Crystal structure of 3 -acetoxy-17 -iodo- 5 -androstenes

The crystal structure of 3β-acetoxy-17α-iodo-Δ⁵-androstene (C₂₁H₃₁O₂I) has been determined from three-dimensional X-ray data and refined to a final reliability index of R = 5.1% for the 2352 observed reflexions. Crystals grown from methylene chloride/methanol are orthorhombic, space group P2₁2₁2₁, with cell constants a = 6.430, b = 10.563, c = 29.369 Å.     

Crystal and molecular structure of bis(N,N-dipropyl-N′-diphenoxythiophosphoryl-thioureato) nickel(II) [(C6H5O)2P(S)NC(S)N(C3H7)2]2Ni

The Ni complex [C₆H₅O₂P(S)N(C₃H₇₂]₂Ni is monoclinic, space group P2₁/n with a = 8.890(3), b = 21.692(5), c = 11.670(4) Å, β = 108.35(5)°, V = 2136(1) ų, F(000) = 916, M_r = 534.01, Z = 2, D_m = 1.318, D_x = 1.358 Mg m^?3, graphite monochromatized MoKα ^? radiation, π = 0.7107 Å, μ = 0.76 mm^?1, T = 293 K. The structure was solved by a heavy atom method and refined to R = 0.044 for 3095 independent reflexions. The Ni atom lies in the centre of symmetry and is coordinated by four S atoms of the two molecules of the ligand in a planar arrangement. Ni? S bond lengths are 2.205 and 2.226 Å resp., the angles S? Ni? S are 97.65 and 82.35° resp.     

The Structure of the Antibiotic Hedamycin. V. Crystal structure and absolute configuration

The crystal structure of the antibiotic hedamycin ( 1 ) has been solved by direct method and refined by least squares techniques to R = 0.091 for 2289 of 2643 independent reflexions. Crystals of C₄₁H₅₀N₂O₁₁ are orthorhombic, space group P2₁2₁2₁ with lattice parameters a = 24.239 (12), b = 21.440 (10), c = 7.369 (4) Å, Z = 4. The structural features of hedamycin derived earlier by chemical and spectroscopical means are confirmed. Optical rotation and circular dichroism indicate that hedamycin ( 1 ) has the absolute configuration of the related antibiotic kidamycin ( 3 ). The conformation of ring F is a chair form with the aryl substituent almost axial. The bioxirane part of the antibiotic is in a synclinal conformation.     

The crystal structure of tetrachloro(diethylphthalate)titanium(IV)

The crystal structure of [C₆H₄(OCOC₂H₅)₂TiCl₄], which in the presence of activators is a good catalyst for olefin polymerization, has been determined by X-ray diffraction methods and refined by full-matrix least-squares techniques to R = 0.045 for 2000 independent non-zero reflexions. Crystals are orthorhombic, space group Pnma, with four molecules in a cell of dimensions: a 11.45(1), b 14.07(1), c 10.56(1) Å. The structure consists of discrete molecules possessing crystallographic m (C_s) point symmetry. The Ti atoms are octahedrally coordinated by four chlorine atoms and two carbonyl oxygen atoms of diethylphthalate. The chelating ligand atoms together with the titanium atom form a seven-membered ring with the Cl and Ti atoms located above the benzene ring.     

Darstellung und Kristallstruktur von Blei(II)-monoglycerat

Preparation and Crystal Structure of Lead(II) Monoglycerolate Crystals of lead(II) monoglycerolate, of a quality suitable for diffraction studies, have been prepared from an alkaline plumbate solution and an excess of glycerol. The compound crystallizes in the monoclinic space group P2₁/c with a = 5.617(6) Å, b = 9.471(8) Å, c = 9.726(7) Å, β = 102.65(11)°. The structure was refined by full matrix least-squares techniques to an R value (1026 F₀) of 0.078. The compound to which the formula Pb(C₃H₆O₃) could be assigned, is polymeric in one direction. The lead and a part of the oxygen atoms built up a zig-zag chain parallel to the aaxis. The oxygen form a distorted tetragonal pyramid with lead at the apex. A decomposition temperature of 235°C has been determined.     

