Zur Struktur des Pentaazadienidions [tol-N=N-N-N=N-tol]-. Synthese und Kristallstruktur von Cs2(18-Krone-6)(tolN5tol)2 und (NH4)[Cr(NH3)6(H2O)4](tolN5tol)4 / The Structure of the Pentaazadienide Anion [tol-N=N—N—N=N-tol]-. Synthesis and Crystal Structure of Cs2(18-Crown-6)(tolN5tol)2 and (NH4)[Cr(NH3)6(H2O)4](tolN5tol)4

1993 ◽  
Vol 48 (11) ◽  
pp. 1574-1580 ◽  
Author(s):  
Susanne Dieterich ◽  
Joachim Strähle

A concentrated solution of CsCI, 18-crown-6, and tol-N=N—N(H)—N=N-tol in aqueous ammonia affords Cs2(18-crown-6)(tolN5tol)2, which crystallizes in the triclinic space group P1̄ with a = 852.6(2), b = 1139.4(3), c = 1373.9(4) pm, α = 104.17(3), ß = 95.94(2), γ = 110.74(2)°, Ζ = 1. In the structure centrosymmetrical [Cs2(18-crown-6)]2+ moieties are packed with pairs of 1,5-bis(tolyl)pentaazadienide anions to built up columns along [100]. The N—N distances N1 —N2 = 128 pm and N4—N5 = 129 pm in the pentaazadienide anions indicate localized double bonds, while the distances N2—N3 and N3—N4 of 134 pm can be assigned to single bonds. A mixture of Cr(NH3)63+ and tolNNN(H)NNtol in concentrated aqueous ammonia yields triclinic (NH4)[Cr(NH3)6(H2O)4](tolN5tol)4 crystallizing in the space group P l with the lattice parameters a = 1561.1(1), b = 1619.3(3), c = 1703.3(2) pm, α = 107.03(1), β = 116.81(1), γ = 101.75(1)°, Ζ = 2. The structure contains tolN5tol- anions, NH4+ cations and [Cr(NH3)6(H2O)4]3+ complexes in which four triangular faces of the Cr(NH3)6 octahedron are capped by water molecules which are linked via hydrogen bonds. Within the pentaazadienide anions which are connected with the [Cr(NH3)6(H2O)4]3+ complexes also via hydrogen bonds an indication for localized double bonds Ν1=Ν2 and N4=N 5 has been obtained.

1996 ◽  
Vol 51 (10) ◽  
pp. 1464-1468 ◽  
Author(s):  
Walter Frank ◽  
Guido J. Reiß

Tris(guanidinium) hexachlororhodate(III) monohydrate, [C(NH2)3]3[RhCl6] · H2O (1 ) has been obtained by the reaction of rhodium(III) chloride with guanidine hydrochloride in hydrochloric acid solution. 1 crystallizes in the triclinic space group P1̅ (a = 7.6013(9) Å, b = 8.6912(10) Å, c = 15.956(2) Å, α = 93.177(10)°, β = 101.691(10)°, γ = 113.995(9)°, V = 931.8(2), Z = 2). Two crystallographically independent hexachlororhodate ions, three crystallographically independent guanidinium ions and one water molecule are linked by a complex framework of hydrogen bonds.


1999 ◽  
Vol 54 (6) ◽  
pp. 747-750 ◽  
Author(s):  
Joachim Pickardt ◽  
Pirka Wischlinski

Crystals o f the complex [K (benzo-18-crown-6][Zn(CN)3] H2O were obtained from a solution o f Zn(CN)2, KCN, and benzo-18-crown-6 in water/methanol. The compound crystallizes in the triclinic space group PI (no. 2),: Z = 2, a = 818,6(5), b = 1236,7(8), c = 1359,6(6) pm, a = 67,02(4), β = 87,38(4), 7 = 75,46(5). Each Zn atom is bonded to one bridging cyanide ion to give chains -Zn(CN)Zn -, and to two terminal CN groups. The N atom of one of the terminal CN groups interacts with a potassium ion o f the [K (benzo-18-crown-6)]+ unit. The coordination spheres of the K ions are completed by water molecules, which in turn form hydrogen bonds to N atoms of terminal CN groups of neighbouring chains, whereby puckered sheets are formed


