Die Kristallstrukturen von [MoCl2(NO)2(OPEt3)]2, [MoCl3(NO)(OPPh3)2•MoCl4(OPPh3)2], [MoCl2(NO)(PPh3)2(CH3CN)] und [MoCl4(NPPh3)(OPPh3)] / The Crystal Structures of [MoCl2(NO)2(OPEt3)]2, [MoCl3(NO)(OPPh3)2 • MoCl4(OPPh3)2], [MoCl2(NO)(PPh3)2(CH3CN)], and [MoCl4(NPPh3)(OPPh3)]

1995 ◽  
Vol 50 (1) ◽  
pp. 1-10 ◽  
Author(s):  
Gunnar Philipp ◽  
Sigrid Wocadlo ◽  
Werner Massa ◽  
Kurt Dehnicke ◽  
Dieter Fenske ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Trans Position ◽  
Nitrosyl Complex ◽  
Centrosymmetric Dimer ◽  
Acetonitrile Molecule ◽  
Space Group ◽  
Structure Determinations ◽  
In Trans ◽  
Complex Forms

The title compounds have been prepared by reactions of MoCl2(NO)2 with PPh3, OPPh3, or Me3SiNPR3 (R = Et, Ph) in dichloromethane and acetonitrile suspension, respectively. All complexes were characterized by IR spectroscopy and by crystal structure determinations. [MoCl2(NO)2(OPEt3)]2: Space group C2/c, Z = 4, 2950 observed unique reflections, R = 0.029. Lattice dimensions at —70 °C: a = 2390.5(11), b = 875.5(5), c = 1399.1(6) pm, β = 113.18(2)°. The complex forms a centrosymmetric dimer with MoCl2Mo bridges, the nitrosyl groups being in a cis-arrangement. The OPEt3 ligand is coordinated in trans position to one of the nitrosyl ligands.[MoCl3(NO)(OPPh3)2 • MoCl4(OPPh3)2]: Space group P21/c, Z = 4, 10243 observed unique reflections, R = 0.060. Lattice dimensions at —60 °C: a = 1900.4(3), b = 1689.1(5), c = 2209.3(7) pm, β = 95.92(2)°. The structure consists of the two independent complexes [MoCl3(NO)(OPPh3)2] and [MoCl4(OPPh3)2]. In both complexes the OPPh3 groups are in a cis-arrangement at the octahedrally coordinated Mo atoms; in the nitrosyl complex one of the OPPh3 molecules is in trans-position to the nitrosyl ligand.[MoCl2(NO)(PPh3)2(CH3CN)]: Space group P21/n, Z = 4, 5107 observed unique reflections, R = 0.028. Lattice dimensions at 20 °C: a = 1006.5(2), b = 1527.2(2), c = 2342.3(2) pm, β = 90.97(1)°. The PPh3 molecules are in trans-positions to one another at the octahedrally coordinated Mo atom, whereas the acetonitrile molecule is in trans-position to the nitrosyl ligand.[MoCl4(NPPh3)(OPPhi)]: Space group P21, Z = 2, 3323 observed unique reflections, R = 0.057. Lattice dimensions at —70 °C: a = 985.7(8), b = 1471.2(9), c = 1215.9(11) pm, β = 100.50(3)°. The OPPh3 molecule coordinates in trans-position to the phosphorane iminato ligand at the octahedrally coordinated Mo atom.

Synthese und Kristallstrukturen der Wolfram(VI)-Alkinkomplexe [WCl4(Ph - C≡C - I)(THF)] und [WCl4(Ph-C≡C-Te-C4H9)(THF)] / Synthesis and Crystal Structures of the Tungsten(VI) Alkyne Complexes [WCl4(Ph-C≡C-I)(THF)] and [WCl4(Ph-C≡C-Te-C4H9)(THF)]

1993 ◽  
Vol 48 (8) ◽  
pp. 1105-1111 ◽  
Author(s):  
Michael Plate ◽  
Peter Hofacker ◽  
Werner Massa ◽  
Birgit Schwarz ◽  
Bernhard Neumüller ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Oxygen Atom ◽  
Crystal Structures ◽  
Molecular Structures ◽  
Trans Position ◽  
Space Group ◽  
Structure Determinations ◽  
In Trans ◽  
Alkyne Complexes