Synthesis, structure and characterization of binuclear copper(Ⅱ) complexes

At room temperature, dibenzoyl peroxide undergoes oxidative addition reaction with metallic copper powder and pyridine N-oxide (triphenylphosphine oxide or 2,9-dimethyl-4,7-diphenyl-1,10-phenanthrolin) which affords the last products as binuclear copper(II) complexes, [Cu(C5H5NO)-(C6H5COO)2]2(1), [Cu(OPPh3)(C6H5COO)2]2(2) and [Cu(C6H5COO)(C26H2oN2)](3, C26H2oN2 is 2,9-dimethyl-4,7-diphenyl-1,10-phenanthrolin). The structure of the complexes were characterized by elemental analyses, IR spectra, TG-DTA and magnetic property. Crystals(1) are triclinic, space group P1,a=0.92617(36),b=1.06973(17), c=1.08813(29) nm, a=59.60(2)°, β=74.83(3)°,γ=72.80(2)°, V=0.880 nm3, Dc=1.520 g/cm3, Z=1, R=0.044, Rw=0.048, Mr=805.78, 3477 reflections with I > 3σ(I). Each copper(Ⅱ) ion is coordinated by two bridging bidentate benzoate ligands and one pyridine N-oxide or triphenylphosphine oxide to form dimeric binuclear molecules. The structure of the compound(1) shows a clear centre of symmetry.     

Präparation und Charakterisierung von PbBr2·C4H10O3 (Diethylenglykol)

Structural Chemistry of PbBr₂·C₄H₁₀O₃ (Diethyleneglycol) Crystals of PbBr₂·C₄H₁₀O₃ have been synthesized and structurally characterized by single‐crystal X‐ray diffraction. PbBr₂·C₄H₁₀O₃ crystallizes monoclinic in space group P2₁/n (No. 14) with a = 9.370(1)Å, b = 10.045(1)Å, c = 21.090(1)Å, β = 98.98(1)° and Z = 8. The compound contains compact Pb—Br groups, which build colums parallel to [0 1 0] direction by Hydrogen Bonding.     

The crystal and molecular structure of 6-oxadihydrouracil

The crystal and molecular structure of 6-oxadihydrouracil (C₃H₄N₂O₃) has been determined by single crystal x-ray diffraction techniques. The compound crystallizes in the space group P2₁ 2₁ 2₁ with four molecules in a unit cell of dimensions: a = 5.106(1)Å, b = 12.461(2)Å and c = 7.112(1)Å. The structure was solved by direct methods and refined to a final value of R = 0.052. The oxauracil ring is non-planar with the C5 atom assuming tetrahedral geometry and the ring oxygen having oxazinal distances and angle (C-O = 1.43₂Å, N-O = 1.40₈Å, and CON angle of 109.0°). The usual hydrogen bonding patterns associated with the uracil ring are absent in this compound.     

Structural study of 5-methoxyfuro[3,2-e]imidazo[1,2-c]pyrimidine

The nmr and X-ray diffraction data of the novel ring system furo[3,2-e]imidazo[1,2-c]pyrimidine are reported in this paper. The crystal and molecular structure of this compound (C₉H₇N₃O₂·1/2H₂O) has been solved at room temperature. Crystals are monoclinic in a space group of P2/n with cell constants a = 9.982(8), b = 13.526(9) and c = 13.981(9) Å, β = 107.44(5)°, V = 1800.9 ų, Z = 8, D_x = 1.462 Mg·m^?3. The structure was solved by full matrix least square refinement giving a final R = 0.054 (Rw = 0.069) for 1263 reflections (I>3.0σ(I)). The compound is essentially planar, existing in two slightly structural different forms, A and B. These are held in pairs with symmetry related molecules by hydrogen bonds formed with two water molecules. Then the dimeric units are stacked parallel to the c axis to form the tridimensional packing.     

The crystal and molecular structure of an unusual49 heterocycle,62 2-thia-1,3,5-triaza-7-phosphaadamantane 2,2-dioxide51

The crystal and molecular structure of 2-thia-1,3,5-triaza-7-phosphaadamantane 2,2-dioxide (C₅H₁₀SPO₂N₃) has been determined by single crystal x-ray diffraction techniques. The compound crystallizes in the space group P2₁/c with four formula weights per unit cell of dimensions a = 6.129 (1) Å, b = 12.440 (2) Å, c = 14.028 (2) Å, β = 127.31 (1)°. The structure was solved by direct methods and refined to a final value of R = 0.079.     

