scholarly journals Complexes with macrocyclic ligands. II. The crystal structures of HgCl2•18-crown-6 and CdCl2•18-crown-6, and the FAB mass spectrum of HgCl2•18-crown-6

1984 ◽  
Vol 62 (2) ◽  
pp. 332-335 ◽  
Author(s):  
Christopher Robin Paige ◽  
Mary Frances Richardson
Keyword(s):  
Mass Spectrum ◽  
Crystal Structures ◽  
Macrocyclic Ligands ◽  
Metal Coordination ◽  
Chlorine Atoms ◽  
Space Group

HgCl2 and CdCl2 form 1:1 complexes with 1,4,7,10,13,16-hexaoxacyclooctadecane (18-crown-6). The complexes are isostructural. The metal coordination is hexagonal bipyramidal, with chlorine atoms strongly coordinated in the axial positions and the 18-crown-6 in the equatorial place. The symmetry of the complex is crystallographically required to be [Formula: see text], but is very nearly [Formula: see text]. The Hg—Cl, Hg—O, Cd—Cl, and Cd—O distances are 2.314(1), 2.825(4), 2.3645(5), and 2.752(1) Å, respectively. Crystals of HgCl2•18-crown-6 are rhombohedral, space group [Formula: see text], a = 7.746(2) Å, α = 95.26(3)°, Z = 1 unit of HgCl2C12H24O6, R = 0.026 for 543 independent reflections with θ < 25°, I > 3σ(I). Crystals of CdCl2•18-crown-6 are also rhombohedral, space group [Formula: see text], a = 7.712(3) Å, α = 95.57(2)°, Z = 1 unit of CdCl2C12H24O6, R = 0.022 for 534 independent reflections with θ < 25°, I > 3σ(I).

scholarly journals Kristallstrukturen zweier Kupfer(II)-Cyclam-Komplexe: [{CuCl(C10N4H24)}2][CdCl4] und [Cu(C10N4H24)][CdCl3(H2O)2]Cl / Crystal Structures of Two Copper(II) Cyclam Complexes: [{CuCl(C10N4H24 )}2][CdCl4] and [Cu(C10N4H24)][CdCl3 (H2O)2]Cl

1995 ◽  
Vol 50 (5) ◽  
pp. 828-832 ◽  
Author(s):  
Joachim Pickardt ◽  
Isabella Hoffmeister
Keyword(s):  
Crystal Structures ◽  
Copper Atom ◽  
Water Molecules ◽  
Cadmium Atom ◽  
Bridging Ligands ◽  
Chlorine Atoms ◽  
Space Group ◽  
Distorted Octahedra ◽  
Cyclam Complexes

Abstract Crystals of both complexes were obtained by evaporation of the ethanol solvent. The crystals of [{CuCl(C10N4H24)}2][CdCl4] are tetragonal, space group I4̄2d, Z = 4, a = b = 1784.1(11), c = 1101.1(8) pm. Each copper atom is bonded to one cyclam ligand and two chlorine atoms which are acting as bridging ligands and connect the copper atoms to chains of distorted octahedra. Distorted tetrahedra of CdCl4 are situated in cavities between these chains. The crystals of [Cu(C10N4H24)][CdCl3(H2O)2]Cl are monoclinic (b), space group C2/c, Z = 4, a = 1581.9(8), b = 1323.3(7), c = 924.0(5) pm, β = 94.31(5)°. Cadmium is coordinated to four chlorine atoms and two water molecules, while all of the chlorine atoms act as bridging ligands connecting every cadmium atom to two adjacent cadmium atoms and to two copper atoms which lie in plane with the N atoms.

