Beiträge zur Chemie des Phosphors, 109 [1] t-Bu6lAs2P6 - der erste Phosphor-Arsen-Polycyclus / Contributions to the Chemistry of Phosphorus, 109 [1] t-Bu6As2P6 - the First Phosphorus Arsenic Polycycle

1982 ◽  
Vol 37 (3) ◽  
pp. 299-305 ◽  
Author(s):  
Marianne Baudler ◽  
Yusuf Aktalay ◽  
Thomas Heinlein ◽  
Karl-Friedrich Tebbe
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Direct Methods ◽  
Crystal Structure Analysis ◽  
Phosphorus Trichloride ◽  
Bond Lengths ◽  
Tert Butyl ◽  
Average Bond ◽  
Structure In Solution ◽  
Endocyclic Bond

The first phosphorus arsenic polycycle t-Bu6As2P6 (1) was synthesized by dehalogenation of a 3:1 mixture of tert-butyldichlorophosphane and phosphorus trichloride using magnesium. 1 has been characterized by spectroscopic methods and by a crystal structure analysis having the t-Bu6Ps-analogous 2,2′,3,3′,4,4′-hexa-tert-butyl-l′-diarsa-2,2′,3,3′,4,4′-hexaphospha- bicyclobutane structure. In solution, the rotation around the exocyclic As-As bond is restricted already at room temperature. 1 crystallizes triclinically in the space group PT (No. 2) with a = 919.4 pm, b = 924.3 pm, c = 1171.7 pm, a = 97.21°, β = 102.98°, γ = 112.75°, and Z = 1 formula unit (V = 0.8694 nm3, Dx = 1.295 Mg · m-3). The crystal structure has been solved by 'direct methods' and refined to R = 0.048 with 2131 observed reflections. The molecule with symmetry C1 consists of two trans oriented and slightly folded four-membered P3As rings. The exocyclic bond length (d(As-As) = 244.1 pm) as well as the average endocyclic bond lengths d̅(As-P) = 235.6 pm; 3d̅(P-P) = 222.6 pm) are normal. The arrangement of the tert-butyl substituents with average bond lengths d̅(P-C) = 189.9 pm and d̅(C-C) = 1 5 2 . 5 p m is all-trans.

Die Kristallstruktur von [Mn(CH3CN)6][MnI4]

1996 ◽  
Vol 51 (2) ◽  
pp. 298-300 ◽  
Author(s):  
Frank Weller ◽  
Hans-Joachim Mai ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Ir Spectrum ◽  
Crystal Structure Analysis ◽  
Site Symmetry ◽  
Bond Lengths ◽  
Structure Solution ◽  
Acetonitrile Solutions ◽  
Average Bond ◽  
Octahedral Cations

Abstract [Mn(CH3CN)6][MnI4] crystallizes from acetonitrile solutions of Mnl2 as yellow single crystals which were characterized by their IR spectrum and by a crystal-structure analysis. Space group P21/n, Z = 4, structure solution with 3742 observed unique reflections with Fo >5σ(Fo), R = 0.050. Lattice dim ensions at 20°C: a = 1258.0(5), b = 1244.7(2), c = 1753.3(6) pm, β = 92.22(3)°. The compound forms octahedral cations [Mn(CH3CN)6]2+ with site symmetry Ci with average Mn-N bond lengths of 222.3 pm and te­trahedral anions [Mnl4]2- without symmetry with average bond lengths MnI of 271.3 pm.

scholarly journals Beiträge zur Strukturchemie phosphorhaltiger Ketten und Ringe, V [1] Die Molekül- und Kristallstruktur des 1.2.3.4-Tetra-tert-butyl-1.4-bis(trimethylsilyl)tetraphosphans, Me3Si-(t-BuP)4-SiMe3 / Structural Chemistry of Phosphorus-Containing Chains and Rings, V [1] Molecular and Crystal Structure of 1,2,3,4-Tetra-tert-butyl-1,4-bis(trimethylsilyl)tetraphosphane, (H3C)3Si-(t-BuP)4-Si(CH3)3