Synthesis and crystal structure of benzyltrimethylammonium dicitratoborate monohydrate

Benzyltrimethylammonium dicitratoborate [C₆H₅CH₂N(CH₃)₃][(C₆H₆O₇)₂B] · H₂O (I) has been synthesized and separated out in the form of single crystals for the first time. Its crystal structure has been studied by X-ray diffraction. Crystals are triclinic with a = 10.0832(2) Å, b = 11.1232(3) Å, c = 11.9617(3) Å, α = 84.874(1)°, β = 73.520(1)°, γ = 85.550(1)°, Z = 2, space group P-1. The structure has been solved by direct methods and refined by the full-matrix least-squares technique in the anisotropic approximation up to R = 0.0485 (Bruker-Nonius KappaCCD automatic diffractometer, λMoK _α). The crystal structure of compound I is based on centrosymmetric dimers that consist of complex anions and water molecules and linked by the system of hydrogen bonds into a three-dimensional framework. The crystals of compound I contains five asymmetric O-H...O hydrogen bonds. A specific feature of the structure is the formation of -COO...H...H₂O hydrogen bonds, in which the carboxyl proton is considerably shifted towards the water molecule.     

CHIRAL METAL COMPLEXES. 30 THE CRYSTAL AND MOLECULAR STRUCTURES OF A-β-[DINITRO{N,N′-BIS(2-PICOLYL)-lR,2R-DIAMINOCY CLOHEXANE}COBALT(III)] PERCHLORATE MONOHYDRATE,AND α-β-EXO-[DINITRO{ 3R-METHYL-1,6-BIS(2-PYRIDYL)-2,5-DIAZAHEXANE}COBALT(III)] PERCHLORATE MONOHYDRATE

Abstract

The structures of two Co(III) complexes containing N-bonded nitrite ions and one of the N⁴ tetradentate ligdnds R,R-picchxn (N,N'-bis(2-picolyl)-1 R,2R-diaminocyclohexane) or R-picpn (3R-methyl-1,6-bis(2-pyridyl)-2.5-diazahexane) have been determined by X-ray analyses. A-β-[Co(R,R-picchxn)(NO₂)₂1 CLO₄,.H₂O is triclinic. space group P1, with a = 8.611(2), b = 9.188(1), c = 8.576(1) Å, α = 117.60(1), β = 96.40(1). γ = 73.69(1)° and Z = 1. The structure ivas refined by full-matrix least-squares methods to R = 0.035 for 2712 non-zero reflexions. δ-β-eso-[Co(R-picpn) NO₂)₂]CIO₄,.H₂O is orthorhombic, space group P2₁2₁2₁. with a = 7.664(1). b = 15.121(3). c = 18.429(4) a and Z = 4. The structure was refined as above to R = 0.040 for 2063 non-zero reflexions. In the R.R-picchxn complex both amine nitrogen atoms of the tetradentate have the same relative configuration, Hhereds in the R-picpn diastereoisomer their relative configurations are opposite. In the latter complex this permits the exo methyl group substituent to adopt a nearly ideal equatorial position in the central chelate ring. Hydrogen bonding networks in the two structures. which link the complex cations to the perchlorate ions and lattice water molecules, are apparent.     

The crystal and molecular structure of 12,13-dibromopseurotin.

The crystal structure of 12,13-dibromopseurotin has been determined by single crystal X-ray analysis. The crystals belong to space group P2₁ with a = 16.75, b = 9.63, c = 7.42 Å, β 95.9°, Z = 2. The structure was solved by the heavy atom technique and refined to R = 0.062 with 819 significant reflexions for 299 parameters.     

Crystal and molecular structure of the ethanol solvate of 2-[bis(diphenylphosphoryl)methyl]phenol