[WCl4(Ph-C≡C-I)(THF)] has been prepared by the reaction of trans-[WCl4(SEt2)2] with Ph - C≡C - I in THF solution, whereas [WCl4(Ph-C≡C-Te-nC4H9)(THF)] has been synthesized by the reaction of Ph-C≡C-Te-nC4H9 with tungsten hexacloride in the presence of C2Cl4 and THF. Both complexes were characterized by IR spectroscopy and by crystal structure determinations.[WCl4(Ph-C≡C-I)(THF)]: Space group P21/c, Z = 4, 2617 observed unique reflections, R = 0.064. Lattice dimensions at –70°C: a = 1518.2(3), b = 714.5(1), c = 1540.0(3) pm, β = 90.09(3)°.[WCl4(Ph-C≡C-Te–nC4H9)(THF)]. Space group P1̄, Z = 2, 3911 observed unique reflections, R = 0.067. Lattice dimensions at 20°C: a = 844.0(3), b = 974.6(4), c = 1002.4(3) pm, α = 76.00(4), β= 105.14(1), γ = 82.03(3)°.Both complexes have molecular structures, in which the tungsten atoms are seven-coordi-nate by four chlorine ligands, by the two alkyne carbon atoms, and in trans position to the latter by the oxygen atom of the THF molecule. The WC bond lengths are 198 and 200(1) in the telluro complex and 206 and 196(1) pm in the iodine derivative.

μ2-Halogenokomplexe von N-Bromsuccinimid und N-Bromphthalimid. Die Kristallstrukturen von PPh4[X(N-Bromsuccinimid)2] und von PPh4[X(N-Bromphthalimid)2] mit X = CI und Br / μ2-Halogeno Complexes of N-Bromosuccinimide and N-Bromophthalimide. The Crystal Structures of PPh4 [X(N-Bromosuccinimide)2] and PPh4 [X(N-Brom ophthalimide)2] with X = Cl and Br

1994 ◽  
Vol 49 (5) ◽  
pp. 593-601 ◽  
Author(s):  
Mitra Ghassemzadeh ◽  
Klaus Harms ◽  
Kurt Dehnicke ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Crystal Structures ◽  
Yellow Crystal ◽  
Halide Ions ◽  
Space Group ◽  
Bond Angles ◽  
Structure Solution ◽  
Structure Determinations ◽  
Acetonitrile Solutions

The μ2-halogeno complexes PPh4[X(N-bromosuccinimide)2] and PPh4[X(N-bromophthali- mide)2] with X = Cl and Br have been prepared by reactions of N-bromosuccinimide and N-bromophthalimide, respectively, with the corresponding tetraphenylphosphonium halides PPh4X in acetonitrile solutions. The compounds form pale yellow crystal needles, which were characterized by IR spectroscopy and by crystal structure determinations. PPh4[Cl(N-Bromosuccinimide)2] (1): Space group P21/n, Z = 4, structure solution with 2516 observed unique reflections, R = 0.040. Lattice dimensions at -25 °C: a = 1775.9(1), b = 764.3(1), c = 2341.7(2) pm, β = 101.84(1)°. PPh4[Br(N-Bromosuccinimide)2] (2): Space group P21/n, Z = 4, structure solution with 5620 observed unique reflections, R = 0.061. Lattice dimensions at 20 °C: a = 1776.9(9), b = 762.2(3), c = 2331(1) pm, β = 103.02(3)°. PPh4[Cl(N-Bromophthalimide)2] (3): Space group P1̅, Z = 4, structure solution with 3812 observed unique reflections, R = 0.039. Lattice dimensions at -50 °C: a = 918.5(2), b = 1115.0(3), c = 2584.4(5) pm, α = 88.22(3)°, β = 83.20(3)°, γ = 85.10(3)°. PPh4[Br(N-Bromophthalimide)2] (4): Space group P1̅, Z = 2, structure solution with 3413 observed unique reflections, R = 0.044. Lattice dimensions at -50 °C: a = 1120.2(2), b = 1308.6(3), c = 1343.2(3) pm, α = 105.10(3)°, β = 104.16(3)°, γ = 92.99(3)°. The structures of 1-4 consist of PPh4+ ions, anions [X(N-bromosuccinimide)2]- and [X(N-bromophthalimide)2]-, respectively, in which the halide ions X- are coordinated by the bromine atoms of N-bromosuccinimide and N-bromophthalimide molecules, respectively. The bond angles Br···X···Br are 86.48(5)° for 1, 85.1(1)° for 2, 102.31(6)° and 93.61(6)° for 3, and 91.86(4)° for 4. The bond angles N-Br···X are nearly linear.

