scholarly journals N-Iod-triphenylphosphanimin. Synthese und Kristallstrukturen von [Me3SiNPPh3· ICl] und Ph3PNI / N -Iodo-triphenylphosphaneimine. Synthesis and Crystal Structures of [Me3SiNPPh3 · ICl] and Ph3PNI

1996 ◽  
Vol 51 (12) ◽  
pp. 1739-1743 ◽  
Author(s):  
Jutta Grebe ◽  
Frank Weller ◽  
Kurt Dehnicke
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Iodine Atom ◽  
Bond Angle ◽  
Potassium Fluoride ◽  
Linear Arrangement ◽  
Space Group ◽  
Bond Lengths ◽  
Structure Determinations ◽  
Donor Acceptor

N-Iodo-triphenylphosphaneimine, Ph3PNI, has been prepared by thermolysis of the donor acceptor complex [Me3SiNPPh3·ICl] in boiling acetonitrile in the presence of potassium fluoride. Both compounds have been characterized by IR spectroscopy and by crystal structure determinations. [Me3SiNPPh3 · ICl]: Space group P1̄, Z = 2, a = 888.3(1), b = 1070.7( 1), c = 1310.2( 1) pm, α = 95.15( 1)°, β = 108.67( 1)°, γ = 97.78( 1)° at 20°C. The complex has a molecular structure in which the N atom of the phosphaneimine is connected with the iodine atom of the ICI molecule in a linear arrangement N-I-Cl with bond lengths N-I = 232.7 pm, I-Cl = 255.37 pm. \Ph3PNI: Space group P21/n, Z = 4, a = 952.8(1), b = 1800.8(2), c = 1003.6(1) pm, β = 110.25(1)° at -50°C. The compound forms monomeric molecules with bond lengths PN = 159.1 pm, I-N = 205.6 pm and an INP bond angle of 113.3°.

Iodbenzol als Lewis-Säure: Synthese und Kristallstrukturen von PPh4[Cl-I-C6H5] und PPh4[Br-I-C6H5] / Iodobenzene as Lewis-Acid: Synthesis and Crystal Structures of PPh4[Cl-I-C6H5] and PPh4[Br-I-C6H 5]

1996 ◽  
Vol 51 (11) ◽  
pp. 1579-1582 ◽  
Author(s):  
Mitra Ghassemzadeh ◽  
Jörg Magull ◽  
Dieter Fenske ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Lewis Acid ◽  
Iodine Atom ◽  
Acid Synthesis ◽  
Halide Ions ◽  
Linear Arrangement ◽  
Space Group ◽  
Structure Determinations ◽  
Donor Acceptor ◽  
Acetonitrile Solutions

The donor-acceptor complexes [X-I-C6H5]− with X− = Cl− and Br− have been prepared as tetraphenylphosphonium salts from iodobenzene and PPh4X in acetonitrile solutions. They form colourless single crystals, which were characterized by crystal structure determinations. PPh4[Cl-I-C6H5]: Space group P21/c, Z = 4. Lattice dimensions at -70°C: a = 1301.1(5), b= 1457.0(5), c = 1478.8(5) pm, β = 114.17(3)°. PPh4[Br-I-C6H5]: Space group P21/n, Z = 4. Lattice dimensions at 20°C: a = 1354.9(1), b= 1480.1(2), c = 1375.5(1) pm, β = 106.13(2)°. The halide ions are coordinate at the iodine atom of the iodobenzene molecule in a linear arrangement [X-I-C6H5]− with bond lengths Cl-I of 327.9 and Br-I of 347.2 pm.