Synthese und Kristallstruktur der (p-Brombenzyl)triphenylphosphonium-bromide: [(p-Br-C6H4-CH2)P(C6H5)3]+B-;[(p-Br-C6H4-CH2)P(C6H5)3]+Br2- und [(p-Br-C6H4-CH2)P(C6H5)3]+Br3-/ Synthesis and Crystal Structures of (p-Bromobenzyl)triphenylphosphonium Bromides, [(p-Br-C6H4-CH2)P(C6H5)3]+Br-;[(p-Br-C6H4-CH2)P(C6H5)3]+Br- and [(p-Br-C6H4-CH2)P(C6H5)3]+Br3-

1996 ◽  
Vol 51 (10) ◽  
pp. 1443-1448 ◽  
Author(s):  
H. Vogt ◽  
D. Wulff-Molder ◽  
M. Meisel
Keyword(s):  
Crystal Structures ◽  
Weak Interactions ◽  
Orthorhombic Space Group ◽  
Tetrahedral Geometry ◽  
Chlorine Atoms ◽  
Triclinic Space Group ◽  
Space Group ◽  
Triphenylphosphonium Bromide

(p-Bromobenzyl)triphenylphosphonium Bromide, [(p-Br-C6H4-CH2)P(C6H5)3]+Br- · (CH2Cl2)2.5 (1) has been prepared by the reaction of triphenylphosphine with p-bromobenzylbromide and its structure determined (triclinic, space group P1̅, Z = 2, a = 1198.03(12), b = 1245.80(11), c = 1258.42(12)pm, a = 100.170(8), β = 103.543(9), γ = 1 18.158(7)°. The compound exists as Br- anions and [(p-Br-C6H4- CH2)P(C2H5)3]+ cations, with weak interactions between the chlorine atoms of the CH2Cl2 molecules and the bromine bonded in the cation. [p-Br-C6H4-CH2)P(C6H5)3]Br2 (2) and [(p-Br-C6H4-CH2)P(C6H5)3]Br3·(CH2Cl2)1.5 (3) have been obtained by reactions of the corresponding amounts of bromine with 1 in methylenechloride solution. The yellow-red crystals of 2 are orthorhombic, space group Pccn, Z = 8, a = 2060.8(3), b = 1223.6(4), c = 1860.8(3) pm. Compound 2 exists as [p-Br-C6H4-CH2)P(C6HO5)3]+ cations and linear Br2-4 units with a bromide-bromine distance of 297.3(4) pm. The red crystals of (3) are triclinic, space group P1̅, Z = 2, a = 1 171.16(7), b = 1260.97(8), c = 1270.35(7)pm, α = 65.510(5), β = 75.811(5), γ = 62.320(5)°, and contain [(p-Br-C6H4-CH2)P(C6H5)3]+ cations and linear, slightly asymmetrical Br-3 anions. In all cases the cation has a slightly irregular tetrahedral geometry around the P atom.

Die Reaktionen von Wolframhexachlorid mit überschüssigem 2,2-Dimethylpropylidinphosphan; die Kristallstrukturen von WCl5P2(C5H9)3, WCl4P5(C5H9)5 und [C3(C4H9)3]+[WCl5(C4H9C≡CC4H9)]- / The Reactions of Tungsten Hexachloride with Excess 2,2-Dimethylpropylidynephosphane; the Crystal Structures of WCl5P2(C5H9)3, WCl4P5(C5H9)5, and [C3(C4H9)3]+[WCl5(C4H9C=CC4H9)]⁻

1991 ◽  
Vol 46 (4) ◽  
pp. 519-529 ◽  
Author(s):  
Frank Weller ◽  
Irene Pauls ◽  
Kurt Dehnicke ◽  
Gerd Becker
Keyword(s):  
Molecular Structure ◽  
Crystal Structures ◽  
Phosphorus Atom ◽  
Type Structure ◽  
Tungsten Atom ◽  
Chlorine Atoms ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations ◽  
Tungsten Hexachloride

