Synthesis and crystal structure of anhydrous Na[MnO4]

2016 ◽  
Vol 71 (9) ◽  
pp. 993-995 ◽  
Author(s):  
Jörg M. Bauchert ◽  
Harald Henning ◽  
Thomas Schleid

AbstractThere are numerous reports in the literature about the amount of hydrate water in sodium permanganate, which is said to be between one half and three water molecules per Na[MnO4]. Because no structural descriptions of the hydrate and the anhydrous compound can be found yet, this work reports the synthesis of anhydrous Na[MnO4] via the Muthmann method and its crystal structure. Na[MnO4] crystallizes as dark purple needles in the monoclinic space group P21/n with a = 572.98(5), b = 842.59(7), c = 715.47(6) pm, β = 92.374(3)° and Z = 4. As such and with its isotype to Ag[MnO4], Na[MnO4] completes the series of anhydrous alkali-metal permanganates, comprising Li[MnO4] (orthorhombic, Cmcm, Cr[VO4] type) and the isostructural heavier congeners A[MnO4] (A = K, Rb, Cs; orthorhombic, Pnma, Ba[SO4] type).

2015 ◽  
Vol 70 (7) ◽  
pp. 455-459 ◽  
Author(s):  
Sidra Nawaz ◽  
Tobias Rüffer ◽  
Heinrich Lang ◽  
Muhammad Ashraf Shaheen ◽  
Saeed Ahmad ◽  
...  

AbstractA copper(II) polymeric complex {[Cu(phen)2(CN)][Ag(CN)2] · 3H2O}n, 1 (phen = 1,10-phenanthroline), has been prepared and structurally characterized. The compound crystallizes in the monoclinic space group P21/c with [Cu(phen)2(CN)]+ and [Ag(CN)2]− units and three water molecules. The cationic and anionic units are linked to each other through M-π and π–π interactions. The array is extended further by hydrogen bonding and π–π interactions to form a 3D network.


2019 ◽  
Author(s):  
Roberto Köferstein

Two new three-dimensional frameworks with zeolite-like channels were prepared in thepresence of 1,6-diaminohexane. Cu1.5(H3N–(CH2)6–NH3)0.5[C6H2(COO)4]·5H2O (1)crystallizes in the triclinic space group P with a = 772.56(7), b = 1110.36(7), c = 1111.98(8)pm, α = 98.720(7)°, β = 108.246(9)°, and γ = 95.559(7)°. Cu2(H3N–(CH2)6–NH3)0.5(OH)[C6H2(COO)4]·3H2O (2) crystallizes in the monoclinic space group P2/c with a =1159.34(11), b = 1059.44(7), c = 1582.2(2) pm, and β = 106.130(11)°. The Cu2+ coordinationpolyhedra are connected by [C6H2(COO)4]4– anions to yield three-dimensional frameworkswith wide centrosymmetric channel-like voids. Complex 1 reveals voids extending along[100] with diagonals of 900 pm and 300 pm, whereas in complex 2 the diagonal of the nearlyrectangular crossection of the channels extending parallel to [001] is 900 pm. The negativeexcess charges of the frameworks are compensated by [H3N–(CH2)6–NH3]2+ cations, whichoccupy the voids along with water molecules. The [H3N–(CH2)6–NH3]2+ cations are notconnected to Cu2+ and have served as templates.


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.


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.


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)


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).


Author(s):  
HEINER HÜCKSTÄDT ◽  
HEINER HOMBORG

Bis(phthalocyaninato(2-)iridium(II)) reacts in methanol with excess tetra(n-butyl)ammonium hydroxide to yield tetra(n-butyl)ammonium hydroxomethoxophthalocyaninato(2-)iridate(III). The complex salt crystallizes as a methanol solvate in the monoclinic space group P21/n(No. 14) with cell parameters a = 12.510(1) Å, b = 19.561(3) Å, c = 18.489(2) Å, = 90.42(1) °, Z = 4. The Ir atom is hexacoordinated with four isoindole N atoms ( N iso ) of the severely saddled pc ligand and two O atoms of the hydroxide ( O 1) and methoxide ( O2 ) ligand respectively in a mutual trans arrangement. The average Ir-N iso distance is 1.981(5) Å, the Ir-O1 distance 2.038(7) Å and the Ir-O2 distance 2.061(6) Å. The O atom of the solvate ( O3 ) is bound to O2 by a strong hydrogen bond with an O2 - O3 distance of 2.60(1) Å.


1993 ◽  
Vol 48 (8) ◽  
pp. 1138-1142 ◽  
Author(s):  
Daryl L. Ostercamp ◽  
Lisa M. Preston ◽  
Kay D. Onan

The unit cell of N-tert-butyl-3-(tert-butylimino)-2-nitropropen-1-amine (4) is monoclinic, space group P21/C, with a = 9.669(4), b = 16.415(6), c = 17.341 (7) Å, and Z = 4. Hydrolysis of 4 leads to (E)-3-(N-tert-butylamino)-2-nitro-2-propenal (5), whose unit cell is monoclinic, space group P21/n, with a = 6.821(1), b = 20.707(6), c = 6.303(1)Å, and Z = 4. Compounds 4 and 5 both possess C2 symmetry in the solid state, their “U-shaped” conjugated cores being essentially planar. In each case this planarity is enforced by an intramolecular hydrogen bond.


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