μ2-Halogenokomplexe von N-Iodsuccinimid. Die Kristallstrukturen von PPh4[X(N-Iodsuccinimid)2] · CH3CN mit X = Cl, Br, / μ2-Halogeno Complexes of N-Iodosuccinimide. The Crystal Structures of PPh4[X(N-Iodosuccinimide)2] · CH3CN with X = Cl, Br, I

1994 ◽  
Vol 49 (5) ◽  
pp. 602-608 ◽  
Author(s):  
Mitra Ghassemzadeh ◽  
Kurt Dehnicke ◽  
Helmut Goesmann ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Crystal Structures ◽  
Yellow Crystal ◽  
Halide Ions ◽  
Space Group ◽  
Bond Angles ◽  
Pale Yellow ◽  
Structure Determinations ◽  
Acetonitrile Solutions

The μ2-halogeno complexes PPh4[X(N-Iodosuccinimide)2] · CH3CN with X = CL Br, I have been prepared by reactions of N-Iodosuccinimide with the corresponding tetraphenylphos- phonium halides PPh4X in acetonitrile solutions. The compounds form pale yellow crystal needles, which were characterized by IR spectroscopy and by crystal structure determinations. PPh4[Cl(N-Iodosuccinimide)2] · CH3CN (1): Space group Pna21, Z = 4, 4461 observed unique reflections. R = 0.027. Lattice dimensions at -60 °C: a = 1840.5(9), b = 2589(1), c = 728.2(4) pm. PPh4[Br(N-Iodosuccinimide)2] · CH3CN (2): Space group Pna21 Z = 4, 4284 observed unique reflections, R = 0.034. Lattice dimensions at -70 °C: a = 724.8(4), b = 1838.6(9), c = 2601(1) pm. PPh4[I(N-Iodosuccinimide)2] · CH3CN (3): Space group Pna21, Z = 4, 5775 observed unique reflections. R = 0.031. Lattice dimensions at -60 °C: a = 1849.2(9). b = 2644(1), c = 730.3(4) pm. 1-3 are isotypical. There structures consist of PPh4+ ions, including acetonitrile molecules without bonding interactions, and anions [X(iodosuccinimide)2]-, in which the halide ions X- are coordinated bv the iodine atoms of the N-iodosuccinimide molecules. The bond angles I··· X···I range from 90.13(4)° (X = Cl) and 88.84(3)° (X = Br) to 87.83(3)° (X = I). The bond angles N- I ··· X are nearly linear.

Substitutionsreaktionen an der N-Chlornitrenogruppe des [WCl4(NCl)]2. Die Kristallstrukturen von [CH3CN—WCl4(NSMe)] und [WNCl3 · NC—CH3]4 / Substitution Reactions at the N-Chloronitreno Group of [WCl4(NCl)]2. The Crystal Structures of [CH3CN—WCl4(NSMe)] and [WNCl3 · NC—CH3]4

1989 ◽  
Vol 44 (8) ◽  
pp. 903-910 ◽  
Author(s):  
Astrid Görge ◽  
Ute Patt-Siebel ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Trans Position ◽  
Crystal Data ◽  
Substitution Reactions ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations

