Synthesis and Crystal Structure of M([12]crown-4)2O3 · 1.5 NH3 with M = K, Rb

2009 ◽  
Vol 64 (11-12) ◽  
pp. 1325-1328 ◽  
Author(s):  
Hanne Nuss ◽  
Martin Jansen

The two new ozonide compounds K([12]crown-4)2O3 ・ 1.5 NH3 (1) and Rb([12]crown-4)2O3 ・ 1.5 NH3 (2) were synthesized from the binary alkali metal ozonides and [12]crown-4 in liquid ammonia. The air- and temperature-sensitive red, needle-shaped compounds crystallize isostructurally in the non-centrosymmetric space group Fdd2 (no. 43) with 16 formula units per unit cell. The lattice parameters are a = 26.917(8), b = 43.25(1), c = 7.823(2) Å, V = 9108(5) Å3; and a = 26.730(6), b = 44.70(1), c = 7.739(2) Å, V = 9245(4) Å3 for 1 and 2, respectively. The structure comprises rod-like [([M([12]crown-4)2(NH3)]O3)2(NH3)] supramolecular units, forming a fishbone pattern parallel to (001). The ozonide anions are separated from the metal cations and interact only weakly with two ammonia molecules via N-H・ ・ ・O hydrogen bonds

2006 ◽  
Vol 61 (10) ◽  
pp. 1205-1208 ◽  
Author(s):  
Hanne Nuss ◽  
Martin Jansen

Cs([18]crown-6)Au ・ 8NH3 was synthesized from CsAu and [18]crown-6 in liquid ammonia. The extremely air- and temperature-sensitive colorless, block-shaped crystals were analyzed by single crystal X-ray diffractometry. The compound forms triclinic crystals of space group P1 (no. 1) with a = 8.765(2), b = 11.186(2), c = 13.997(3) Å , α = 86.180(6), β = 89.669(6), γ = 83.774(6)°, V = 1361.2(4) Å3. The crystal structure consists of ammonia nets extending perpendicular to [110] in which the Cs([18]crown-6) fragments and the auride anions are embedded


2015 ◽  
Vol 70 (3) ◽  
pp. 161-164 ◽  
Author(s):  
Patrick Woidy ◽  
Florian Kraus

AbstractVanandium trifluoride reacts with dry liquid ammonia under the formation of lilac plate-shaped crystals of mer-triammine trifluorido vanadium(III) (1), mer-[VF3(NH3)3]. Single-crystal X-ray analysis was carried out at low temperature to elucidate the structure. The compound crystallizes in the monoclinic space group P21/c with a = 5.7284(4), b = 9.2033(5), c = 10.5271(6) Å, β = 91.795(6)°, and V = 554.72(6) Å3 at 123 K with Z = 4. The discrete [VF3(NH3)3] molecules are interconnected by hydrogen bonds.


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.


1991 ◽  
Vol 46 (11) ◽  
pp. 1539-1543 ◽  
Author(s):  
Bernhard Neumüller

The title compound 1 has been prepared by the reaction of i-PrInCl2 with LiCH(SiMe3)2 in diethylether at -30 °C. The colorless substance 1 was characterized by NMR, IR, and RE spectroscopy, as well as by mass spectrometry. 1 is dimer in solution and the solid state and crystallizes in the space group P21/c with the cell parameters a = 1206.4(3) pm, b = 905.7(2) pm, c = 1591.2(5) pm, and β = 101.18(2)°. The unit cell contains two centrosymmetrical dimeric molecules.


1977 ◽  
Vol 32 (11) ◽  
pp. 1271-1276 ◽  
Author(s):  
Jochen Ellermann ◽  
Norbert Geheeb ◽  
Gerd Zoubek ◽  
Gerhard Thiele

X-ray investigations of brown crystals, formed as a by-product in the reaction of Co2(CO)8 with (C6H5)2P(CH2)2P(C6H5)2 show the existence of the complexCo2(µ-CO)2(CO)4μ-[(C6H5)2P]2NH.The triclinic unit cell (space group PĪ ) contains two complex molecules and one molecule benzene as a solvate. The ligand (C6H5)2P(CH2)2P(C6H5)2, prepared by literature methods, obviously sometimes contains some [(C6H5)2P]2NH. The compoundCo2(μ-CO)2(CO)4μ-[(C6H5)2P]2NH can also be directly synthesized by the reaction of Co2(CO)8 with [(C6H5)2P]2NH.


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.


1989 ◽  
Vol 44 (5) ◽  
pp. 615-618 ◽  
Author(s):  
Evamarie Hey ◽  
S. Bruce Wild ◽  
Simon G. Bott ◽  
Jerry L. Atwood

The unit cell of (R*,R*)-(±)-[(η5-C5H5){1.2-C6H4(PMePh)2}Fe(PCl3)]Cl · 2 MeCN is orthorhombic, space group Pccn, with a = 1531.2(3). b = 2202.7(20). c = 1874.6(16) pm, and Z = 8. The salt crystallizes as a racemic compound with four pairs of asymmetric cations of opposite helicity and associated anions and solvent molecules in each unit cell.


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.


1988 ◽  
Vol 43 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Dieter Fenske ◽  
Eberhard Böhm ◽  
Kurt Dehnicke ◽  
Joachim Strähle

Abstract The title compound has been prepared by the reaction of N-trimethylsilyl-iminotriphenylphos-phorane with copper(II) chloride in boiling CCl4 /C2H5OH, and forms moisture sensitive crystals, which are green in transmittance and black in reflexion. [Me3SiNPPh3 · CuCl2 ] 2 was characterized by its IR spectrum as well as by a crystal structure determination (4197 observed, independent reflexions, R = 0.049). The lattice dimensions are at 20 °C: a = 1102.7. b = 1407.3. c = 1560.2 pm; β = 94.27°; space group P21/n with two formula units in the unit cell. The complex consists of centrosymmetric, dimeric molecules with a planar Cu2 Cl2 ring (Cu-CI bond lengths 229 and 231 pm). A terminally bonded CI atom (Cu-CI = 221 pm) and the N atom of the Me3SiNPPh3 ligand (Cu-N = 198.5 pm) complete the coordination number four of the nearly planar surroundings of the Cu atoms.


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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