Crystal and molecular structure of the ethanol solvate of 2-[bis(diphenylphosphoryl)methyl]phenol, C₃₁H₂₆O₃P₂·3/4 C₂H₅OH (I), was determined by X-ray diffraction analysis. Crystals I are monoclinic: a=11.896(3), b=17.207(3), c=28.421(6) Å, β=90.75(2)°, Z=8, space group P2₁/c. The structure of I was solved by direct methods and refined anisotropically by large-block least-squares analysis to R=0.066 (CAD-4 automatic diffractometer, λMoK_α radiation, 3650 independent reflections with I≥3σ). The crystal structure of I contains two independent molecules, Ia and Ib, of the basic substance and two independent solvate molecules of ethanol. The P atoms in molecules Ia and Ib have distorted tetrahedral environments; the average bond lengths are: P=O 1.476(3), P-C(sp³)=1.833(4) and P-C(Ar)=1.809(4) Å. Molecule Ia has an approximate symmetry plane C_s. The conformation of molecule Ib differs from that of Ia in rotation of one diphenylphosphoryl substituent around the P-C(sp³) bond by an angle of ≈34°. In molecule Ia, the O=P-C-P=O fragment has the form of a chela with two nearly parallel P=O bonds. In the crystal structure of I there are O-H...O=P intermolecular H-bonds; in molecules Ia and Ib there is an intramolecular H-bond of C-H...OH type.     

Einfach und doppelt deprotonierte Maleinsäure in Praseodym‐hydrogenmaleat‐octahydrat,Pr(C4O4H3)3 · 8 H2O,und Praseodym‐maleatchlorid‐tetrahydrat,Pr(C4O4H2)Cl · 4 H2O

Single and Double Deprotonated Maleic Acid in Praseodymium Hydrogenmaleate Octahydrate, Pr(C₄O₄H₃)₃ · 8 H₂O, and Praseodymiummaleatechloride Tetrahydrate, Pr(C₄O₄H₂)Cl · 4 H₂O Single crystals of Pr(C₄O₄H₃)₃ · 8 H₂O grew by slow evaporation of a solution which had been obtained by dissolving Pr(OH)₃ in aqueous maleic acid. The triclinic compound (P1, Z = 2, a = 728.63(3), b = 1040.23(3), c = 1676.05(8) pm, α = 72.108(2)°, β = 87.774(2)°, γ = 70.851(2)°, R_all = 0.0261) contains Pr³⁺ ions in ninefold coordination of oxygen atoms which belong to two monodentate maleate ions and seven H₂O molecules. There is one further non‐coordinating maleate ion and one crystal water molecule in the unit cell. Thermal treatment of Pr(C₄O₄H₃)₃ · 8 H₂O leads first to the anhydrous compound which then decomposes to the respective oxide in two steps upon further heating. Evaporation of a solution of Pr(C₄O₄H₃)₃ · 8 H₂O which contained additional Cl^– ions yielded single crystals of Pr(C₄O₄H₂)Cl · 4 H₂O. In the crystal structure (monoclinic, P2₁/c, Z = 4, a = 866.0(1), b = 1344.3(1), c = 896.9(1) pm, β = 94.48(2)°, R_all = 0.0227), the Pr³⁺ ions are surrounded by nine oxygen atoms. The latter belong to four H₂O molecules and three maleate ions. Two of the latter act as bidentate ligands.     

The crystal and molecular structure of dl-BI-(o-trimethyl-cis-brazilane)

X-ray crystallographic analysis has established the crystal and molecular structure of the title compound, C₃₈H₃₈O₈. The monoclinic crystals belong to the centrosymmetric space group P2₁/c, with a = 16.701(5), b = 8.037(2), c = 23.600(9) Å, β = 93.10(2)° and Z=4. The structure was solved by direct methods from diffractometer data measured with CuKα radiation, and refined to a final R index of 0.081 for the 2088 observed terms. The dimeric molecule has approximate two-fold symmetry and its presence in the unit cell in both chiralities forms a racemic structure. The three central bonds, C(10)-C(11), C(11)-C'(11), C'(11)-C'(10), are significantly elongated with a mean value 1.59 Å.     

Molybdännitridtrichlorid-di-n-butylether, [MoNCl3 · O(C4H9)2]4; Darstellung,IR-Spektrum und Kristallstruktur