[WCl4(NCl)]2 reacts in acetonitrile with the trimethylsilyl compounds Me3SiSR (R = Me, Ph), and Me3SiESiMe3 (E = S, Se), with substitution of the chlorine atom of the N-chloronitreno group W=N–Cl and formation of CH3CN–WCl4(NSR) and CH3CN–WCl4(NEN)WCl4–NCCH3, respectively. Excess Me3SiBr reacts with CH3CN–WCl4(NSMe) to afford CH3CN–WBr4(NSMe). [CH3CN–WNCl3]4 was obtained from CH3CN–WCl4(NCl) and N(SiMe3)3. The products were characterized by their IR spectra. Two X-ray crystal structure determinations were also carried out. CH3CN—WCl4(NSMe) forms twinned crystals, and only non-overlapping reflexions of one of the twin individuals were used for the structure determination (846 unique values, R = 0.055). Crystal data: a = 592.4(2), b = 758.8(2), c = 1203.7(8) pm, β = 95.06(4)°, monoclinic, space group P21/m, Z = 2. The compound is a monomer in which the acetonitrile ligand is situated in the trans position to the W≡N–S̱̅–Me group. The bond lengths (W≡N 174(2), N–S 161(2) pm) and bond angles (WNS 176(1), NSC 102.1(9)°) are in agreement with the proposed formula. Crystal data for [CH3CN–WNCl3]4: a = 1009.5(2), b = 1274.5(2), c = 1287.9(2) pm, β = 108.17(1)°, monoclinic, space group P21/c, Z = 2 (2113 unique reflexions, R = 0.057). The compound forms tetrameric units, in which the W atoms form a square and are linked with one another via N atoms at alternating distances (W=N 171(2), W–N 207(2), W–NCMe 238(2) pm).

Ionische Phosphaniminato-Komplexe von Schwefel(IV) und Selen(IV ). Die Kristallstrukturen von [S(NPMe3)3]Cl · CH2Cl2, [S(N PPh3)3]S4N5 und [Se(NPMe3)3]Cl · C7H8 / Ionic Phosphorane Iminato Complexes of Sulfur(IV) and Selenium(IV). Crystal Structures of [S(NPMe3)3]Cl ·CH2Cl2, [S(NPPh3)3]S4N5 and [Se(NPMe3)3]Cl · C7H8

1995 ◽  
Vol 50 (10) ◽  
pp. 1455-1463 ◽  
Author(s):  
Frank Kunkel ◽  
Hella Folkerts ◽  
Sigrid Wocadlo ◽  
Hak-Chul Kang ◽  
Werner Massa ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Crystal Structures ◽  
Acetonitrile Solution ◽  
Formula Unit ◽  
Selenium Compound ◽  
Space Group ◽  
Sulfur Dichloride ◽  
Structure Determinations ◽  
Moisture Sensitive

[S(NPMe3)3]Cl · CH2C12 and [S(NPPh3)3]S4N5 were prepared by the reaction of Me3SiNPMe3 or Me3SiNPPh3 with sulfur dichloride and S3N2Cl2, respectively, in CH2Cl2 solutions as colourless, moisture sensitive crystals. The corresponding selenium compound was prepared from SeCl4 and Me3SiNPMe3 in acetonitrile solution; it crystallizes from toluene solutions with one mole of toluene per formula unit. All complexes have been characterized by IR spectroscopy and by crystal structure determinations.[S(NPMe3)3]Cl-CH2Cl2: Space group Pna21, Z = 8 , 3930 observed unique reflections, R = 0.033. Lattice dimensions at -120 °C: a = 1200.9(1), b = 1020.2(1), c = 1790.5(1) pm.[S(NPPh3)3]S4N5: Space group P63, Z = 2, 2586 observed unique reflections, R = 0.054. Lattice dimensions at -100 °C: a = b = 1334.7(2), c = 1652.6(2) pm.[Se(NPMe3)3]Cl · C7H8: Space group C2/c, Z = 8 , 1475 observed unique reflections, R = 0.059. Lattice dimensions at -40 °C: a = 1853.6(8), b = 1159.2(4), c = 2053.2(4) pm. β = 101.92(3)°.All compounds contain cations [E(NPR3)3]+ (E = S, Se) with pyramidal structures. Bond lengths and bond angles are in average: S-N 162.5 pm, S-N-P 120.5° (R = Me), S-N 161.8 pm, S-N-P 119.2° (R = Ph), Se-N 177.8 pm, Se-N-P 120.3°.

