AbstractThe Title Compound Research Articles

Structure of 2,6-di-(4-tert-butylphenyl)-4,4′-biphenyl-4H-pyran

Abstract The title compound (C37H38O) belongs to the family 1-hetero-2,5-cyclohexadienes. The structure is triclinic, space group P[unk], with a = 11.576(5), b = 12.229(5), c = 12.305(5) Å, α = 68.52(3), β = 71.50(3), γ = 77.54(3)° and Z = 2. Three-dimensional intensity data collected on the SYNTEX P21 diffractometer using CuKα radiation at room temperature used for the structure determination and refinement. The final R value is 0.082 for 3713 observed reflections. Both tert-butyl groups are disordered as a result of their rotation around the C(phenyl)-C(tertbutyl) bond.

Phosphaniminato-Cluster des Kupfers. Synthese und Kristallstrukturen von [Cu6Cl6(NPMe3)4]Cl[Me3SiNPMe3] · CH2Cl2 und [Cu6Cl6(NPMe3)4][Cu(Me3SiNPMe3)2]Cl2 / Phosphoraneim inato Clusters of Copper. Syntheses and Crystal Structures of [Cu6Cl6(NPMe3)4]Cl[Me3SiNPMe3] · CH2Cl2 and [Cu6Cl6(NPMe3)4][Cu(Me3SiNPMe3)2]Cl2

Abstract The title compounds have been prepared as black-blue crystals with metallic lustre by the reaction of CuCl2 and CuCl, respectively, with Me3SiNPMe3 in CH2Cl2 suspensions. The complexes have been characterized by cyclic voltammetry and by crystal structure determinations. [Cu6Cl6(NPMe3)4]Cl[Me3SiNPMe3] · CH2Cl2: Space group P212121, Z = 4, structure solution with 4407 unique observed reflections, R = 0.057. Lattice dimensions at -70 °C: a -1159.3(8), b = 2027.1(14), c = 2063.3(12) pm. The compound consists of cluster ions [Cu6Cl6(NPMe3)4]+, in which the copper atoms form a regular octahedron. Four planes of the octahedra are capped by μ3-nitrogen atoms of the (NPMe3)- groups. Each of the Cu atoms is connected with a terminal chlorine atom . Another chloride ion serves for charge compensation; this ion occupies another Cu3 plane of the octahedron. Without bonding interaction one Me3SiNPMe3 molecule and one CH2Cl2 molecule are included in the lattice. [Cu6Cl6(NPMe3)4][Cu(Me3SiNPMe3)2]Cl2: Space group Pna21, Z = 4, structure solution with 5676 unique observed reflections, R = 0.071. Lattice dimensions at -70 °C: a = 3117.2(21), b = 1927.4(11), c = 1002.7(8) pm. The compound consists of cluster ions [Cu6Cl6(NPMe3)4]+, the complex ion [Cu(Me3SiNPMe3)2]+, and chloride ions. In the cation [Cu(Me3SiNPMe3)2]+ the copper atom is linearly coordinated by the nitrogen atoms of the phosphaneimine molecules.

Crystal and molecular structure of bis(3-cyano-2,4 pentanedionato)-bis(N,N-dimethylethylenediamine)copper(II). An unusual conformation and co-ordination of a β-dione

Abstract The title compound, C10H19N3O2Cu, is monoclinic, space group P21/n, Z = 2. Cell dimensions are a = 7.6071(6) Å, b = 20.623(1) Å, c = 7.9777(7) Å and β = 101.7359(7)°. A total of 3510 reflections were measured with an Enraf Nonius CAD-4 automatic diffractometer using CuKα radiation. The structure was refined by full-matrix least squares to a conventional R = 0.047 for 2957 unique reflections. The coordination around the central copper atom is octahedral with the copper atom on the equatorial plane of four nitrogen atoms. The Cu–N bond lengths have a mean value of 2.0646 Å. The two remaining apices of the octahedron are occupied by two nitrogen atoms of the β-dione groups at distances Cu–N = 2.5143 Å.

Complexes of Copper, Silver, and Gold with Urea Homologues. Crystal Structures of [{µ2-SeC(NH2)2} Ag{SeC(NH2)2}2]2 2+2Cl- • 4 DMF and [Ph3PAu{SC(NHMe)2}]+Cl- • SC(NHMe)2

Abstract The title compounds were prepared from chloro(organophosphine)metal(I) complexes and the urea homologues SeC(NH2)2 and SC(NHMe)2 in good yields. Recrystallization of [Ph3,PAg{SeC(NH2)2}]+Cl- from DMF/CH2Cl2 leads in low yield to the dinuclear complex [{µ2-SeC(NH2)2}Ag{SeC(NH2)2}2]2 2+2Cl- • 4DMF. The crystal structure reveals short Ag-Ag contacts and unexpectedly acute angles at the bridging selenium atom. The crystal structure of [Ph3PAu{SC(NHMe)2}]+Cl- • SC(NHMe)2 shows short N•••Cl and N•••S contacts that probably correspond to hydrogen bonding.

