Die Kristallstrukturen der Palladium(II)-Komplexe [Pd(CH3CN)4](BF4)2, [PdCl(μ2 -PPh2)(HPPh2)]2 · CH2Cl2 und [PdCl(HPPh2) {H(OPPh2)2}] / The Crystal Structures of the Palladium(II) Complexes [Pd(CH3CN)4](BF4)2, [PdCl(μ2-PPh2)(HPPh2)] · CH2Cl2, and [PdCl(HPPh2){H(OPPh2)2}]

1992 ◽  
Vol 47 (11) ◽  
pp. 1505-1512 ◽  
Author(s):  
Thorsten Gebauer ◽  
Gerlinde Frenzen ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structures ◽  
Phosphorus Atom ◽  
Palladium Atom ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Bond Lengths ◽  
Group Type ◽  
Polymorphic Forms ◽  
Ray Methods

The crystal structures of the title compounds were solved by X-ray methods.[Pd(CH3CN)4](BF4)2: Space group Pbca, Z = 4,812 observed unique reflections, R = 0.057, wR = 0.033. Lattice dimensions at -80 °C: α = 1027.5(5), b = 1242.8(6), c = 1280.3(6) pm. The compound consists of planar [Pd(CH3CN)4]2+ ions with Pd-N bond lengths of 195.6 pm and BF4- anions.[PdCl(μ2-PPh2(HPPh2)]2 • CH2Cl2 crystallizes in two polymorphic forms in the same space group type but with different cell parameters, which depends on the conditions of the synthesis. α-form: Space group P21/c, Z = 4, 4680 observed unique reflections, R = 0.041, wR = 0.033. Lattice dimensions at -80 °C: a = 937.2(2), b = 1750.3(6), c = 1593.9(5) pm, β = 106.32(2)°. β-form: Space group Ρ21/n, Ζ = 4, 2519 observed unique reflections, R = 0.105, wR = 0.067. Lattice dimensions at -80 °C: a = 1118.0(4), b = 1222.4(3), c = 1849.9(4) pm, β = 90.72(2)°. Both polymorphs contain centrosymmetric molecules [PdCl μ2- PPh2)(HPPh2)]2 with Pd-P bond lengths of 226.6 pm for the bridging PPh2 groups and Pd-P bond lengths of 232.2 pm for the terminal HPPh2 ligands.[PdCl(HPPh2){H(OPPh2)2}]: Space group Pbca, Z = 8,3673 observed unique reflections, R = 0.038, wR = 0.032. Lattice dimensions at -80 °C: a = 1736.6(3), b = 1874.4(4), c = 1983.1(4) pm. The palladium atom has planar coordination consisting of the chlorine atom, the phosphorus atom of the HPPh2 ligand (Pd-P bond length 235.5 pm), and by the two phosphorus atoms of the H(OPPh2)2 chelate (Pd-P bond lengths 225.9 and 231.0 pm).

Die Kristallstrukturen von Ph3PNPh, [Ph3PN(H)Ph][AuI2] und von 2,3-Bis(triphenylphosphoranimino)maleinsäure-N-methylimid / The Crystal Structures of Ph3PNPh, [Ph3PN(H)Ph][AuI2] and of 2,3-Bis(triphenylphosphoranimino)maleic Acid-N-methylimide

1988 ◽  
Vol 43 (2) ◽  
pp. 138-148 ◽  
Author(s):  
Eberhard Böhm ◽  
Kurt Dehnicke ◽  
Johannes Beck ◽  
Wolfgang Hiller ◽  
Joachim Strähle ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Maleic Acid ◽  
Staudinger Reaction ◽  
Space Group ◽  
X Ray ◽  
Bond Angles ◽  
Bond Lengths ◽  
Structure Determinations ◽  
Ray Methods

[Ph3PN(H)Ph][AuI2] (2) is formed by the reaction of AuI with N-Phenyl-iminotriphenylphosphorane, Ph3PNPh in a toluene suspension. 2,3-Bis(triphenylphosphinimino)maleic acid-N-methylimide (3) has been prepared by the Staudinger reaction of 2,3-bis(azido)maleic acid-N-methylimide with PPh3 in THF solution in the form of red crystals. Crystal structure determinations of three iminophosphoranes were carried out by X-ray methods.Ph3PNPh (1): space group P21/c, Z = 4, 2176 independent observed reflexions, R = 0.057. Lattice dimensions (-30 °C): a = 1126.4, b = 1148.6, c = 1476.0 pm; β = 97.21°. The compound forms monomeric molecules with P=N = 160.2 pm and an PNC angle of 130.4°.[Ph3PN(H)Ph][AuI2] (2): space group P1̄, Z = 2, 1780 independent observed reflexions, R = 0.057. Lattice dimensions (18 °C); a = 824.9, b = 1022, c = 1476.2 pm; α = 89.23°, β = 87.41°, γ = 85.65°. The compound consists of ions [Ph3PN(H)Ph]⊕ with P=N = 162.4 pm and PNC = 129.3°, and anions [AuI2]⊖ with Au-I = 261.9 and 259.3 pm, IAuI = 176.8°.(Ph3P)2N2C4O2 (NMe) (3): space group P1̄, Z = 2, 4972 independent observed reflexions, R = 0.050. Lattice dimensions (-90 °C): a = 904.7, b = 993.8, c = 2017.4 pm; α = 101.55°, β = 96.39°, γ = 105.81°. The compound forms monomeric molecules with syn-conformation of the two NPPh3 groups. Bond lengths: P=N = 157.1; 155.3 pm, bond angles: PNC = 133°; 136°

