1,1,3,5,5,7,9,9,11-Nonachlor-1,5,9-triphospha-2,4,6,8,10,12-hexaazacyclododecahexaen: [Cl2PN2CCl]3, Synthese, Spektren und Kristallstruktur/ 1,1,3,5,5,7,9,9,11-Nonachloro-1,5,9-triphospha-2,4,6,8,10,12-hexaazacyclododecahexaene: [Cl2PN2CCl]3, Preparation, Spectra and Crystal Structure

1986 ◽  
Vol 41 (7) ◽  
pp. 839-844 ◽  
Author(s):  
H .-D. Hausen ◽  
G. Rajca ◽  
J. Weidlein

AbstractThe title compound, Cl2PN2CCl, has been synthesized by the reaction of PCl5 with Me3Si -N = C = N - SiMe3 (Me - CH3) in a 1:1 molar ratio. The colourless com pound is trimericin benzene solution and in the solid state and has a structure with a highly puckered 12-membered P3N6C3-ring skeleton of low symmetry. The X-ray structure determination shows a monoclinic space group P 21/a with 4 trimeric units per cell.

1995 ◽  
Vol 50 (1) ◽  
pp. 66-70 ◽  
Author(s):  
Inge Pabst ◽  
Peter Sondergeld ◽  
Mirjam Czjzek ◽  
Hartmut Fuess

The title compound has been prepared in two different ways: First, by boiling single crystals of [(C2H5)4N]HgCl3 in a mixture of n-hexane/n-octane [4:1] at T = 350 K, and second, in a synthesis from stoichiometric quantities of the components. X-ray structure analysis gave the stoichiometry [(C2H5)4N]2Hg3Cl8, monoclinic, space group P21, a = 7.538(3), b = 19.909(6), c = 10.274(3) Å, β = 95.13(1)°, V = 1535.7(9) A3, Z = 2. The basic [Hg3Cl8]2--units form broken zig-zag chains along [100]. The Hg–Cl distances within the [Hg3Cl8]2- clusters range from 2.315(3) to 2.755(4) Å. This is a new coordination type for halomercurates.


2014 ◽  
Vol 38 (1) ◽  
pp. 97-101
Author(s):  
Jagodish C Sarker ◽  
Md Saifur Rahman ◽  
Shariff E Kabir ◽  
Tasneem A Siddiquee

The solid-state molecular structure determination of the bimetallic osmium-tin compound [(?-H)Os2(CO)4(SnPh3)2(?-HSnPh2)(?-dppf)] (1) was carried out to determine the relative orientationof the coordinated ligands. Compound 1 crystallizes in the monoclinic space group P 21/c with a =22.366(7), b = 14.217(4), c = 25.213(8) Å, ? = 98.865(7)°, Z = 8 and V = 7921(4) Å3. It is a 34-electron bimetallic cluster with the Os-Os edge concomitantly bridged by a dppf and two HSnPh2 ligands DOI: http://dx.doi.org/10.3329/jbas.v38i1.20218 Journal of Bangladesh Academy of Sciences, Vol. 38, No. 1, 97-101, 2014


2014 ◽  
Vol 69 (3) ◽  
pp. 294-298 ◽  
Author(s):  
Olaf Reckeweg ◽  
Armin Schulz ◽  
Francis J. DiSalvo

Transparent and colorless single crystals of Yb26B12O57 were obtained by reacting Yb2O3 and B powder at 1000 °C in the presence of a KCl flux for 24 h in silica-jacketed Nb ampoules and subsequent removal of the flux by washing with water. Yb26B12O57 crystallizes in the monoclinic space group C2/m (no. 12, Z = 1) with the lattice parameters a = 2454:1(3), b = 357:78(4), c = 1426:7(2) pm and β = 115:111(6)°, and its structure differs slightly from that of a known compound with the same stoichiometry. Raman spectra of single crystals of the title compound were recorded and compared to those of known borate compounds


1984 ◽  
Vol 39 (9) ◽  
pp. 1219-1223 ◽  
Author(s):  
G. Rajca ◽  
W. Schwarz ◽  
J. Weidlein

Tetrachloroantimony trimethylsilylcarbodiimide, Cl4SbNCNSiMe3, has been synthesized by the reaction of SbCl5 with Me3SiNCNSiMe3 in a 1:1 molar ratio. The pale yellow compound is dimeric in solution and in the solid state and has according to the vibrational spectra a centrosymmetric structure of C2h symmetry. The X-ray structure determination shows the monoclinic space group P21/c with two dimeric units per cell. The structure was refined to an R-value of 0,04.


