1,3-Digermapropan und 1,3,5-Trigermacyclohexan / 1,3-Digermapropane and 1,3,5-Trigermacyclohexane

1988 ◽  
Vol 43 (6) ◽  
pp. 727-732 ◽  
Author(s):  
Hubert Schmidbaur ◽  
Johann Rott ◽  
Gabriele Reber ◽  
Gerhard Müller

AbstractFrom the copper-catalyzed reaction of germanium powder with dichloromethane at 350 °C a mixture of alkylchlorogermanes is obtained, in which CH3GeCl3, CH2(GeCl3)2 (1) and (Cl2GeCH2)3 (2) are the major products. Treatment of 1 and 2 with LiAlH4 in di-n-butyl or diethylether, resp., affords the hydrides CH2(GeH3)2 (3) and cyclic (H2GeCH2)3 (4), the latter along with the heterocycle H2Ge(CH2GeH2)2 (5). Compounds 3-5 have been identified by analytical and spectroscopic data, and the crystal structure of 4 has been determined by single crystal X-ray diffraction. The compound crystallizes in the orthorhombic space group Pmn21, with two molecules in the unit cell (a = 8.663(1), b = 7.783(1), c = 6.124(1) Å). The molecules, which are in a chair conformation, have crystallographic mirror symmetry with bond angles slightly larger than tetrahedral and Ge-C distances of 1.944(6), 1.953(3) and 1.955(4) Å. The compounds show potential as substrates for plasma-enhanced chemical vapour deposition (PE-CVD) of amorphous germanium carbon alloys (a-Ge, C:H).

1993 ◽  
Vol 57 (387) ◽  
pp. 329-336 ◽  
Author(s):  
M. A. Hoyos ◽  
T. Calderon ◽  
I. Vergara ◽  
J. Garcia-Solé

AbstractX-ray diffraction refinement of the crystal structure of eosphorite has been carried out with reference to the orthorhombic space group Cmca. The structure is similar to that previously described by Hanson (1960), but the standard deviations are improved. Optical absorption and photoluminescence have also been studied for this mineral. Two sharp emission lines, denoted as R1 and R2, superimposed to a broad band (630-750 nm) have been related to the presence of Cr3+ ions. The excitation spectrum of these emissions confirms that the absorption (excitation) bands centred at 431 nm and 585 are related to with 4A2 → 4T1 and 4A2 → 4T2 spin allowed transitions of this ion.


2014 ◽  
Vol 51 (3) ◽  
pp. 51-57 ◽  
Author(s):  
G. Chikvaidze ◽  
N. Mironova-Ulmane ◽  
A. Plaude ◽  
O. Sergeev

Abstract Polytypes of colourless and coloured single crystals of silicon carbide (SiC) grown on SiC substrates by chemical vapour deposition are studied using Raman spectroscopy supplemented by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analyses. The SEM analysis of the defect stacking faults, inclusions of defects and their distribution has shown that they correlate with the peak positions of the obtained Raman spectra and with the XRD data on the crystal structure


1985 ◽  
Vol 63 (6) ◽  
pp. 1166-1169 ◽  
Author(s):  
John F. Richardson ◽  
Ted S. Sorensen

The molecular structures of exo-7-methylbicyclo[3.3.1]nonan-3-one, 3, and the endo-7-methyl isomer, 4, have been determined using X-ray-diffraction techniques. Compound 3 crystallizes in the space group [Formula: see text] with a = 15.115(1), c = 7.677(2) Å, and Z = 8 while 4 crystallizes in the space group P21 with a = 6.446(1), b = 7.831(1), c = 8.414(2) Å, β = 94.42(2)°, and Z = 2. The structures were solved by direct methods and refined to final agreement factors of R = 0.041 and R = 0.034 for 3 and 4 respectively. Compound 3 exists in a chair–chair conformation and there is no significant flattening of the chair rings. However, in 4, the non-ketone ring is forced into a boat conformation. These results are significant in interpreting what conformations may be present in the related sp2-hybridized carbocations.


2017 ◽  
Vol 72 (12) ◽  
pp. 983-988 ◽  
Author(s):  
Martin K. Schmitt ◽  
Hubert Huppertz

Abstractβ-Y(BO2)3 was synthesized in a Walker-type multianvil module at 5.9 GPa/1000°C. The crystal structure has been elucidated through single-crystal X-ray diffraction. β-Y(BO2)3 crystallizes in the orthorhombic space group Pnma (no. 62) with the lattice parameters a=15.886(2), b=7.3860(6), and c=12.2119(9) Å. Its crystal structure will be discussed in the context of the isotypic lanthanide borates β-Ln(BO2)3 (Ln=Nd, Sm, Gd–Lu).