Molybdenum-nitride-trichloride-di-n -butylether [MoNCls₃ · 0 (C₄H₉)₂]₄; Preparation, I.R. Spectrum, and Crystal Structure Phenyldiazonium tetrachloronitridomolybdate, C₆H₅N₂[MoNCl₄], was obtained in the form of orange-red crystals from phenyldiazonium chloride and molybdenum nitride chloride in POCl₃ suspension. In boiling di-n-butylether it decomposes to chlorobenzene and the title compound which is obtained in the form of dark red crystals, sensitive to moisture. [MoNCl₃ · O(C₄H₉)₂]₄ can also be obtained directly from MoNCl₃ and dibutylether. It crystallizes in the monoclinic space group P2₁/c with two tetrameric molecules per unit cell. The lattice constants are at ?49°C a = 1 283, b = 1 170, c = 1 922 and β = 94.11°. The crystal structure was determined with the aid of X-ray diffraction data and was refined to a residual index of R = 0.047 for 1951 observed reflexions. In the [MoNCl₃ · O(C₄H₉)₂]₄ molecule the Mo atoms form a square; they are linked with one another via the N atoms with alternating Mo? N distances of 165 and 215 pm, which indicate triple and single bonds, respectively. In the position trans to the shorter Mo?N bond, the ether molecule is bonded by its oxygen atom. The I.R. spectra of C₆H₅N₂[MoNCl₄], C₆H₅N₂[MoCl₆], and [MoNCl₃ · O(C₄H₉)₂]₄ are recorded.     

Crystal and molecular structure of tris(3,3,4,4-tetramethyl- 3,4-dihydrodiazete)bis(tricarbonylchromium), (N2C2Me4)3[Cr(CO)3]2

Crystals of C₂₄H₃₆N₆O₆Cr₂ are monoclinic, a 15.380(3), b 13.965(2), c 14.459(3) Å, β 92.18(1)°; Z = 4; space group P2₁ with two independent molecules in the asymmetric unit. The crystal structure was determined from X-ray diffractometer data by direct methods and refined by least-squares methods to R = 0.066 for 2430 independent observed reflections. It consists of discrete molecules, in which each Cr atom is surrounded by three cis carbonyl groups and three cis nitrogen atoms of three 3,3,4,4-tetramethyl-1,2-diazetine ligands, in a deformed octahedral coordination. There is no evidence of intramolecular Cr ? Cr interaction.     

Synthesis,X-ray structure and spectroscopy of Cu(II) complexes derived from diacetylazine dioxime

Complexes of Cu(II) with the polydentate diacetylazine dioxime ligand C₈H₁₄N₄O₂ have been synthesized by template and non-template reactions. The crystal structure of [Cu(C₈H₁₃N₄O₂)]₂[ClO₄]₂(C₂H₅OH)₂ has been determined to establish the conformation of the ligand and the coordination of the oxime function. The structural analysis shows that the nearly planar [C₈H₁₃N₄O₂]^? group behaves as a bridging tetradentate ligand. The distorted square-pyramidal coordination about each Cu atom includes three N donors from two oxime and azine and one O donor from the other oxime, the ethanol molecule occupying the apical position. A perchlorate anion is loosely bonded to Cu. The intramolecular Cu…Cu separation is 3.725(2) Å. The compound crystallizes in the centrosymmetric space group P$\text{1}$ triclinic lattice with refined lattice parameters of a = 11.963(8) Å, b = 9.784(7) Å, c = 7.501(6) Å, α = 90.69(4)°, β = 104.53(4)°, γ = 90.83(4)°, V = 849.7 ų and Z = 2. Full-matrix least-squares refinement of 1490 independent reflexions led to final discrepancy indices, R = 0.059, and R_w = 0.065. The Cu centres are highly coupled as indicated by the ESR spectrum. There is no evidence that the C₈H₁₄N₄O₂ ligand stabilizes unusual oxidation states of Cu.     

Synthesis,characterization and crystal structure of the anilinium β-octamolybdate dihydrate

The anilinium β-octamolybdate dihydrate has been prepared in acidic aqueous solution. TG, DTG, IR and ¹H NMR techniques have been used to identify the compound. It belongs to a series of molybdates of alkyl-N- and -N,N-substituted anilinium cations. Single crystals have been analyzed by X-ray diffraction. Crystal data are: (C₆H₈N)₄[Mo₈O₂₆] · 2H₂O, space group P$\text{1}$, Z = 1, a = 10.007(1), b = 8.014(2), c = 14.645(8)Å, α = 109.81(3), β = 108.59(2), γ = 85.44(2)°, V = 1052.9(6) ų, D_o = 2.49(1), D_x = 2.52 mg m^?3, R = 0.026 and R_w = 0.031 for 5297 observed reflexions. The crystal structure consists of discrete [β-Mo₈O₂₆]^4? polyanions, two crystallographically independent (C₆H₈N)⁺ cations and one independent water molecule. Polyanions are linked to the cations and to the water molecules by hydrogen bonds of types NH…O and OH…O.