Oxotetrafluoro-vanadate(V): Die Kristallstruktur von [enH2] [VOF4(H2O)]2.

1976 ◽  
Vol 31 (5) ◽  
pp. 541-543 ◽  
Author(s):  
Helmut Rieskamp ◽  
Rainer Mattes
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Trans Position ◽  
Space Group ◽  
X Ray ◽  
In Trans ◽  
Oxygen Atoms

The crystal structure of [enH2][VOF4(H2O)]2 has been determined from X-ray diffractometer data. Crystals are monoclinic, space group C2/c with Z = 4 in a unit cell of dimensions a = 16.576(13), b = 7.781(4), c = 10.338(8) Å, β = 120.0(1)°.The structure was refined by least-squares methods to R 0.053 for 1436 reflections. The structure contains monomeric [VOF4(H2O)]⁻-ions with the oxygen atoms in trans position. The bond distances are 1.577 Å (terminal oxygen) and 2.333 Å (H2O molecule), resp. The V–F distances vary between 1.769(2) and 1.858(2) Å for fluorine atoms involved in strong hydrogen bonds.

Synthese und Kristallstruktur des Imidokomplexes {TaCl4NC(Ph)[N(SiMe3)2]}2 · 2 CH2Cl2 / Synthesis and Crystal Structure of the Imido Complex {TaCl4NC(Ph)[N(SiMe3)2]}2 · 2 CH2Cl2

1989 ◽  
Vol 44 (9) ◽  
pp. 1003-1006 ◽  
Author(s):  
Kurt Merzweiler ◽  
Dieter Fenske ◽  
Eva Hartmann ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Title Compound ◽  
Bond Angle ◽  
Trans Position ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Bond Lengths ◽  
In Trans ◽  
Complex Forms

The title compound has been prepared by the reaction of N,N,N′-tris(trimethylsilyl)benzamidine with tantalum pentachloride in CH2Cl2 suspension, forming amber-coloured, moisturesensitive crystals, which were characterized by an X-ray structure determination. Space group P 21/n, Z = 2, 4895 observed independent reflexions, R = 0.059. Lattice dimensions (-65°C): a = 1165.2(6), b = 1335.4(6), c = 1629.0(7) pm, β = 93.23(4)°. The complex forms centrosymmetric molecules dimerized via chloro bridges TaCl2Ta with TaCl bond lengths of 247.2(2) and 277.1(2) pm, the longer one being in trans-position to the imido group, which can be formulatedas [xxx] (bond lengths Ta=Ν = 183.5(8), C=N = 134(1) pm, bond angle TaNC = 162.7(7)°).

Synthese und Kristallstruktur des Amido-Palladats (PPh4)2[Pd2Cl4(NH2)2] · CH2Cl2 und des Benzamidin-Palladats PPh4{ [Ph– C(NH2)(NH)]PdCl3} · CH3CN / Synthesis and Crystal Structure of the Amido Palladate (PPh4)2[Pd2Cl4(NH2)2] · CH2Cl2 and of the Benzamidine Palladate PPh4{[Ph—C(NH2)(NH)]PdCl3} · CH3CN

1991 ◽  
Vol 46 (8) ◽  
pp. 992-998 ◽  
Author(s):  
Henning von Arnim ◽  
Werner Massa ◽  
Alfred Zinn ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Ir Spectroscopy ◽  
Acetonitrile Solution ◽  
Chlorine Atoms ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations ◽  
Hcl Gas