The reaction of tungsten hexachloride with excess 2,2-dimethylpropylidynephosphane, C4H9—C≡P, leads to the tungsten phosphaalkyne clusters WCl5P2(C5H9)3 and WCl4P5(C5H9)5, as well as to the tris(t-butyl)cyclopropenium pentachloro tungsten alkyne complex [C3(C4H9)3]+[WCl5(C4H9C≡CC4H9)]-. All complexes were characterized by X-ray structure determinations.WCl5P2(C5H9)3: Space group P2,/n, Z = 8,4653 observed unique reflexions, R = 0.033. Lattice dimensions at 20 °C: a = 1577.8(2), b = 1661.3(1), c = 1869.8(2) pm, β = 110.64(1)°. The compound has a molecular structure, in which the tungsten atom is surrounded by three chlorine atoms, three carbon atoms with W—C distances of 182, 230, and 231 pm, and by one phosphorus atom with W—P = 246 pm.WCl4P5(C5H9)5: Space group P21/c, Z = 4, 3517 observed unique reflexions, R = 0.043. Lattice dimensions at 20 °C: a = 1770.0(2), b = 1032.9(2), c = 1876.0(3) pm, β = 102.86(1)°. The complex has a molecular structure, in which the tungsten atom is surrounded by two chlorine atoms, two carbon atoms with W—C distances of 189 and 215 pm, as well as by four phosphorus atoms with W — P distances of 242, 250, 264, and 268 pm.[C3(C4H9)3]+[WCl5(C4H9C=CC4H9)] : Space group P21/c, Ζ = 4, 3284 observed unique reflexions, R = 0.052. Lattice dimensions at 20 °C: a = 941.5(3), b = 1762.2(6), c = 1903.5(7) pm, β = 92.27(3)°. The compound consists of tris(t-butyl)cyclopropenium ions, and anions [WCl5(C4H9C=CC4H9)]⁻, in which the bis(t-butyl)alkyne ligand is coordinated side-on, corresponding to a cyclopropene type structure with W—C distances of 198 pm.

Structural Characterization of Cationic 16-Electron Pentamethylcyclopentadienyl Ruthenium(II) Complexes Containing the Binuclear [Cp*Ru(μ-Cl)3RuCp*]– Anion

2008 ◽  
Vol 63 (10) ◽  
pp. 1155-1159 ◽  
Author(s):  
Thomas Glöge ◽  
Dejan Petrovic ◽  
Cristian G. Hrib ◽  
Peter G. Jones ◽  
Matthias Tamm
Keyword(s):  
Crystal Structures ◽  
Structural Characterization ◽  
Complex Salt ◽  
Monoclinic Space Group ◽  
Chlorine Atoms ◽  
Space Group ◽  
X Ray ◽  
Diimine Ligand ◽  
Half Sandwich

AbstractThe reaction of the diimine ligand 1,2-bis(1,3-diisopropyl-4,5-dimethylimidazolin-2-imino)ethane (BLiPr) with tetrameric [Cp*RuCl]4 in a 1 : 0.75 ratio afforded the complex salt [1][2] containing the 16-electron half-sandwich cation [Cp*Ru(BLiPr)]+ (1) and the dinuclear anion [Cp*Ru(μ- Cl)3RuCp*]− (2). The X-ray crystal structures of [1][2]·31/2THF (monoclinic, space group P21/n, Z = 4) and of [1][2]·THF (monoclinic, space group C2/m, Z = 4) are reported, allowing the structural characterization of the unprecedented anion 2, in which two [(η5-C5Me5)Ru(II)] moieties are bridged by three μ2-chlorine atoms.

Structural studies in the iron(III)/chloride/α,α'-diimine system. I. The six-coordinate mononuclear fac-[FeCl3(phen)X] system, X = MeOH, H2O, Cl-

1983 ◽  
Vol 36 (10) ◽  
pp. 2031 ◽  
Author(s):  
PC Healy ◽  
JM Patrick ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Iron Complexes ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Chlorine Atoms ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