2010 ◽  
Vol 97-101 ◽  
pp. 4213-4216
Author(s):  
Jian Xiong Liu ◽  
Zheng Yu Wu ◽  
Guo Wen Meng ◽  
Zhao Lin Zhan

Novel single-crystalline SnO2 zigzag nanoribbons have been successfully synthesized by chemical vapour deposition. Sn powder in a ceramic boat covered with Si plates was heated at 1100°C in a flowing argon atmosphere to get deposits on a Si wafers. The main part of deposits is SnO2 zigzag nanoribbons. They were characterized by means of X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM) and selected-area electron diffraction (SAED). SEM observations reveal that the SnO2 zigzag nanoribbons are almost uniform, with lengths near to several hundred micrometers and have a good periodically tuned microstructure as the same zigzag angle and growth directions. Possible growth mechanism of these zigzag nanoribbons was discussed. A room temperature PL spectrum of the zigzag nanoribbons shows three peaks at 373nm, 421nm and 477nm.The novel zigzag microstructures will provide a new candidate for potential application.


1979 ◽  
Vol 57 (1) ◽  
pp. 57-61 ◽  
Author(s):  
R. Melanson ◽  
F. D. Rochon

The crystal structure of [Pt(diethylenetriamine)(guanosine)](ClO4)2 has been determined by X-ray diffraction. The crystals are orthorhombic, space group P212121, with a = 12.486(6), b = 13.444(7), c = 14.678(11) Å, and Z = 4. The structure was refined by block-diagonal least-squares analysis to a conventional R factor of 0.050 and a weighted Rw = 0.045.The coordination around the platinum atom is square planar. Guanosine is bonded to platinum through N(7). The purine planar ring makes an angle of 62.7° with the platinum coordination plane. The structure is stabilized by hydrogen bonding.


Author(s):  
Cristian Biagioni ◽  
Luca Bindi ◽  
Koichi Momma ◽  
Ritsuro Miyawaki ◽  
Yoshitaka Matsushita ◽  
...  

Abstract Tsugaruite was originally defined as a lead-arsenic sulfosalt from the Yunosawa mine, Aomori Prefecture, Japan. Until recently its crystal structure remained unsolved and its actual classification in the sulfosalt realm was unknown. Here the refinement of the crystal structure of tsugaruite using single-crystal X-ray diffraction data is reported. The mineral is orthorhombic, space group P2nn, with unit-cell parameters a = 8.0774(10), b = 15.1772(16), c = 38.129(4) Å, V = 4674.3(9) Å3, in agreement with previous studies. The solution of the crystal structure of this mineral revealed Cl occupying a specific position. Chlorine was thus sought and found using the electron microprobe; the average of six spot analyses gave (in wt.%): Pb 68.04, As 12.83, S 18.29, Cl 0.63, total 99.80. The empirical formula, calculated on the basis of Pb + As = 43 atoms per formula unit, is Pb28.26As14.74S49.08Cl1.52. Tsugaruite is an N = 4 plesiotypic derivative of the homologous series of Pb-Sb chloro-sulfosalts having the general formula Pb(2+2N)(Sb,Pb)(2+2N)S(2+2N)(S,Cl)(4+2N)ClN. It has a Cl/(Cl + S) atomic ratio close to that of other known Pb-Sb chloro-sulfosalts (pillaite, pellouxite) and slightly higher than that of dadsonite.


1985 ◽  
Vol 40 (12) ◽  
pp. 1631-1637 ◽  
Author(s):  
Ruth Christophersen ◽  
Paul Klingelhöfer ◽  
Ulrich Müller ◽  
Kurt Dehnicke

Abstract The pyridine complexes of cyclo-thiazeno vanadium dichloride, [VCl2(N3S2)py] and [VCl2(N3S2)(py)2] were synthesized by reactions of polymeric VCl2(N3S2) with varying amounts of pyridine in CH2Cl2. The compounds were characterized by their IR spectra as well as by their 51V NM R spectra. The crystal structure of [VCl2(N3S2)(C5H5N)] was determined by means of X-ray diffraction (1582 independent observed reflexions, R = 0.031). Crystal data: orthorhombic, space group Pnma, a = 1372, b - 2261, c - 1068 pm, Z = 12. In the lattice there are two monomeric, crystallographically independent molecules [VCl2(N3S2)(C5H5N)], which differ only slightly. The vanadium atoms have a trigonal bipyramidal coordination with the N atom of the pyridine molecule and one chlorine atom in apical positions, and with one chlorine atom and the N atoms of the cyclo-thiazeno ligand in equatorial positions. The VN bond lengths of the planar VN3S2 ring of 174 pm correspond to double bonds


1990 ◽  
Vol 43 (12) ◽  
pp. 2083 ◽  
Author(s):  
DC Craig ◽  
VJ James ◽  
JD Stevens

The crystal structure of the title compound (1) has been determined by X-ray diffraction. Crystals of (1) are orthorhombic, space group P21212 with a 11.425(1), b 24.916(1), c 5.8952(3)Ǻ, Z 4. Refinement on 1675 observed reflections measured with Cu Kα radiation converged at R 0.034. The seven- membered ring adopts a boat conformation in which the pseudo plane of symmetry passes through the ring oxygen.


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