Synthese und Kristallstruktur von (Cyclopentadienyl)(dicarbonyl)(1,5-di-/Molyl-pentaazadienido)molybdän, (Cp)Mo(CO)2(tolN5tol)/ Synthesis and Crystal Structure of (Cyclopentadienyl)(dicarbonyl)(1,5-di-p-tolyl-pentaazadienido)molybdenum, (Cp)Mo(CO)2(tolN5tol)

1988 ◽  
Vol 43 (8) ◽  
pp. 1029-1032 ◽  
Author(s):  
Johannes Beck

Abstract(Cp)Mo(CO)2(tolN5tol) is formed in the reaction of (Cp)Mo(CO)3Cl with tolNN(NH)NNtol and NaOH in ethanol. It forms red platelike crystals from THF/hexane which crystallize in the monoclinic space group P21/n with the lattice parameters a = 765.6(2), b = 2372.3(3), c = 1149.4(2) pm, β = 97.06(2)°, Z = 4. The structure consists of monomeric complexes. The pentaazadienido ligand chelates with its nitrogen atoms N1 and N3 the Mo atom of a (Cp)Mo(CO)2 unit. The nitrogen atom N5 is not coordinated to the metal atom. Although asymmetrically bonded, the all trans N5 zig zag chain is planar. The N -N distances in the four membered chelate ring are nearly equal (N1 - N2 = 131.0 and N2 - N3 = 132.6 pm)

1998 ◽  
Vol 51 (12) ◽  
pp. 1131 ◽  
Author(s):  
Donald C. Craig ◽  
Marcia L. Scudder ◽  
Wendy-Anne McHale ◽  
Harold A. Goodwin

The crystal structures of bis(2,2′:6′,2″-terpyridine)ruthenium(II) perchlorate hydrate, bis(2,2′:6′,2″- terpyridine)osmium(II) perchlorate hemihydrate and bis((1,10-phenanthrolin-2-yl)(pyridin-2-yl)- amine)iron(II) tetrafluoroborate dihydrate are described. In the terpyridine complexes the ruthenium-nitrogen distances and the corresponding osmium-nitrogen distances are not significantly different. In both complexes the ligand geometry and the metal ion environment show the distortions usual for bis(terpyridine) systems. Distortions are less marked in the bis((1,10-phenanthrolin-2-yl)(pyridin-2-yl)amine)iron(II) cation in which each tridentate unit forms one five-membered and one six-membered chelate ring. [Ru(trpy)2] [ClO4]2.(H2O)1.1: tetragonal, space group I 41/a, a, b 12·527(2), c 40·202(11) Å, Z 8. [Os(trpy)2] [ClO4]2.(H2O)0·5: monoclinic, space group P 21/n, a 8·842(3), b 8·861(1), c 39·22(2) Å, β93·89(2)°, Z 4. [Fe(phpyam)2] [BF4]2.(H2O)2: triclinic, space group P -1, a 12·43(1), b 12·45(1), c 13·35(1) Å, α 62·70(10), β 78·55(8), γ 72·46(9)°, Z 2.


1985 ◽  
Vol 40 (8) ◽  
pp. 1073-1076 ◽  
Author(s):  
Johannes Beck ◽  
Eberhard Schweda ◽  
Joachim Strähle

AbstractMoN(N3)2Cl(terpy) is formed by the reaction of MoCl4(C2H5CN)2 with (CH3)3SiN3 and subsequent addition of terpy. This complex appears also as the main product o f the heterogeneous reaction between MoCl3(terpy) and (CH3)3SiN3. It crystallizes in the monoclinic space group P 21/c with the lattice parameters a = 875.5, b = 1041.4, c = 1891.3 pm, β = 97.00°, Z = 4. The central Mo atom is seven-coordinated in the form of a slightly distorted pentagonal bipyramid, the nitrido and chloro ligands being in axial positions. The triply bonded nitrido ligand ( Mo - N 1 = 166.2 pm) causes a strong trans effect, resulting in a long Mo-Cl distance of 271.9 pm.


1996 ◽  
Vol 49 (12) ◽  
pp. 1301 ◽  
Author(s):  
GW Allen ◽  
ECH Ling ◽  
LV Krippner ◽  
TW Hambley

The preparation and purification of [Pt( hpip )Cl2] and [Pd( hpip )Cl2] ( hpip = homopiperazine = 1,4-diazacycloheptane) are described. Crystal structures of [Pt( hpip )Cl2] and [Pd( hpip )Cl2] have been determined by X-ray diffraction methods and refined to R values of 0.023 (932 F) and 0.023 (948 F). The crystals of [Pt( hpip )Cl2] are orthorhombic, space group Pbcm , a 7.7019(8), b 9.8080(12), c 12.1944(14) Ǻ, and those of [Pd( hpip )Cl2] are monoclinic, space group P21/m, a 6.1001(9), b 11.527(2), c 6.458(I) Ǻ, β 106.30(2)°. The seven- membered rings of the ligands in both complexes adopt boat-like conformations in which the five- membered chelate ring has an eclipsed N-C-C-N group and the six- membered chelate ring adopts a chair conformation. Molecular mechanics methods were used to investigate whether this conformation was a crystallographic artefact but it was found to be real. An alternative conformation in which the six-membered chelate ring adopts a skew-boat conformation was also investigated. It was found to be less stable than the conformation observed in the crystal structures, but to a degree that depends on whether non-bonded interactions involving the metal atom were included or not.