The crystal structures of three iron complexes [FeCI3(phen)(MeOH)].MeOH (I), [FeCl3(phen)(H2O)] (2) and [phenH]+ [FeCl4(phen)]- (3) have been determined by single-crystal X-ray diffraction methods at 295(1) K, and refined by least squares to residuals of 0.044 (1600 'observed' reflections), 0.040 (806) and 0.050 (2496), respectively. Crystals of (1) are monoclinic, P21/c, a 8.005(9), b 14.805(11), c 14.830(12) A, P 101.03(7)°, Z 4; for (2), triclinic, space group P1 , a 10.591(8), b 10.227(7), c 6.613(3) Ǻ, α 108.21(5), β 100.69(5), γ 91.98(6)°2, 2 ; for (3), triclinic, P1, a 18.560(8), b 10.302(5), c 6.981(3) Ǻ, α 106.79(4), β 94.50(4), γ 103.15(4)°, Z 2. In all structures, the iron atoms are six-coordinate, with the disposition of the three chlorine atoms being fac in (1) and (2).

Synthese von [LRe(CO)3]+-Komplexen mit makrocyclischen Liganden Die Kristallstrukturen von 1,4,7-Triazacyclononan-tricarbonylrhenium( I)-thiocyanat und 1,4,7-Trithiacyclononan-tricarbonylrhenium( I) -bromid-hemihydrat / Synthesis of [LRe(CO)3]+ Complexes with Macrocyclic Ligands The Crystal Structures of 1,4,7-Triazacyclononane-tricarbonyl-rhenium(I) Thiocyanate and of 1,4,7-Trithiacyclononane-tricarbonyl-rhenium(I) Bromide Hemihydrate

1988 ◽  
Vol 43 (3) ◽  
pp. 299-305 ◽  
Author(s):  
Christa Pomp ◽  
Stefan Drüeke ◽  
Heinz-Josef Küppers ◽  
Karl Wieghardt
Keyword(s):  
Crystal Structures ◽  
Macrocyclic Ligands ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cyclic Amines ◽  
Yellow Orange

The tridentate macrocyclic ligands 1,4,7-triazacyclononane, its thia analogue 1,4,7-trithiacyclononane, 1-oxa-4,7-diazacyclononane, and N,N′,N″-trimethyl-1 ,4,7-triazacyclononane react with Re(CO)5Br in dimethylformamide to yield colorless, air-stable [LRe(CO)3]Br complexes (L = tridentate macrocycle). With Mn(CO)5Br only the cyclic amines react to afford yellow-orange [LMn(CO)3]Br complexes whereas 1,4,7-trithiacyclononane does not give stable complexes of manganese. The crystal structures of [([9]aneN3)Re(CO)3](NCS) and [([9]aneS3)Re(CO)3]Br · 1/2 H2O have been determined. The former crystallizes in the orthorhombic space group P bca (a = 12/763(4), b = 12.662(5), c = 17.472(9) Å; Z = 8); whereas the latter crystallizes in the monoclinic space group P21/c (a = 9.444(1). b = 11.797(2), c = 28.095(3) Å. β = 90,86(1); Z = 8).

scholarly journals Metallkomplexe mit Cyanoguanidin als Liganden: Kristallstrukturen von [Cd(cnge)2F2]·3H2O , Cd(cnge)2Br2 und Hg(cnge)Cl2 (enge = C yanoguanidin) / Metal Complexes with Cyanoguanidine as Ligand: Crystal Structures of [Cd(cnge)2F2]·3H2O, Cd(cnge)2Br2 and Hg(cnge)Cl2 (cnge = Cyanoguanidine)

1996 ◽  
Vol 51 (12) ◽  
pp. 1701-1706 ◽  
Author(s):  
Joachim Pickardt ◽  
Britta Kühn
Keyword(s):  
Metal Complexes ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Bridging Ligands ◽  
Chlorine Atoms ◽  
Triclinic Space Group ◽  
Space Group ◽  
Halogen Atoms