Tetrahalogenotellurate(II): Synthese und Kristallstrukturen von Verbindungen mit den Ionen TeX42- (X = Cl, Br, I)/Tetrahalotellurates(II): Syntheses and Crystal Structures of Compounds with TeX42- Ions (X = Cl, Br, I)

1985 ◽  
Vol 40 (2) ◽  
pp. 251-257 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak ◽  
Bernt Krebs
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Acetonitrile Solution ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Square Planar

Abstract The compounds [(C6H5)4As]2 TeCl4 (1), [(C2H5)4 N]2 TeBr4 · CH3CN (2), and [(C2H5)4N]2TeI4 (3) were prepared by the reaction of Te, X2 , and excess (C2H5)4NX (X = Br, I) in acetonitrile solution or by heating of [(C6H5)4 As]2TeCl6 , Te, and (C6H5)4 ASCl for several hours in the same solvent.The structures of 1-3 were determined from single crystal X-ray data.1 crystallizes in the monoclinic space group P21/n with a = 1061.8(2), b = 1614.2(3), c = 1341.7(3) pm, β = 94.21° and Z = 2; 2: tetragonal, P4/mmm, a = 1039.7(2), c = 690.5(1), Z = 1; 3: tetragonal, I4/mmm, a = 1061.7(2), c = 1342.8(4), Z = 2. In 1-3 Te(II) exhibits a square planar coordination. The Te -CI, Te -Br, and Te-I bond lengths were found to be 260.7 (mean), 275.3, and 298.5 pm, respectively.

scholarly journals Die Jahn-Teller-Verzerrung in den Kristallstrukturen der Dinatrium-Tetrafluorometallate Na2CuF4 und Na2CrF4 / The Jahn-Teller Distortion in the Crystal Structures of the Disodium-Tetrafluorometallates Na2CuF4 and Na2CrF4

1989 ◽  
Vol 44 (7) ◽  
pp. 715-720 ◽  
Author(s):  
Dietrich Babel ◽  
Michael Otto
Keyword(s):  
Crystal Structures ◽  
Chain Structure ◽  
Teller Distortion ◽  
Space Group ◽  
X Ray ◽  
Edge Sharing Octahedra ◽  
Jahn Teller ◽  
A Chain ◽  
Jahn Teller Distortion ◽  
Ray Methods

The crystal structures of the isotypic monoclinic fluorides Na2CuF4 (a = 326.7(1), b = 937.0(2), c = 561.2(1) pm, β = 92.49(1)°; V = 171.63 x10-30 m3) and Na2CrF4 (a = 334.8(1), b = 954.9(2), c = 566.5(3) pm, β = 92.85(3)°; V = 180.89 × 10-30 m3) have been redetermined by single crystal X-ray methods. The compounds are Jahn-Teller distorted variants of the orthorhombic Sr2PbO4type (space group Pbam) and crystallize with Z = 2 in space group P21/c, a subgroup of Pbam. They form a chain structure of edge-sharing octahedra which are strongly elongated. The following distances were obtained: Cu-F = 190.4/193.8/235,7(2) pm and Cr-F = 199.1/199.7/241.7(4) pm. The geometry is compared to that of the corresponding distorted rutile type difluorides; relations to further compounds are discussed.

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.