1992 ◽  
Vol 47 (4) ◽  
pp. 460-464 ◽  
Author(s):  
Klaus Brodersen ◽  
Jürgen Hofmann

The structure of bis(m-aminobenzonitrile)dimercury(I) dinitrate, [Hg2(m -NH2C6H4CN)2](NO3)2 has been determined by single crystal X-ray diffraction techniques and refined to an Rw-value of 0.022. The crystals are triclinic, space group P1 with a = 5.4878(1) Å, b = 8.4085(1) Å, c = 9.6062(1) Å, α = 92.599(3)°, β = 94.763(3)°, γ = 89.614(3)° and Z = 1.The Hg22+-ion [Hg-Hg 2.524(1) Å] is approximately axially coordinated to amino nitrogen atoms [Hg - N 2.209(4) Å, Hg - Hg - N 169.5(3)°]. Additional amino hydrogen bonds to oxygen are building chains along the b-axis containing units of L - Hg - Hg - L groups.


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.


1988 ◽  
Vol 43 (5) ◽  
pp. 529-532 ◽  
Author(s):  
Raimund Schmid ◽  
Johannes Beck ◽  
Joachim Strähle

Cs+(tolN5tol)- (1) is formed as a yellow crystalline precipitate after addition of a concentrated aqueous solution of CsCl to a concentrated solution of 1,5-Bis(p-tolyl)pentaazadiene(1,4) in ammonia. 1 crystallizes in the orthorhombic space group Pccn with a = 3169(1), b = 434.3(2), c = 1109.4(7) pm, Z = 4. The structure contains (tolN5tol)- anions and Cs+ cations both occupying two-fold axes. The all-trans N5 zigzag chain is planar with localized double bonds N1 - N2 and N2′ - N1′ of 127.7 pm and shortened single bonds N2-N3 and N3-N2′ of 136.9 pm. The tolyl substituents are titled by 25.5° against the plane of the N atoms. Cs+ is surrounded in a square antiprismatic arrangement by eight N atoms of four N5 chains with distances Cs-N in the range of 314.6 to 366.2 pm.


1985 ◽  
Vol 40 (6) ◽  
pp. 736-739 ◽  
Author(s):  
Herbert W. Roesky ◽  
Jörg Sundermeyer, ◽  
Jürgen Schimkowiak ◽  
Peter G. Jones ◽  
Mathias Noltemeyer ◽  
...  

AbstractThe reaction of N,N-dichlorophenylsulphonamide with tungsten hexacarbonyl in refluxing CCl4 leads in good yield to the yellow polymeric complex [(PhSO2N)2WCl2]x, which may be converted to the octahedral nitrene complex [(PhSO2N)2WCl2(CH3CN)2] by recrystallisation from aceto­nitrile. Crystals of the acetonitrile complex are triclinic, space group P 1̅, a = 820.7(2), b = 1128.8(3), c = 1286.9(3) pm, α = 89.25(3), β = 89.54(3). γ = 72.67(2)°, Z = 2, R = 0.027 for 2527 unique observed reflections.


1995 ◽  
Vol 50 (8) ◽  
pp. 1175-1180 ◽  
Author(s):  
Hans-Christian Böttcher ◽  
Helmut Hartung ◽  
André Krug

[{Ru(CO)3Cl2}2] reacts with the in situ prepared reagent Li2[Fe(CO)3(PBut2)2] to give the new heterobinuclear complex [FeRu(CO)5(μ-PBut2)2] (1). Crystals of 1 are isomorphous to those of the known compound [Fe2(CO)5(μ-PBut2)2] (2) and crystallize in the triclinic space group P1̄ with a = 867,5(1), b = 1181,0(2), c = 1373,1(2) pm; α = 76,64(1), β = 79,72(1) and γ = 76,48(1)°. A double bond between the two metal atoms concluded for 2 from the results of EHMO calculations is also proposed for 1 (Fe=Ru: 259,8(1) pm).