Crystals of [Cd(cnge)2F2]·3H2O (1), Cd(cnge)2Br2 (2) and Hg(cnge)Cl2 (3) (cnge = cyanoguanidine) were obtained by crystallisation from solutions of CdF2, CdBr2 or HgCl2 and cyanoguanidine in water/ethanol or methanol. 1 crystallizes monoclinically, space group C2, Z = 2,a = 1629.2(4), b = 1056.6(4), c = 353.9( 1) pm, β = 101.05(2)°; 2 is monoclinic, space group P21/n, Z = 2, a = 391.9(1), b = 850.7(2), c = 1722.1(4) pm, β = 94.06(2)°, 3 is triclinic, space group P1, Z = 1, a = 686.7( 1), b = 693.0(5), c = 387.2(4) pm, α = 94.45(5)°, β = 95.05(4)°, γ = 78.58(5)°. In 1 and 2 each Cd atom is bonded to four halogen atoms to form polymeric (CdF2)n and (CdBr2)n chains, resp., and to two cyanoguanidine molecules. In 3 each Hg atom is bonded to four chlorine atoms also forming (HgCl2)n chains, which are connected via cyanoguanidine molecules acting as a bidentate bridging ligands to form a network.

Amidinatokomplexe von Bor, Aluminium, Gallium, Indium und Zinn Die Kristallstrukturen von Ph-C(NSiMe3)2AICI2 und Ph-C(NSiMe3)2SnCl3 / Amidinato Complexes of Boron, Aluminium, Gallium, Indium, and Tin The Crystal Structures of Ph-C(NSiMe3)2AlCl2 and Ph-C(NSiMe3)2SnCl3

1988 ◽  
Vol 43 (12) ◽  
pp. 1621-1627 ◽  
Author(s):  
Christina Ergezinger ◽  
Frank Weller ◽  
Kurt Dehnicke
Keyword(s):  
Ir Spectra ◽  
Bond Length ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Aluminium Atom ◽  
Chlorine Atoms ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Boron Tribromide

Abstract The trichlorides of aluminium, gallium, and indium, as well as boron tribromide and tin tetra-chloride react with N,N,N'-tris(trimethylsilyl)benzamidine to form the monomeric N.N'-bis-(trimethylsilyl)benzamidinato complexes Ph-C(NSiMe3)2MX2(M = B, Al. Ga, In; X = Cl, Br) and Ph -C(NSiMe3)2SnCl3 , respectively. All compounds have been characterized by their IR spectra, two of them by X-ray diffraction studies. Ph - C(NSiMei)2AlCl2 : Space group C2/c, Z = 4, 1152 independent observed reflexions, R = 0.052. Lattice dimensions (19 °C): a = 1558.6(1), b = 1116.6(1), c = 1307.0(1) pm, β = 115.17(1)°. The compound forms monomeric molecules, in which the aluminium atom is tetra-hedrally coordinated by two chlorine atoms and by the two nitrogen atoms of the benzamidinato chelate. Bond length A1N = 188.2 pm. Ph - C(NSiMe3)2SnCU: Space group P1̄, Z = 2, 3293 independent observed reflexions, R = 0.034. Lattice dimensions (19 °C): a = 980.1(1), b = 1025.9(1), c = 1230.5(2) pm. a = 68.40(1)°, β = 87.71(1)°, y - 68.92(1)°. The compound forms monomeric molecules, in which the tin atom is five-coordinated by three chlorine atoms and by the two nitrogen atoms of the benzamidinato chelate. Bond lengths SnN = 213.5 and 215.2 pm.

scholarly journals Die Kristallstrukturen von (PPh4)2[TiCl3(NSiMe3)]2 • CH3CN und (PPh4)2[TiCl4(OSPCl2)]2 / The Crystal Structures of (PPh4)2[TiCl3(NSiMe3)]2 · CH3CN and (PPh4)2[TiCl4(OSPCl2)]2

1992 ◽  
Vol 47 (10) ◽  
pp. 1386-1392 ◽  
Author(s):  
René Wollert ◽  
Sigrid Wocadlo ◽  
Kurt Dehnicke ◽  
Helmut Goesmann ◽  
Dieter Fenske
Keyword(s):  
Oxygen Atom ◽  
Crystal Structures ◽  
Titanium Tetrachloride ◽  
Unit Cell ◽  
Acetonitrile Solution ◽  
Formula Unit ◽  
Chlorine Atoms ◽  
Triclinic Space Group ◽  
Space Group