1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2


1983 ◽  
Vol 36 (11) ◽  
pp. 2333 ◽  
Author(s):  
B Kamenar ◽  
RA Pauptit ◽  
JM Waters

The X-ray crystal structure of 3α,4α:5β,6β-diepoxyandrostan-17-one has been determined. Crystals of the title compound (C19H26O3)are monoclinic, space group P21, with a 9.208(2), b 9.620(4), c 9.312(3) �, β 99.14(2)�, V 814.5 Ǻ3 and Z 2. The structure was solved by direct methods and refined to R 0.039 for 887 observed reflexions. The 3α,4α:5β,6β configuration of the epoxide rings confirms the assignment based on proton n.m.r. studies.


1985 ◽  
Vol 40 (7) ◽  
pp. 872-877 ◽  
Author(s):  
W. Kolondra ◽  
W. Schwarz ◽  
J. Weidlein

Abstract Unexpectedly the reaction of SbCl3 with Na(N{SiMe3}2) in a 1:3 molar ratio forms MeSb(N{SiMe3}2)2, I, (Me = CH3) and other trimethylsilyl compounds. The colourless and liquid methylstibane derivative I is monomeric in solution and forms MeSbCl2(N{SiMe3}2)2 (II) on reaction with SO2Cl2. Both new compounds have been characterized by analyses, NMR, IR and Raman spectra. The X-ray structure determination for II shows the monoclinic space group P21/C with 4 monomeric units per cell. The structure was refined to an R-value of 0,052.


1993 ◽  
Vol 48 (7) ◽  
pp. 1009-1012 ◽  
Author(s):  
Kurt Merzweiler ◽  
Harald Kraus

[{Cp(CO)2Fe}SnCl3] reacts with Na2Se in THF to form the compound [{Cp(CO)2Fe}3ClSn3Se4] 1. 1 crystallizes in the monoclinic space group P21/n with 4 formula units per unit cell. The lattice constants are α = 1435.2(7), b = 1124.4(4), c = 1972.7(12) pm, β = 94.59(4)°. According to the X-ray structure determination 1 contains a bicyclic Sn3Se4 framework.


2008 ◽  
Vol 23 (3) ◽  
pp. 232-240
Author(s):  
Abderrahim Aatiq ◽  
Rachid Bakri ◽  
Aaron Richard Sakulich

Synthesis and structure of two phosphates belonging to the ternary Sb2O5–In2O3–P2O5 system are realized. Structures of SbV1.50InIII0.50(PO4)3 and (SbV0.50InIII0.50)P2O7 phases, obtained by solid state reaction in air at 950 °C, were determined at room temperature from X-ray powder diffraction using the Rietveld method. SbV1.50InIII0.50(PO4)3 have a monoclinic (space group P21/n) distortion of the Sc2(W O4)3-type framework. Its structure is constituted by corner-shared SbO6 or InO6 octahedra and PO4 tetrahedra. Monoclinic unit cell parameters are a=11.801(2) Å, b=8.623(1) Å, c=8.372(1) Å, and β=90.93(1)°. (Sb0.50In0.50)P2O7 is isotypic with (Sb0.50Fe0.50)P2O7 and crystallizes in orthorhombic system (space group Pna21) with a=7.9389(1) Å, b=16.0664(2) Å, and c=7.9777(1) Å. Its structure is built up from corner-shared SbO6 or InO6 octahedra and P2O7 groups (two group-types). Each P2O7 group shares its six vertices with three SbO6 and three InO6 octahedra, and each octahedron is connected to six P2O7 groups.


2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Mohamed I. Attia ◽  
Hazem A. Ghabbour ◽  
Aida A. El-Azzouny ◽  
Omar A. Al-Deeb ◽  
Maha S. Almutairi ◽  
...  

Synthesis, spectroscopic characterization and X-ray crystal structure of a new (2E)-2-[3-(1H-imidazol-1-yl)-1-phenylpropylidene]-N-phenylhydrazinecarboxamide (4) are reported. The stereochemistry of the title compound4, C19H19N5O, about the imine bond [1.296 (4) Å] was assigned to have (E)-configuration. In the urea moiety, the N–H entities aretransto each other, and one of these forms is an intramolecular N–H⋯H hydrogen bond. The compound crystallizes in the monoclinic space groupP21/cwitha= 5.8093 (2) Å,b= 20.5575 (6) Å,c= 14.0355 (5) Å,α= 90.00°,β= 97.365° (2),γ= 90.00°,V= 1662.36 (10) Å3, andZ= 4. The molecules are packed in crystal structure by weak intermolecular hydrogen interactions.


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