1982 ◽  
Vol 37 (5) ◽  
pp. 534-541 ◽  
Author(s):  
Karl-Friedrich Tebbe ◽  
Roland Fröhlich
Keyword(s):  
Crystal Structure ◽  
Structural Chemistry ◽  
Space Group ◽  
Short Contact ◽  
Bond Lengths ◽  
Tert Butyl ◽  
Phosphorus Containing ◽  
Central Bond ◽  
Inner Region ◽  
Average Bond

The compound 1,2,3,4-tetra-tert-butyl-1,4-bis(trimethylsilyl)tetraphosphane, Me3Si-(t-BuP)4-SiMe3, C22H54P4Si2, crystallizes monoclinically in the space group P21/n (No. 14) with a = 889.9 pm, b = 2292.8 pm, c = 1568.0 pm, β = 94.14° and Z = 4 formula units.The molecule forms a twisted Si-P4-Si-chain with two kinds of P-P-bonds. The atoms neighbouring the silicium atoms take part in bonds of length d̄(P-P) = 218.8 pm, whereas the central bond d̄(P-P) = 221.4 pm is much longer. A special feature of the structure is a short contact d̄(P-P) = 345.6 pm. Therefore, the inner region of the molecule has the shape of a nearly planar trapezium of the four phosphorus atoms. The periphery of the molecule is as expected. The average bond lengths are d̄(P-Si) = 228.5 pm, d̄(P-C) - 190.2 pm, d̄(Si-C) = 186.6 pm, d̄(C-C) = 151.8 pm and d̄(C-H) = 94 pm

scholarly journals Crystal structure of K[Hg(SCN)3] – a redetermination

2014 ◽  
Vol 70 (9) ◽  
pp. i46-i46 ◽  
Author(s):  
Matthias Weil ◽  
Thomas Häusler
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Three Dimensional ◽  
Lattice Parameters ◽  
Bond Lengths ◽  
Dimensional Network ◽  
Anisotropic Displacement Parameters ◽  
Precision And Accuracy ◽  
Standard Deviations ◽  
Atomic Coordinates

The crystal structure of the room-temperature modification of K[Hg(SCN)3], potassium trithiocyanatomercurate(II), was redetermined based on modern CCD data. In comparison with the previous report [Zhdanov & Sanadze (1952).Zh. Fiz. Khim.26, 469–478], reliability factors, standard deviations of lattice parameters and atomic coordinates, as well as anisotropic displacement parameters, were revealed for all atoms. The higher precision and accuracy of the model is, for example, reflected by the Hg—S bond lengths of 2.3954 (11), 2.4481 (8) and 2.7653 (6) Å in comparison with values of 2.24, 2.43 and 2.77 Å. All atoms in the crystal structure are located on mirror planes. The Hg2+cation is surrounded by four S atoms in a seesaw shape [S—Hg—S angles range from 94.65 (2) to 154.06 (3)°]. The HgS4polyhedra share a common S atom, building up chains extending parallel to [010]. All S atoms of the resulting1∞[HgS2/1S2/2] chains are also part of SCN−anions that link these chains with the K+cations into a three-dimensional network. The K—N bond lengths of the distorted KN7polyhedra lie between 2.926 (2) and 3.051 (3) Å.

A fourfold interpenetrating diamond-like three-dimensional zinc(II) coordination polymer: synthesis, crystal structure and physical properties

2019 ◽  
Vol 75 (5) ◽  
pp. 504-507 ◽  
Author(s):  
Hui-Ru Chen
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Three Dimensional ◽  
Fluorescence Emission ◽  
Crystal Structure Analysis ◽  
The Novel ◽  
X Ray Diffraction ◽  
Metal Compounds ◽  
X Ray ◽  
Coordination Framework

Excellent fluorescence properties are exhibited by d 10 metal compounds. The novel three-dimensional ZnII coordination framework, poly[[{μ2-bis[4-(2-methyl-1H-imidazol-1-yl)phenyl] ether-κ2 N 3:N 3′}(μ2-furan-2,5-dicarboxylato-κ2 O 2:O 5)zinc(II)] 1.76-hydrate], {[Zn(C6H2O5)(C20H18N4O)]·1.76H2O} n , has been prepared and characterized using IR spectroscopy, elemental analysis and single-crystal X-ray diffraction. The crystal structure analysis revealed that the compound exhibits a novel fourfold interpenetrating diamond-like network. This polymer also displays a strong fluorescence emission in the solid state at room temperature.

