. 5,Z = 4). The lattice constants are a = 21.543(4), b = 6.433(1), c = 8.019(2) Å, and = 97.82(3)°. Characterizations include physical property determinations and spectrometric identifications employing IR, ¹H and ¹³C NMR, and X-ray powder analyses. The molecules in the crystal lattice are held together by van der Waals forces. Selected bond distances and angles are presented and discussed as well as synthesis and peripheral studies.     

Syntheses, characterization, and structural analyses of several f-block isothiocyanatonitrato complexes

Reactions of tetra-n-butylammonium thiocyanate with lanthanide and uranyl nitrates yield complexes of the general type [(Bu)₄N]_x[M(NCS)_y(NO₃)_z]. Samples of [(Bu)₄N]₂ [UO₂(NCS)₃( NO₃)] (1), [(Bu)₄N]₃[Yb(NCS)₄(NO₃)₂] (2), and [(Bu)₄N]₃[Nd(NCS)₄(NO₃)₂rsqb; (3) were prepared from alcohol solutions. Crystallization of 1 occurs in the centrosymmetric monoclinic space group C2/c (No. 15) with a = 17.949(4) Å, b = 16.587(3) Å, c = 16.763(3) Å; = 99.77(3)°; and Z = 4. The seven-coordinate uranium(VI) ion exhibits a pentagonal bipyramid coordination environment. Crystallization of 2 occurs in the centrosymmetric orthorhombic space group Pnnn (No. 48) with a = 12.530(2) Å, b = 12.9440(10) Å, c = 21.203(2) Å; Z = 2. The eight-coordinate ytterbium(III) ion expresses a dodecahedral coordination environment. Crystallization of 3 occurs in the noncentrosymmetric monoclinic space group Cc (No. 9) with a = 16.556(2) Å, b = 18.130(2) Å, c = 23.984(4) Å; Z = 4. The 10-coordinate neodymium(III) ion exhibits a dodecahedral coordination environment. Characterization includes physical property determinations, conoscopic studies, IR spectroscopic identifications, and UV spectral data. Details of the syntheses along with selected bond distances and angles are presented and discussed.Deceased, 30 March 1999     

X-ray structures of two methoxybenzo[b]thiophenes

The crystal and molecular structures of two methoxybenzo[b]thiophenes have been determined by three-dimensional, single-crystal X-ray diffractometry. Both 3-(4-hydroxy-3, 5-dimethoxybenzoyl)-2-(4-methoxyphenyl)-6-methoxybenzo[b]thiophene and 3-(2,6-dimethoxybenzoyl)-2-(4-methoxyphenyl)-6-methoxybenzo[b]thiophene (hereafter referred to asI andII, respectively) crystallize in the monoclinic centrosymmetric space groupP2₁/n (No. 14, C _2h ⁵ ) with four formula units-per cell witha=6.866(1),b=28.638(2),c=11.830(2) Å, and =105.52(1)° anda=9.328(1),b=7.977(1),c=29.650(4) Å, and =97.87(1)°, respectively. The phase problems were solved by direct methods and the respective final full-matrix least-squares refinements converged toR=0.046 and 0.031. The structures differ in the positioning of the dimethoxy groups of the benzoyl ligands and the addition of a hydroxyl group inI. The molecules in the crystal lattice are held together by van der Waals forces plus the addition of hydrogen bonding in compoundI. Selected bond distances and angles and torsion angles are tabularized.     

Structure analysis of (3S)(2-oxo-6-thioxo-3-piperidinyl)-phenylmethylcarbamate,C13H14N2O3S

The crystal structure of (3S)(2-oxo-6-thioxo-3-piperidinyl)-phenylmethylcarbamate (I) has been determined from three-dimensional single-crystal X-ray diffraction data. This compound crystallizes in the monoclinic noncentrosymmetric space group P2₁ (No. 4, C ₂ ² ) withZ=2 anda=5.737(2),b=8.908(2),c=13.402(2)Å, and =10034(2)°. The phase problem was solved by direct methods and the standard difference-map technique. The final least-squares full-matrix refinement based on 1832 unique reflections yielded a reliability factor of 0.043. Bond lengths and angles are internally consistent and the molecules in the crystal lattice are held together by van der Waals forces and hydrogen bonding. Important geometric details are tabularized. Infrared,¹H and¹³C NMR, and UV spectral results are presented and discussed.Formerly M. L. Fink.     

X-ray crystal structure ofcis-H(Ph3Si)Pt[Ph2P(CH2)4PPh2] ·0.5 C6H6

The title compound, cis-hydrido(triphenylsilyl)-1,4-butanediyl-bis-(diphenylphosphine)platinum(II) (I), crystallizes in the monoclinic space groupP2 ₁/n (No. 14) witha=9.472(4),b=16.924(5),c=25.799(4) Å, β=91.29(3)° andZ=4. The structure was solved using the direct methods and refined by the full-matrix least-squares procedure to yield residuals ofR=0.024 andR _w =0.025 based on 4160 unique reflections. The square-planar geometry about the Pt atom is angularly distorted with P(1)?Pt?P(2) and Si?Pt?P(2) angles of 103.5(1) and 102.1(1)°, respectively. The Pt?P(1) bond is longer than the Pt?P(2) bond due to thetrans influence of the SiPh₃ group. Distortion due to steric bulk of the ligands is accommodated by the opening of the tetrahedral angles at the silicon and phosphorous atoms.