(PPh4)2[TiCl3(NSiMe3)]2 · CH3CN has been prepared from [TiCl2NSiMe3)]∞ with PPh4Cl in acetonitrile solution as yellow crystals. The compound crystallizes in the triclinic space group P T with one formula unit per unit cell, 3447 observed unique reflections, R = 0.053. Lattice dimensions at 200 K: a = 1030(1), b = 1253(1), c = 1374(1) pm, α = 77.46(8)°, β = 73.93(8)°, γ = 69.99(9)°. The structure consists of PPh4+ ions and centrosymmetric dimeric anions [TiCl3(NSiMe3)]22-, in which pentacoordinate titanium atoms are associated via the nitrogen atoms of the silylimido groups.(PPh4)2[TiCl4(OSPCl2)]2 has been prepared by the reaction of PPh [OSPCl2] with titanium tetrachloride in CH2C12 solution as orange crystals. (Space group P1̄, Ζ = 1, 3242 observed unique reflections, R = 0.033). Lattice dimensions at 193 K: a = 1114.8(2), b = 1190.6(2), c = 1218.7(2) pm, α = 72.18(1)°, β = 85.45(1)°, γ = 69.19(1)°. The structure consists of PPh4+ ions and centrosymmetric dimeric anions [TiCl4(OSPCl2)]22-, in which hexacoordinate titanium atoms are associated via two chlorine atoms. The OSPCl2- group is coordinated via the oxygen atom.

scholarly journals Crystal-to-Crystal Transformation from K2[Co(C2O4)2(H2O)2]·4H2O to K2[Co(μ-C2O4)(C2O4)]

2021 ◽  
Vol 7 (6) ◽  
pp. 77
Author(s):  
Bin Zhang ◽  
Yan Zhang ◽  
Guangcai Chang ◽  
Zheming Wang ◽  
Daoben Zhu
Keyword(s):  
Hydrogen Bond ◽  
Physical Properties ◽  
Crystal Structures ◽  
Molecular Crystal ◽  
Trigonal Prism ◽  
Space Group ◽  
Cell Parameters ◽  
Oxalate Anion ◽  
Crystal Transformation ◽  
Antiferromagnetic Ordering

Crystal-to-crystal transformation is a path to obtain crystals with different crystal structures and physical properties. K2[Co(C2O4)2(H2O)2]·4H2O (1) is obtained from K2C2O4·2H2O, CoCl2·6H2O in H2O with a yield of 60%. It is crystallized in the triclinic with space group P1 and cell parameters: a = 7.684(1) Å, b = 9.011(1) Å, c = 10.874(1) Å, α = 72.151(2)°, β = 70.278(2)°, γ = 80.430(2)°, V = 670.0(1) Å3, Z = 2 at 100 K. 1 is composed of K+, mononuclear anion [Co(C2O4)2(H2O)22−] and H2O. Co2+ is coordinated by two bidentated oxalate anion and two H2O in an octahedron environment. There is a hydrogen bond between mononuclear anion [Co(C2O4)2(H2O)22−] and H2O. K2[Co(μ-C2O4)(C2O4)] (2) is obtained from 1 by dehydration. The cell parameters of 2 are a = 8.460(5) Å, b = 6.906 (4) Å, c = 14.657(8) Å, β = 93.11(1)°, V = 855.0(8) Å3 at 100 K, with space group in P2/c. It is composed of K+ and zigzag [Co(μ-C2O4)(C2O42−]n chain. Co2+ is coordinated by two bisbendentate oxalate and one bidentated oxalate anion in trigonal-prism. 1 is an antiferromagnetic molecular crystal. The antiferromagnetic ordering at 8.2 K is observed in 2.

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