Structural studies of organoboron compounds. XLIII. 4-[(1-Hydroxycyclohexyl)methyl]-2,2,5-triphenyl-1,3-dioxa-4-azonia-2-borata-4-cyclopentene

1991 ◽  
Vol 69 (3) ◽  
pp. 545-549 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Ute Schumacher ◽  
Mahmood Tajerbashi ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Key Words ◽  
Hydroxamic Acid ◽  
Direct Methods ◽  
Organoboron Compound ◽  
Structural Studies ◽  
Full Matrix ◽  
Bond Lengths ◽  
Acid Chelate

The reaction of N′-hydroxy-N-[(1-hydroxycyclohexyl)methyl]benzamide and diphenylborinic anhydride gives 4-[(1-hydroxycyclohexyl)methyl]-2,2,5-triphenyl-1,3-dioxa-4-azonia-2-borata-4-cyclopentene in nearly quantitative yield. Crystals of the product are monoclinic, a = 9.9117(6), b = 13.308(1), c = 17.339(2) Ǻ, β = 99.420(7)°, Z = 4, space group P21/c. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.040 and Rw = 0.047 for 2423 reflections with I > 3σ(I). The molecule has a normal five-membered hydroxamic acid chelate structure, the BONCO ring having a B-envelope conformation. Bond lengths (corrected for libration) (N)O—B = 1.535(3), (C)O—B = 1.569(3), C—B = 1.603(3) and 1.601(3) Ǻ are normal for this type of complex. Key words: organoboron compound, boron compound, crystal structure.

Preparation, properties, and X-ray crystal structure of a 1:1 complex of tetrathiafulvalene and p-dinitrobenzene

1982 ◽  
Vol 60 (16) ◽  
pp. 2057-2061 ◽  
Author(s):  
Martin R. Bryce ◽  
Anthony S. Secco ◽  
James Trotter ◽  
Larry Weiler
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Direct Methods ◽  
X Ray Diffraction ◽  
Crystalline Complex ◽  
X Ray ◽  
Triclinic System ◽  
Donor Acceptor ◽  
Bulk Magnetic Susceptibility ◽  
R Value

A crystalline complex of tetrathiafulvalene and p-dinitrobenzene has been prepared and characterised by esr and ir spectroscopy, bulk magnetic susceptibility, dc conductivity, and an X-ray diffraction analysis. It is a neutral 1:1 complex which is an insulator at room temperature, σRT = 2.5 × 10−7 ohm−7 cm−1. The complex crystallizes in the triclinic system, space group [Formula: see text] with cell constants a = 6.915(1), b = 7.615(1), c = 8.149(1) Å, α = 79.39(1), β = 69.55(1), γ = 70.81(1)°, Z = 1. Data were collected on an Enraf-Nonius CAD-4 diffractometer. The structure was solved by direct methods and refined to an R-value of 0.028 for 1222 observed reflections. The structure consists of molecules stacked in an alternating donor–acceptor fashion along the c-axis. Mixed sheets parallel to [Formula: see text] are comprised of tetrathiafulvalene and p-dinitrobenzene molecules arranged end-on in the [021] direction.