Synthesen und Kristallstrukturen von [PPh3Me]NO2 und [PPh3 Me]HCO2H2O / Syntheses and Crystal Structures of [PPh3Me]NO2 and [PPh3Me]HCO2H2O

1988 ◽  
Vol 43 (10) ◽  
pp. 1279-1284 ◽  
Author(s):  
Mervat El Essawi ◽  
H Gosmann ◽  
D Fenske ◽  
F Schmock ◽  
K Dehnicke
Keyword(s):  
Crystal Structure ◽  
Aqueous Solutions ◽  
Ir Spectra ◽  
Bond Angle ◽  
Water Molecules ◽  
Moist Air ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Structure Determinations

Triphenylmethylphosphonium nitrite and formate have been prepared by the reaction of [PPh3Me]I with silver nitrite, and lead formate, respectively, in aqueous solutions. [PPh3Me]NO2 (1) forms pale yellow crystals, and [PPh3Me]HCO2·H2O (2) forms white crystals. Both compounds are soluble in water, ethanol, and dichloromethane. In moist air 2 is hydrated to yield [PPh3Me]HCO2·2H2O (3). The compounds were characterized by their IR spectra, 1 and 2 also by X-ray crystal structure determinations.[PPh3Me]NO2 (1): space group P21/n, Z = 4, 2088 independent observed reflexions, R = 0.062. Lattice dimensions (20 °C): a = 914.7(3), b = 1887.5(9), c = 1080.0(4) pm, β = 110.29(3)°. The compound consists of PPh3Me+ ions and NO2- anions with bond lengths of 114.2(6) pm and a bond angle of 124.1(7)°. [PPh3Me]HCO2·H2O (2): space group P21/n, Z = 4, 2973 independent observed reflexions, R = 0.069. Lattice dimensions (-20 °C): a = 931(2), b = 1558(3), c = 1281(2) pm, β = 105.9(1)°. The compound consists of PPh3Me+ ions and formate anions which form centrosymmetric dimeric units [HCO2·H2O]22- through hydrogen bridges of the water molecules. Bond lengths CO 122.4(4) and 120.9(4) pm. bond angle OCO 129.9(4)°.

Kupfer(I)-chlorid-Addukte von Phosphoraniminen Die Kristallstrukturen von Ph 3 PNPh * CuCl und von 2,3-Bis(triphenylphosphoranylidenamino)maIeinsäure-N-methylimid- Kupfer(I)-chlorid / Copper(I) Chloride Adducts of Phosphoranimines The Crystal Structures of Ph3 PNPh·CuCl and of 2,3-Bis(triphenylphosphoranylideneamino)maleic Acid N-Methylimide Copper(I) Chloride

1988 ◽  
Vol 43 (1) ◽  
pp. 5-11 ◽  
Author(s):  
Andrea Maurer ◽  
Dieter Fenske ◽  
Johannes Beck ◽  
Joachim Strähle ◽  
Eberhard Böhm ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Crystal Structures ◽  
Maleic Acid ◽  
Bond Angle ◽  
Asymmetric Unit ◽  
Space Group ◽  
Bond Lengths ◽  
Structure Determinations ◽  
Independent Molecules

Abstract The title compounds Ph3PNPh · CuCl (1) and (Ph3P)2 N2 C4O2 (NMe) CuCl (2) have been prepared by the reactions of CuCl with the corresponding phosphoranimines Ph3PNPh and 2.3-bis(triphenylphosphoranylideneamino)maleic acid N-methylimide, respectively. Both com-plexes were characterized by their IR spectra as well as by crystal structure determinations. Ph3PNPh · CuCl (1): space group P1, Z = 4, 3639 independent observed reflexions, R = 0.038. Lattice dimensions (18 °C): a = 1047.6; b = 1251.5; c = 1755 pm; α = 103.43°; β = 97.24°; γ = 101.30°. The compound forms monomeric molecules; the asymmetric unit contains two crystallo-graphically independent molecules. The CuCl molecule is bonded via the N atom of the phos-phoranimine. Bond lengths: Cu-N = 189 pm; Cu-CI = 209 pm; bond angle N - Cu - CI = 177°. (Ph3P)2N2C4O2(NMe) · CuCl (2): space group Pbca, Z = 8, 5611 independent, observed reflexions, R = 0.069. Lattice dimensions (25 °C): a = 1224.3; b = 1962.5: c = 2994.0 pm. The compound forms monomeric molecules with the CuCl molecule bonded via one of the N atoms of the phosphoranimine groups. Bond lengths: Cu - N = 194 pm; Cu-CI = 212 pm; bond angle N-Cu -CI -175°.