Crystal structure and spectra of (2,9-dimethyl-1,10-phenanthroline) 2,2,6,6-tetramethyl-3,5-heptanedionato copper(II) nitrate

Abstract The title compound (C25H31N3O5Cu) is monoclinic, with space group P21/c, Z = 4 and cell dimensions a = 9.5077(10), b = 9.8105(14), c = 27.123(4) Å and β = 91.315(13). A total of 7833 reflections were measured on a Philips PW1100 automatic diffractometer using MoKα radiation. The structure was refined by full-matrix least-squares to a conventional R = 0.0496 for the 3648 unique reflections. The co-ordination around the central copper atom is square pyramidal with the copper atom 0.177(2) Å above the base plane of three oxygen and one nitrogen atoms. The Cu–O bond lengths have a mean value of 1.956 Å, whereas the Cu–N bond length is 2.030 Å. The apex of the pyramid is occupied by the second nitrogen atom of neocuproine at a distance of Cu–N = 2.266 Å.

2,5-Bis(1′,3′-dithiol-2′-ylidene)-1,3,4,6-tetrathiapentalene and Its Related Unsymmetrical Donors

Abstract The title compound (1a) and its related unsymmetrical derivatives were prepared as new donors for organic conductors, and electrochemical properties and crystal structure of 1a were investigated. Several charge-transfer complexes and cation radical salts using them showed metallic temperature dependence of conductivity down to ca. 100 K.

Preparation, Crystal Structure and Electrical Properties of 2-Cyclopentanylidene-1,3-dithiolo[4,5-d]tetrathiafulvalene Derivatives

Abstract The title compounds (1) were prepared as the donor components for organic conductors. The molecular and crystal structures of bis(methylthio) derivative were determined by X-ray diffractional analysis. Among charge-transfer complexes and cation radical salts of 1 prepared so far, I3− salt of unsubstituted-1 and IBr2− salt of methylenedithio-1 showed metallic temperature dependence of conductivities.

Cyclopropylidene Dianion Equivalent. Preparation of 1,1-Dilithio-2,2-diphenylcyclopropane

Abstract The title compound was prepared by the treatment of the corresponding 1,1-dibromocyclopropane with lithium naphthalene radical anion (Li-C10H8). Trapping of the dilithio compound by chlorotrimethylsilane provided evidence for its highly basic profile which can compete with silylation.

Synthesen und Kristallstrukturen der Lithiumphosphide {Li(DME)[P(t-Bu)2]}2 und [Li(DME)PPh2]∞ / Syntheses and Crystal Structures of the Lithium Phosphides {Li(DME)[P(t-Bu)2]}2 and [Li(DME)PPh2]∞

Abstract The title compounds have been prepared by the reaction of n-butyllithium with the corresponding diorganophosphanes HPR2 (R = t-Bu, Ph) in DME solutions. Both compounds were characterized by crystal structure determinations. {Li(DME)[P(t-Bu)2]}2: Space group P 1̄, Z = 1, 2027 observed unique reflections, R = 0.055. Lattice dimensions at -80 °C: a = 879.9(3), b = 986.3(1), c = 1064.0(2) pm, α = 70.69(1)°, β = 70.63(2)°, γ - 69.89(2)°. The compound forms centrosymmetric dimers of symmetry Ci with Li-P bond lengths of 260.0 and 257.3 pm for the Li2P2 four-membered ring. [Li(DME)PPh2]∞: Space group P21/n, Z = 4. 3437 observed unique reflections, R = 0.055. Lattice dimensions at - 80 °C: a = 1034.8(2), b = 812.48(9), c = 1978.4(3) pm, β = 103.30(2)°. The compound forms polymeric chains via LiP bridges with Li-P bond lengths o f 256.3 and 254.1 pm.

Redetermination of the structure of tetrakis(acetonitrilo)silver(I) perchlorate at 173 K

Abstract The title compound contains three independent formula units. There is a large spread of values for chemically equivalent dimensions, notably in the cations, which display tetrahedral coordination at silver; Ag–N 2.228(4)–2.315(5) [av.2.266] Å, N–Ag–N 104.6(2)–115.7(2) [av. 109.6]°.