1967 ◽  
Vol 45 (20) ◽  
pp. 2303-2316 ◽  
Author(s):  
J. S. Stephens ◽  
C. Calvo

β-Zn3(PO4)2 crystallizes in the monoclinic space group P 21/c with lattice parameters, a = 9.393(3) Å, b = 9.170(6) Å, c = 8.686(3) Å, β = 125.73(10)°, and Z = 4. The three independent cations are strongly ligated to 4, 5, and 5 oxygen atoms, with average Zn—O bond distances of 1.98 ± 0.09 Å, 2.10 ± 0.10 Å, and 2.08 ± 0.13 Å respectively. In addition there are two longer Zn—O distances of 2.51 Å and 2.55 Å in this structure. The PO4 groups exist as independent, nearly regular tetrahedra, with each oxygen atom ligated to two cations. Unlike the structures found for the α and γ phases of Zn3(PO4)2, which contain ribbons and sheets respectively as the basic cation coordination motif, the structure of β-Zn3(PO4)2 contains interconnected sheets.


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.


1996 ◽  
Vol 51 (3) ◽  
pp. 319-324 ◽  
Author(s):  
Silke Busche ◽  
Karsten Bluhm

Abstract Single crystals of the new compound Ba2KZn3(B3O6)(B6O13) were obtained by using a B2O3 flux technique; they crystallize in an as yet unknown structure type. X-ray investigations led to the space group Ci1-P1̄ (Nr.2) with lattice parameters a = 705.2(2), b = 712.5(2), c = 1880.3(6), a = 93.43(3)°, β = 90.72(2)°, γ = 119.57(2)°, Z = 2. The structure contains (B3O6)3--rings and a new discrete (B6O13)8- anion, which is composed of two BO4 and two B2O5 units. Zn2+ is tetrahedrally coordinated by oxygen and two out of three tenfold coordinated Ba-sites are statistically occupied by Ba2+ and K+.


1988 ◽  
Vol 43 (5) ◽  
pp. 525-528 ◽  
Author(s):  
Edmund Hartmann ◽  
Joachim Strähle

1,3-Bis(4-ethoxyphenyl)triazenido silver(I) (1) is obtained from equimolar amounts of the triazenido anion and AgNO3 in THF/CH3CN. 1 forms in pyridine the dimer [Ag(EtOC6H4NNNC6H4OEt)·py]2 (2) which crystallizes as yellow pyridine solvate 2·2 py in the monoclinic space group P21/n and a = 1067.1(7), b = 1764.5(9), c = 1373.0(9) pm, β = 106.46(7)°, Z = 2. In the centrosymmetric dimer 2, two triazenido ligands bridge two Ag(I) atoms with their atoms N1 and N3 forming an eight-membered heterocycle Ag2N6 with a short Ag-Ag interaction of 272.6 pm. To each Ag atom an additional pyridine ligand is weakly coordinated with a distance Ag-N40 = 245.5 pm. The bond axis N1 - Ag-N3′ within the heterocycle is not linear (158.5°). The Ag-N distances to the N-atoms of the triazenido ligand are 217.6 and 218.5 pm.


1990 ◽  
Vol 45 (8) ◽  
pp. 1193-1196 ◽  
Author(s):  
Klaus Brodersen ◽  
Axel Knörr

[Hg2(p-SC6H4NO2)]NO3 is formed by the reaction of p-nitrothiophenol with dimercury(I)-dinitrate in methanol. It crystallizes in the monoclinic space group P21/n with a = 1175.5(9) pm, b = 1079.8(8) pm, c = 876.2(8) pm, β = 110.74(4)° and Z = 4. The crystal structure has been determined by X-ray diffraction and refined to an R-value of 0.052. The results show that the compound exists as a chain structure of [—®S(C6H4NO2)— Hg— Hg—]n with nitrate ions connecting the chains.


Author(s):  
Rénald David

The title compound, tetrasodium heptanickel hexaarsenate, was obtained by ceramic synthesis and crystallizes in the monoclinic space groupC2/m. The asymmetric unit contains seven Ni atoms of which two have site symmetry 2/mand three site symmetry 2, four As atoms of which two have site symmetrymand two site symmetry 2, three Na atoms of which two have site symmetry 2, and fifteen O atoms of which four have site symmetrym. The structure of Na4Ni7(AsO4)6is made of layers of Ni octahedra and As tetrahedra assembled in sheets parallel to thebcplane. These layers are interconnected by corner-sharing between NiO6octahedra and AsO4tetrahedra. This linkage creates tunnels running along thecaxis in which the Na atoms are located. This arrangement is similar to the one observed in Na4Ni7(PO4)6, but the layers of the two compounds are slightly different because of the disorder of one of the Ni sites in the structure of the title compound.


2015 ◽  
Vol 2015 ◽  
pp. 1-5
Author(s):  
Shuang Gao ◽  
Hai-Tao Qu ◽  
Fei Ye ◽  
Ying Fu

A new compound,N-dichloroacetyl-3,4-dihydro-3-methyl-6-chloro-2H-1,4-benzoxazine, was synthesized and characterized. The crystal structure of the title compound (C11H10Cl3NO2,Mr=294.55) has been determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space groupP21/c, witha=6.7619(14),b=24.866(5),c=9.737(3) Å,α=90.00,β=130.982(18),γ=90.00°,V=1235.9(5) Å3,Z=4,Dx=1.583 Mg/cm3,λ(Mo  Ka)=0.71073 Å,F(000)=600,μ=0.729 mm−1,R=0.0476, andwR=0.1274for 2217 reflections withI>2σ(I).


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