Die Kristallstruktur von Tris(trimethylstannyl) acetonitril / Crystal Structure of Tris(trimethylstannyl)- acetonitrile

1997 ◽  
Vol 52 (1) ◽  
pp. 145-148 ◽  
Author(s):  
Ralf Hillwig ◽  
Klaus Harms ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Single Crystals ◽  
Structure Determination ◽  
Bond Angle ◽  
Potassium Fluoride ◽  
Crystal Structure Determination ◽  
Space Group ◽  
Bond Lengths

Single crystals of (Me3Sn)3CCN were obtained by the reaction of tris(trimethylstannyl)amine with boiling acetonitrile in the presence of potassium fluoride and trimethylarsane. The compound has been characterized by IR spectroscopy and by a crystal structure determination. Space group P21/n, Z = 4; lattice dimensions at -50 °C: a = 975.4(1), b = 1316.3(2), c = 1485.3(1), β = 98.55(1)°, R = 0.029. (Me3Sn)3CCN forms monomeric molecules with a linear CCN axis (bond angle 178.7(6)°) and bond lengths of CC = 142.1(8) pm and CN = 114.5(8) pm

Nitrido-und Oxochlorokomplexe des Vanadiums(V); die Kristallstruktur von AsPh4 [V0C14] Nitrido and Oxochloro Complexes of Vanadium(V); the Crystal Structure of AsPh4[VOCl4]

1980 ◽  
Vol 35 (5) ◽  
pp. 522-525 ◽  
Author(s):  
Gisela Beindorf ◽  
Joachim Strähle ◽  
Wolfgang Liebelt ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Bond Length ◽  
Bond Angle ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Linear Arrangement ◽  
Space Group ◽  
X Ray ◽  
Complex Anions

The complexes AsPh4[Cl4V = N-Cl] and AsPh4[VOCl4] are prepared by the reaction of AsPh4Cl with Cl3VNCl and VOCl3, respectively. The IR spectra indicate C4v symmetry for the complex anions with multiple VN and VO bonds and a linear arrangement for the VNCl-group. AsPh4[VOCl4] crystallizes in the tetragonal space group P4/n with two formula units in the unit cell. The crystal structure was solved by X-ray diffraction methods (R = 0,062, 1096 observed, independent reflexions). The structure consists of AsPh4+ cations and [VOCl4]- anions with symmetry C4v. The extremely short VO bond length corresponds with a VO triple; its steric requirements cause the relatively large bond angle OVCl of 103.4°.

Crystal and molecular structure of L-prolinatodiphenylboron

1977 ◽  
Vol 55 (6) ◽  
pp. 958-965 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Conformational Disorder ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of L-prolinatodiphenylboron are monoclinic, a = 5.9427(5), b = 14.4633(7), c = 8.9654(4) Å, β = 98.423(8)°, Z = 2, space group P21. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.037 and Rw of 0.053 for 1477 reflections with I ≥ 3σ(I). The proline ring exhibits conformational disorder. The crystal structure consists of discrete molecules linked by N—H … O hydrogen bonds (N … O = 2.893(3) Å) along the short a axis. Intramolecular N—B coordination occurs to form a system of two fused five-membered rings. Bond lengths (corrected for libration) are: N—B, 1.630(3), O—B, 1.529(3), O—C, 1.219(3) and 1.300(3), N—C, 1.506(3) and 1.507(3), C(sp3)–C(sp3), 1.525(4), C(sp2)—C(sp3), 1.517(3), and mean C—C(phenyl), 1.394 Å.