Orange crystals of (PPh4)2[Pd2Cl4(NH2)2] have been prepared by the reaction of (PPh4)2[Pd2Cl6] with N,N,N′-tris(trimethylsilyl)benzamidine in boiling acetonitrile in the presence of water, and orange brown crystals of PPh4{[Ph—C(NH2)(NH)]PdCl3} by the reaction of the amidinato complex PPh4[Ph—C(NSiMe3)2PdCl2] with HCl gas in acetonitrile solution. The complexes were characterized by IR spectroscopy as well as by X-ray structure determinations.(PPh4)2[Pd2Cl4(NH2)2] · CH2Cl2: Space group PĪ, Z = 1, 2784 observed unique reflections, R = 0.043. Lattice dimensions at —60 °C: a = 1053.3(4), b = 1081.1(4), c = 1249.2(4) pm, α = 102.90(2)°, β = 110.44(2)°, γ = 102.23(2)°. The compound consists of PPh4+ ions and centrosymmetric anions [Pd2Cl4(NH2)2]2- with bridging chlorine atoms and terminal amido groups.PPh4{[Ph—C(NH2)(NH)]PdCl3} -CH3CN: Space group C2/c, Z = 8, 1183 observed unique reflections, R = 0.033. Lattice dimensions at —60 °C: a = 3106.7(6), b = 1059.0(1), c = 1818.0(4) pm, β = 90.98(2)°. The compound consists of PPh4+ ions, [Ph—C(NH2)(NH)PdCl3]-ions, and included CH3CN molecules. In the anion the benzamidine ligand is bound via the nitrogen atom of the imido group.

N,N′-Dim ethylharnstoff als chelatisierende Lewis-Säure: Synthese und Kristallstrukturen von PPh4[Cl(H2Me2N2CO)] und (PPh4)2[Cl(H2Me2N2CO)]Cl / N.N′-Dimethylurea as a Chelating Lewis Acid: Synthesis and Crystal Structures of PPh4[Cl(H2Me2N2CO)] and (PPh4)2[Cl(H2Me2N2CO)]Cl

1996 ◽  
Vol 51 (10) ◽  
pp. 1423-1427
Author(s):  
Mitra Ghassemzadeh ◽  
Klaus Harms ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Lewis Acid ◽  
Acid Synthesis ◽  
Space Group ◽  
Molar Ratios ◽  
Tetraphenylphosphonium Chloride ◽  
Structure Determinations

The title compounds have been prepared from tetraphenylphosphonium chloride and N,N′- dimethylurea in acetonitrile using different molar ratios of the educts. Both compounds were characterized by IR spectroscopy and by crystal structure determinations. PPh4[Cl(H2,Me2,N2,CO)]: Space group P1̅, Z = 4 ,a = 1021.8(2), b = 1192.7(2), c = 2143.9(4) pm, α = 87.21(3)°, β = 85.95(3)°, γ = 74.16(3)° (-50°C). (PPh4)2[Cl(H2Me2N2CO)]Cl: Space group P21/n, Z = 4, a = 1138.4(2), b = 2855.4(3), c = 1394.0(1) pm, β = 91.19(10)° (-60°C). In both compounds the N.N′-dimethylurea molecule acts as a chelating Lewis acid via two Cl···H hydrogen bonds forming nearly planar ClH2N2C-six-membered heterocycles.

Synthese und Kristallstruktur von PPh4[ReF2Cl2(N2S2)] / Synthesis and Crystal Structure of PPh4[ReF2Cl2(N2S2)]

1989 ◽  
Vol 44 (12) ◽  
pp. 1509-1512 ◽  
Author(s):  
Stefan Vogler ◽  
Kurt Dehnicke ◽  
Wolfgang Hiller
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Sodium Fluoride ◽  
Structure Determination ◽  
Membered Ring ◽  
Trans Position ◽  
Rhenium Atom ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
In Trans

PPh4[ReF2Cl2(N2S2)] has been prepared by the reaction of PPh4[ReCl4(NSCl)2] · CH2Cl2 with sodium fluoride in acetonitrile suspension. The compound forms black crystals, which were characterized by IR spectroscopy as well as by an X-ray structure determination.Space group P21/c, Z = 4, 2525 observed unique reflexions, R = 0.053. Lattice dimensions at 20°C: a = 1277.4(3), b = 713.2(3), c = 2860.8(4) pm. β = 97.20(3)°. The compound consists of PPh4+ and [ReF2Cl2(N2S2)]- ions, in which the rhenium atom is surrounded octahedrally by two fluorine atoms, two chlorine atoms, and by the nitrogen atoms of a ReN2S2 five-membered ring, the fluorine ligands being in trans position to the N atoms. The bond lengths ReN (172; 177 pm) and NS (155; 160 pm) are in the range of double bonds, the S—S bond is relatively long (243 pm).

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