Ein Orthoperrhenat mit flächenverknüpften ReO6-Oktaedern: Hochdrucksynthese und Kristallstruktur von K3NaRe2O9 / An Orthoperrhenate with Face-Sharing ReO6 Octahedra: High-Pressure Synthesis and Crystal Structure of K3NaRe2O9

Abstract The title compound was prepared by high-pressure reaction of rhenium metal with technical grade (i.e., Na containing) KO2 in a modified Belt-type apparatus (20 kbar, 1000 °C, 60 min, Au capsule). The amber-coloured crystals are very hygroscopic and decompose rapidly when exposed to air. K3NaRe2O9 crystallizes hexagonally, space group P63/mmc, with a = 6.012(1), c = 14.342(14) Å, c/a = 2.386 and Z = 2. The structure was refined to R = 0.031, Rw = 0.023 for 422 independent, absorption-corrected reflections with l > σ (I). K3NaRe2O9 is isostructural with 6H-BaTiO3, a perowskite variant, and contains Na and Re in octaedral coordination. Two ReO6 octahedra are face-sharing, thus creating a Re2O9 double octahedron with a Re-R e distance of 2.92 Å.

Notizen: Synthese und Kristallstruktur des Diethylaminogallan-Dimers, (H2GaN(CH2CH3)2]2 / Synthesis and Crystal Structure of the Diethylaminogallane Dimer, [H2GaN(CH2CH3)2]2

Abstract The title compound was prepared by reacting gallane etherate H3Ga · OEt2 at -40 °C in Et2O with diethylamine upon warming to room temperature for several hours. It forms white crystals from ether solution which were identified by X-ray structure determination. Space group C 2/c, Z = 4; 930 observed unique reflections, R/wR = 0.0482/0.0450. Lattice dimensions at 193 K: a = 1292.9(3), b = 721.1(2), c = 1443.1(2) pm; β = 92.81(2)°. The structure reveals a centrosymmetric dimeric molecule with a planar square (GaN)2 fourmembered ring: average distance Ga - N = 201.7 pm, Ga ··· Ga 284.5(2) pm.

Synthese und Einkristall-Strukturanalyse des Oxidnitrits K5AgO2(NO2)2 / Synthesis and Single Crystal Structure Analysis of the Oxide Nitrite K5AgO2(NO2)2

Abstract The title compound has been characterized by X-ray powder and single crystal diffraction: Pbam. a = 715.8(1), b = 1393.1(2), c = 539.4(1) pm; Z = 2; 1088 diffractometer data; R = 0.087, Rw = 0.083. The crystal structure is a variant of the anti-perovskite type of structure. The NO2 - anion is rotationally disordered.

Crystal structure and bonding of tetrakis(tert-butyl-ammonium) β-octamolybdate(VI) hexahydrate

Abstract The title compound, (HC4H11N)4 [Mo8O26] · 6 H2O, M = 1588.18 crystallizes in the monoclinic system, space group P21/c, with cell dimensions a = 10.909(3), b = 9.927(2), c = 22.018(4) Å, β = 101.73(2)°, Dx = 2.259, Do = 2.257(1) Mg/m3, Z = 2. The structure has been refined to R = 0.028 and Rw = 0.030 for 3041 observed reflexions with I > 3 σ(I). The unit cell contains discrete centrosymmetric polyanions β-[Mo8O26]4−, (HC4H11N)+ cations and water molecules. Both cations and water molecules are oriented to permit hydrogen contacts with either molybdate oxygen atoms and water oxygen atoms to form an extensive network of hydrogen bonds. Seven different types of hydrogen contacts have been found: N–H…O, N–H…O w , O w ,–H w …N, O w –H w …O, O w –H w …O w , C–H…O and C–H…O w . The proposed hydrogen-bonding interactions appear to stabilize the crystal structure. The compound shows a relative low thermal stability and its water molecules are lost between 58 and 150°C in an oxygen-argon atmosphere during an endothermic process.

Crystal structure of 2S,4S-2,4-carboxymethyl-1,3-dimethylthiazolidine hydrochloride

Abstract The title compound is the condensation product of the aminoacid d-penicillamine with glyoxylic acid, followed by esterification with methanol/HCl. It crystallizes from ether/petroleum ether orthorhombically in the space group P212121 with a = 1033.4(6), b = 1678.2(6) and c = 730.7(3) pm.