Structure of 5,5-dimethyl-2-phenylimino-Δ3-1,3,4-thiadiazoline from oxidative cyclization of a thiosemicarbazone

1987 ◽  
Vol 65 (6) ◽  
pp. 1154-1157 ◽  
Author(s):  
R. Faggiani ◽  
M. Kaminski ◽  
C. J. L. Lock ◽  
J. Warkentin
Keyword(s):  
Crystal Structure ◽  
Hydrogen Atom ◽  
Phenyl Ring ◽  
Direct Methods ◽  
Oxidative Cyclization ◽  
Repulsive Interaction ◽  
Sulphur Atom ◽  
Normal Range ◽  
X Ray ◽  
Bond Lengths

The X-ray crystal structure of 5,5-dimethyl-2-phenylimino-Δ3-1,3,4-thiadiazoline, C10H11N3S, has been determined. The compound is monoclinic, P21/c (No. 14), with a = 13.200(5), b = 6.340(4), and c = 13.823(4) Å, β = 113.50(4)°, and Z = 4. The structure was determined by direct methods and refined to R = 0.061, Rw = 0.067 for 1277 unique reflections. The molecule has the Z configuration. The thiadiazoline ring is planar. C—N and N=N bond lengths are within the normal range. The C—S bond lengths are similar to those we have observed previously in thiazolidines. Angles differ markedly from an expected average 108°. The small C—S—C angle (90.6(2)°) is accompanied by larger C—N=N angles (114.9(3), 117.8(3)°). The phenyl ring is not coplanar with the thiadiazoline ring (dihedral angle 38.6(4)°) because of repulsive interaction of the phenyl o-hydrogen atom with the sulphur atom.

scholarly journals 1,2,3,4,5,6,7,8,13,13,14,14-Dodecachloro-1,4,4a,4b,5,8,8a,12b-octahydro-1,4:5,8-dimethanotriphenylene at 90 K

2012 ◽  
Vol 68 (8) ◽  
pp. o2538-o2538
Author(s):  
Brandon W. Jenkins ◽  
Frank R. Fronczek ◽  
Steven F. Watkins
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Title Compound ◽  
Room Temperature ◽  
Bond Angle ◽  
Average Bond Length ◽  
Volume Contraction ◽  
Compound C ◽  
Independent Unit ◽  
Average Bond

The previously reported room-temperature crystal structure [Jaud Baldy, Negrel, Poite & Chanon (1993).Z. Kristallogr.204, 289–291] of the title compound, C20H8Cl12, is monoclinic withZ′ = 1, whereas the 90 K structure reported herein is triclinic withZ′ = 2 and shows a 2% volume contraction. The crystallographically independent unit chosen consists of both enantiomers (Λ and Δ) of this propeller-like molecule. Both enantiomers display quasi-twofold symmetry, with average bond-length/bond-angle deviations of 0.0018 (4) Å and 0.41 (2)° for Λ, and 0.0026 (4) Å and 0.50 (2)° for Δ.

Die Kristallstruktur von Gadolinium (III)-sulfit Trihydrat Gd2(S03)3∙ 3H2O / Crystal Structure of Gadolinium(III)-sulfite Trihydrate Gd2(SO3)3 ∙3H2O

1994 ◽  
Vol 49 (1) ◽  
pp. 60-62 ◽  
Author(s):  
Hans-Ulrich Hummel ◽  
Petra Joerg ◽  
Gerhard Pezzei ◽  
Alexander Wolski
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Room Temperature ◽  
Triclinic Space Group ◽  
Space Group ◽  
Bond Lengths ◽  
Clear Solution ◽  
Oxygen Atoms

Abstract Gd2(SO3)3 • 3 H20 is obtained by passing gaseous SO2 through a suspension of Gd2O3 in H2O at room temperature until a clear solution is formed. Single crystals are obtained by heating to 70(2) °C for 6 days. The compound crystallizes in the triclinic space group P 1 with a = 6.499(6), b = 6.621(3), c = 6.954(3) Å, α = 110.71(5), β = 90.54(3), γ = 106.05(1)° and Z = 1. The two crystallographically different gadolinium atoms are both coordinated by eight oxygen atoms forming distorted square antiprisms. Gd(l) is coordinated by six O atoms of sulfite ligands and two O atoms of water, while Gd(2) is surrounded by seven O atoms of SO3 and one of H2O. Gd-O-bond lengths vary between 2.31(3) and 2.50(3) Å.

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