1975 ◽  
Vol 53 (15) ◽  
pp. 2345-2350 ◽  
Author(s):  
Monique Authier-Martin ◽  
André L. Beauchamp

The title compound belongs to space group P21/c with a = 23.99(1), b = 4.245(2), c = 25.98(1) Å, β = 117.58(7)°, and Z = 8. The structure was solved by the heavy-atom method and refined by block-diagonal least squares on 2589 independent observed reflections. All non-hydrogen atoms were refined anisotropically and some of the hydrogen atoms were located but their parameters were not refined. The final values of R and Rw were 0.042 and 0.047, respectively.The two nonequivalent mercury atoms have very similar environments. Two short Hg—Cl bonds (2.34–2.38 Å) at ∼ 165° define a quasi-molecular HgCl2 unit. Overall octahedral coordination is completed with two chloride ions at 2.76–2.84 Å and two chlorine atoms at 3.19–3.26 Å on neighboring HgCl2 quasi-molecules. HgCl6 octahedra share edges to form twofold ribbons in the b direction. This pattern of octahedra is identical with the onereported for β-NH4HgCl3. The cations are pairs of N(1)-protonated adenine molecules linked by two N(10)—H(10)… N(7) hydrogen bonds and stacked in the b direction. Water molecules act as acceptors in moderately strong hydrogen bonds with acidic protons H(1) and H(9) of adeninium ions. Other generally weaker hydrogen bonds exist between the various parts of the structure.


1988 ◽  
Vol 43 (9) ◽  
pp. 1161-1166 ◽  
Author(s):  
Hans-Jürgen Meyer ◽  
Joachim Pickardt

Abstract By diffusion of methanolic solutions of hexamethylenetetramine into aqueous solutions of hexacyanoferrates(III) of sodium and potassium, resp., single crystals of the adducts were ob­tained. Na3[Fe(CN)6] · 2C6H12N4-5H2O, orthorhombic, space group Pca21. Z = 4, a = 14.122(4). b = 14.380(4), c = 14.381(4) Å, 3153 reflections, R = 0.044. K3[Fe(CN)6]•2C6H12N4-4H2O, triclinic, space group P1̄, Z = 4, a = 14.125(4), b = 17.808(4), c =14.116(4) Å, α = 114.14(5), β = 94.91(4), γ = 108.36(5)°. 5550 reflections, R = 0.042. Both structures may be regarded as Elpasolite-Iike arrangements of [Fe(CN)6]3- ions, C6H12N4 molecules and [M2(OH2)x]3+ units (M = Na, K; x = 5, 4), linked together unsymmetrically by M-N contacts of metal ions and nitrogen atoms with mean distances of Na-NHMT = 264 pm. Na-NCYan = 243 pm, K-NHMT = 293 pm and K-Ncyan = 290 pm. Stabilization of the crystal structures is obtained by N---H-O hydrogen bonds of coordination water molecules in three dimensions.


2011 ◽  
Vol 66 (8) ◽  
pp. 868-870 ◽  
Author(s):  
Florian Kraus ◽  
Sebastian A. Baer

The synthesis and crystal structure of the first ammine complex of a cerium fluoride, tetraammine tetrafluorido cerium(IV) ammonia (1/1), [CeF4(NH3)4] ・NH3, are presented. The compound crystallizes in the form of colorless, block-shaped single crystals in the tetragonal space group P4/ncc with a = 9.03215(9), c = 10.96404(17) Å , V = 894.443(19) Å3, and Z = 4. The compound contains discrete [CeF4(NH3)4] molecules interconnected by N-H···F hydrogen bonds.


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