Silberdiammin-disilber-hexacyanometallate(III): Kantenverknüpfte Doppeltetraeder-Einheiten Ag2N6 in den unterschiedlichen Strukturen von Eisen- und Cobaltkomplex / Silverdiammine Disilver Hexacyanometallates(III): Edge-Sharing Tetrahedra Ag2N6 in the Different Structures of Iron and Cobalt Complex

1988 ◽  
Vol 43 (12) ◽  
pp. 1589-1597 ◽  
Author(s):  
B. Ziegler ◽  
K. Seitz ◽  
D. Babel
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Dihedral Angle ◽  
Cobalt Complex ◽  
Iron Complex ◽  
Space Group ◽  
X Ray ◽  
R Factors ◽  
Ray Methods

Abstract The crystal structures of the monoclinic compounds Ag(NH3)2Ag2Fe(CN)6 (a = 948.2, b = 1235.5, c = 1246.8 pm, β = 94.98°. Z = 4. space group Cc) and Ag(NH3)2Ag2Co(CN)6 (a = 772.1, b = 1347.9, c = 1405.2 pm, β = 101.25°, Z = 4, C2/c) have been determined by x-ray methods from single crystals. Using 1947 and 2739 reflections, resp.. R factors of about 5% were reached. Both compounds are similar in containing approximately linear Ag(NH3)2+ dumb-bells (Ag-N = 216 pm) and dimeric Ag2N6 units. The latter consist of distorted edge-sharing tetrahedra (average Ag-N = 229 and 231 pm, resp.), the cavities of which are provided by the nitrogen ends of six surrounding M(CN)63- octahedra (Fe -C =195 pm, Co -C = 189 pm, C - N = 115 and 114 pm, resp.). In the iron complex, which is elpasolite-related, the central Ag2N2 ring is planar (Ag-Ag = 327.0 pm). By contrast the unit is folded (Ag-Ag = 307.8 pm, dihedral angle 126° between AgN2 triangles) in the cobalt complex, which has a different structure as discussed in detail

Reaction products of ammonium pertechnetate(VII) with triphenylphosphine and crystal structures of mer-Tc(PPh3)2Cl3(DMF) •2PPh3 and NH2(CH3)2+DMAH+ [TcCl6]2−•PPh3O

1991 ◽  
Vol 69 (3) ◽  
pp. 397-403 ◽  
Author(s):  
Fernande D. Rochon ◽  
Robert Melanson ◽  
Pi-Chang Kong
Keyword(s):  
Key Words ◽  
Crystal Structures ◽  
Bond Distance ◽  
Acetone Solution ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Group A

The reaction of NH4TcO4 with PPh3 in DMF solution in the presence of HCl produces mer-Tciii(PPh3)2Cl3(DMF)•2PPh3 (1). When the reaction is done in acidic DMA, the yellow product isolated was identified as NH2(CH3)2+DMAH+ [TcCl6]2−•PPh3O (2). The dimethylammonium cation was produced from the reaction of the solvent (DMA) with aqueous HCl. The reaction of NH4TcO4 with PPh3 in acidic acetone solution produces yellow (PPh3H)2[TcCl6] (≈15% yield) and some orange crystals (≈65% yield) identified by X-ray diffraction as [Ph3P-C(CH3)2-CH2-CO-CH3]+ [Tc(PPh3)Cl5]−. The cation was produced from the reaction of acetone used as solvent with HCl and PPh3. The crystals of 1 are monoclinic with P21/m space group, a = 11.393(4), b = 24.993(11), c = 12.398(4) Å, β = 106.98(3)°, Z = 2. The structure was refined to R = 0.072 and wR = 0.058. The Tc—O bond distance is 2.115(12) Å while the Tc—P bond lengths are 2.496(5) and 2.499(5) Å and the Tc—Cl are 2.399(5) and 2.342(3) Å. The C atoms of the DMF ligand are disordered. The crystals of 2 are triclinic, [Formula: see text] space group with a = 8.627(5), b = 13.308(7), c = 14.401(9) Å, α = 97.62(5), β = 91.31(5), γ = 106.42(5)°, and Z = 2. The structure was refined to R = 0.060 and wR = 0.076. The proton on DMAH+ is hydrogen bonded to the oxygen of PPh3O with a distance [Formula: see text] Key words: technetium, DMF, triphenylphosphine, dimethylacetamide.

Isoselenocyanatoborate -Kristallstrukturen von (n-Bu4N)[BH(NCSe)3] und (Ph4P)[B3H7(NCSe)] / Isoselenocyanatoborates -Crystal Structures of (n-Bu4N)[BH(NCSe)3] and (Ph4P)[B3H7(NCSe)]

1998 ◽  
Vol 53 (3) ◽  
pp. 271-274 ◽  
Author(s):  
B. Steuer ◽  
W. Preetz
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Elemental Selenium ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Structure Determinations ◽  
Average Bond