Synthese und Kristallstrukturen der ionischen Kronenetherkomplexe [TiCl3(15-Krone-5)(CH3CN)][SbCl6) und [VCI(OH)(18-Krone-6)(CH3CN)2][SbCl6] · ½(18-Krone-6 · CH3CN) / Synthesis and Crystal Structures of the Ionic Crown Ether Complexes [TiCl3(15-Crown-5)(CH3CN)][SbCl6) und [VCI(OH)(18-Crown-6)(CH3CN)2][SbCl6] · ½(18-Crown-6 · CH3CN)

Abstract The title compounds were prepared by the reaction of titanium tetrachloride with 15-crown-5 and antimony pentachloride, and by the reaction of vanadium trichloride with 18-crown-6 and antimony pentachloride in the presence of traces of water in acetonitrile solution, respectively. The complexes were characterized by IR spectroscopy and by X-ray structure determinations. [TiCl3(15-crown-5)(CH3CN)][SbCl6]: Space group Pnma, Z = 4, 1355 observed unique reflections, R = 0.035. Lattice dimensions at -80 °C: a = 1987(1), b = 1742.2(6), c = 111.0(2) pm. The compound consists of SbCl6- anions and cations [TiCl3(15-crown-5)(CH3CN)]+, in which the titanium atom is coordinated octahedrally by three chlorine atoms in facial arrangement, by the nitrogen atom of the acetonitrile molecule, and by two oxygen atoms of the crown ether molecule. [VCl(OH)(18-crown-6 )(CH3CN)2][SbCl6] · ½(18-crown-6 · CH3CN); Space group P 1̄, 3936 observed unique reflections, R = 0.714. Lattice dimensions at -80 °C: a = 1194.2(6), b = 1349.8(6), c = 1365.5(6) pm, α = 93.55(4)°, β = 111.23(4)°, γ = 93.15(4)°. The compound consists of SbCl6 - anions, included 18-crown-6 and acetonitrile molecules, and cations [VCl(OH)(18-crown-6)(CH3CN)2]+, in which the vanadium atom is octahedrally coordinated by two nitrogen atoms of the acetonitrile molecules in trans positions, by a chlorine atom and a hydroxyl group in cis position, and by two oxygen atoms of the crown ether molecule. One of the acetonitrile molecules forms weak hydrogen bridges with two oxygen atoms of the included crown ether molecule as well as with one chlorine atom of the SbCl6 - ion.

Crystal structure of 2S,4S-2,4-carboxymethyl-5,5-dimethyl-1,3-thiazolidine

Abstract The title compound was prepared by esterification of the corresponding dicarboxylic acid with methanol/SOCl2. It crystallizes from diethyl ether monoclinically in the space group P21 with a = 1004.2(7), b = 665.0(3), c = 980.3(5) pm and β = 115.06(4)°.

The crystal structures of Mn3As2(II) and Mn5As4 determined from intergrown crystals

Abstract The title compounds have closely related structures and intergrown crystals are very common. Both compounds have the same orthorhombic space group Cmc21 and both have – within the error limits – two translation periods in common: a = a′ = 376.1(1) pm, b = b′ = 1376.0(2) pm, c = 1319.0(1) pm, c′ = 1212.3(2) pm, Z = 8, Z′ = 4 for Mn3As2(II) and Mn5As4, respectively. Both structures were determined from one intergrown “single-crystal”. The conventional residuals are R = 0.044(669 structure factors, 61 variable parameters) and R′ = 0.048 (553 F's, 55 variables). The difference between the two compounds arises through the absence of one Mn position in Mn5As4. The structures are intermediate between those of NiAs and Ni2In. They are also closely related to the earlier determined structure of Mn3As2(I).

Crystal structure of a C2-symmetric Schiff base from 1,4-diacetyl-2,3,5,6-tetramethoxybenzene and (S)-1-phenylethylamine

Abstract The title compound was prepared by a TiCl4-catalyzed reaction of bisacetylated benzene and 1-phenylethylamine. It crystallizes from ethyl acetate/petroleum ether orthorhombically in the space group P21212 with a = 796.2(1), b = 1908.7(5) and c = 924.1(2) pm.

Crystal and molecular structure of 1,4-diphenyl-2-(4,7-dimethoxy-1-naphthyl) but -2-ene-1,4-dione

Abstract The title compound C28H22O4 of molecular weight 422.46 crystallizes in the monoclinic system, space group C2/c, a = 27.56(2), b = 10.340(9), c = 18.25(2) Å, β = 122.52°(7), Z = 8, V = 4385.26 Å3, F(000) = 1776.00, Dm = 1.277 gcm−3, Dx = 1.279 gcm−3, linear absorption coefficient μ = 0.48 cm−1. The crystal structure has been determined with a final agreement index R = 0.043 and Rw . = 0.059 for 2531 independent observed reflections with I > 3σ(I). X-ray studies revealed the difference in conformation of the two carbonyl groups and also confirmed the cis geometry of the molecule. The rotamer with s-cis conformation of C11 = C19 with respect to C7 = C8 is found to be the preferred one.