Abstract The treatment of [B6H6]2- with an excess of (SCN)2 in dichloromethane in the presence of solid KOH gives the hexaisoselenocyanatodiborate anion [B2(NCSe)6]2- as an intermediate (δ(11B) = -10.3 ppm), from which [BH(NCSe)3]- and elemental selenium are formed. The X-ray structure determinations on single crystals of (n-Bu4N)2[BH(NCSe)3] (1) (triclinic, space group Pi with a = 8.512(2), b = 10.885(3), c = 14.895(4) Å, α = 79.52(2), β = 74.86(2), γ = 86.768(2)°, Z = 2) and (Ph4P)[B3H7(NCSe)] (2) (monoclinic, space group C2, a = 7.686(5), b = 10.366(3), c = 17.533(3) A, β = 108.89°, Z = 4) show that the selenocyanate groups are coordinated exclusively via the N atoms with average bond lengths of B-N = 1.52, C-N = 1.15, C-Se = 1.75 A and angles N-C-Se = 179°, B-N-C = 168.7 - 176.8°. The N-B-N angles of 1 range from 107.5 to 109.5°.

Molecular and Crystal Structure of Sildenafil Base

2012 ◽  
Vol 67 (5) ◽  
pp. 491-494 ◽  
Author(s):  
Dmitrijs Stepanovs ◽  
Anatoly Mishnev
Keyword(s):  
Crystal Structure ◽  
Erectile Dysfunction ◽  
Crystal Structures ◽  
Unit Cell ◽  
Sildenafil Citrate ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

Sildenafil citrate monohydrate, well known as Viagra®, is a drug for the treatment of erectile dysfunction. Here we present the X-ray crystal structure of the sildenafil base, C22H30N6O4S. The compound crystallizes in the monoclinic system, space group P21/c with the unit cell parameters a = 17:273(1), b=17:0710(8), c=8:3171(4) Å , b =99:326(2), Z = 4, V = 2420:0(3) Å3. A comparison with the known crystal structures of sildenafil citrate monohydrate and sildenafil saccharinate is also presented.

Crystallographic studies of BaR2ZnO5 (R=La, Nd, Dy, Ho, Er, and Y)

1998 ◽  
Vol 13 (3) ◽  
pp. 144-151 ◽  
Author(s):  
Winnie Wong-Ng ◽  
Brian Toby ◽  
William Greenwood
Keyword(s):  
Neutron Diffraction ◽  
Crystal Structures ◽  
Lattice Parameters ◽  
Trigonal Prism ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

The crystal structures of BaR2ZnO5, where R=La, Nd, Dy, Ho, and Y, were studied by neutron diffraction, and that of the Er analog was investigated by synchrotron X-ray diffraction. Two structure types were confirmed for this series of compounds and agreed with those reported in literature. The compounds with a smaller size of R (R=Dy, Ho, Y, and Er) are isostructural to the orthorhombic “green phase (BaY2CuO5)” compounds. The cell parameters for compounds with the R=Er to Dy range from a=7.0472(1) Å to 7.0944(1) Å, b=12.3022(1) Å to 12.3885(2) Å, and c=5.6958(1) Å to 5.7314(1) Å, respectively. R is 7-fold coordinated inside a monocapped trigonal prism. These prisms share edges to form wavelike chains parallel to the long b-axis. The Ba atoms reside in 11-fold coordinated cages. The compounds which contain a larger size R (R=La and Nd) crystallize in the tetragonal I4/mcm space group, but are not isostructural to the “brown phases” BaR2CuO5. The lattice parameters for the La and Nd analogs are a=6.9118(1) Å, c=11.6002(2) Å for BaLa2ZnO5, and a=6.7608(1) Å and c=11.5442(2) Å for BaLa2ZnO5. The structure consists of ZnO4 tetrahedral groups (instead of planar CuO4 groups as found in the brown phase) with Ba ions inserted in between. The structure can be viewed as consisting of alternate layers of Zn-Ba-O and Nd-O extending infinitely in the xy plane and perpendicular to the z-axis.

Darstellung und Kristallstrukturen von LiGaCl4 und LiGaI4/ Preparation and Crystal Structure of LiGaCL4 and LiGaI4

1987 ◽  
Vol 42 (2) ◽  
pp. 248-250 ◽  
Author(s):  
Wolfgang Hönle ◽  
Bernhard Hettich ◽  
Arndt Simon
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
X Ray ◽  
Common Features ◽  
Bond Lengths ◽  
Ray Methods

Abstract The crystal structures of LiGaCl4 and LiGaI4 have been determined by single crystal X-ray methods. Both compounds are isotypic with LiAlCl4 and characterized by LiX6 octahedra and GaX4 tetrahedra. Mean bond lengths are: d̄(Ga-X) = 217.4 pm (Cl) and 255.9 pm (I); d̄(Li-X) = 263.9 pm (Cl) and 305.3 pm (I), respectively. Common features of the isotypic compounds LiGaX4 (X = Cl, Br. I) are discussed.

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