Synthesen und Kristallstrukturen der Lithiumphosphide {Li(DME)[P(t-Bu)2]}2 und [Li(DME)PPh2]∞ / Syntheses and Crystal Structures of the Lithium Phosphides {Li(DME)[P(t-Bu)2]}2 and [Li(DME)PPh2]∞

1993 ◽  
Vol 48 (2) ◽  
pp. 156-160 ◽  
Author(s):  
Gudrun Stieglitz ◽  
Bernhard Neumüller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Membered Ring ◽  
Space Group ◽  
Bond Lengths ◽  
Polymeric Chains ◽  
Structure Determinations ◽  
Centrosymmetric Dimers

AbstractThe title compounds have been prepared by the reaction of n-butyllithium with the corresponding diorganophosphanes HPR2 (R = t-Bu, Ph) in DME solutions. Both compounds were characterized by crystal structure determinations.{Li(DME)[P(t-Bu)2]}2: Space group P 1̄, Z = 1, 2027 observed unique reflections, R = 0.055. Lattice dimensions at -80 °C: a = 879.9(3), b = 986.3(1), c = 1064.0(2) pm, α = 70.69(1)°, β = 70.63(2)°, γ - 69.89(2)°. The compound forms centrosymmetric dimers of symmetry Ci with Li-P bond lengths of 260.0 and 257.3 pm for the Li2P2 four-membered ring.[Li(DME)PPh2]∞: Space group P21/n, Z = 4. 3437 observed unique reflections, R = 0.055. Lattice dimensions at - 80 °C: a = 1034.8(2), b = 812.48(9), c = 1978.4(3) pm, β = 103.30(2)°. The compound forms polymeric chains via LiP bridges with Li-P bond lengths o f 256.3 and 254.1 pm.

Synthesen und Kristallstrukturen von PPh4[RuCl4(NO)(NSCl)] und (PPh4)2[RuCl4(NS)]2·4C H2Cl2 / Syntheses and Crystal Structures of PPh4[RuCl4(NO)(NSCl)] and (PPh4)2[RuCl4(NS)]2·4C H2Cl2

1986 ◽  
Vol 41 (5) ◽  
pp. 560-566 ◽  
Author(s):  
Wolfgang Willing ◽  
Ulrich Müller ◽  
Udo Demant ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Crystal Structures ◽  
Crystal Data ◽  
Acceptor Interaction ◽  
X Ray ◽  
Bond Lengths ◽  
Vacuum Pyrolysis ◽  
Structure Determinations ◽  
Donor Acceptor

Abstract By reaction of trithiazylchloride, (NSCl)3, with PPh4[RuCl4(NO)]2 in dichloromethane the thiazylchloridenitrosyl complex PPh4[RuCl4(NO)(NSCl)] is obtained; its vacuum pyrolysis at 200-220 °C yields the thionitrosyl com plex (PPh4)2[RuCl4(NS)]2 which crystallizes from CH2Cl2 solution with four molecules of CH2Cl2. Both com pounds were charaterized by their IR spectra and by X-ray crystal structure determinations. Crystal data: PPh4[RuCl4(NO)(NSCl)], mono­clinic, space group P 21/n, Z = 4, a = 982.6, b = 1700.0, c = 1772.3 pm , β = 104.79° (2548 observed reflexions, R = 0.046); (PPh4)2[RuCl4(NS)]2·4CH2Cl2, triclinic, P1̄ , Z = 1, a = 952.9, b = 1380.0, c = 1458.5 pm , α = 112.91, β = 106.67, γ = 92.61° (3760 observed reflexions, R = 0.053). In the [RuCl4(NO)(NSCl)]⊖ ion the nitrosyl and thiazyl chloride ligands occupy ex ­ positions; bond lengths indicate double bonds in the linear Ru=N=O group, while the NSCl molecule is attached by a donor-acceptor interaction Ru-N≡S̲-Cl , although with a rather short Ru-N bond of 198 pm (N≡S 144 pm, S-Cl 213 pm). The centrosymmetric [RuCl4(NS)]22⊖ ions have chloro bridges and NS ligands in axial positions; the nearly linear Ru=N=S group has bond lengths Ru=N 175 pm and N=S 147 pm.

Crystal and Molecular Structure of B-Phenyl-diptychboroxazolidine,

1975 ◽  
Vol 53 (10) ◽  
pp. 1393-1401 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Thermal Motion ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of B-phenyl-dictychboroxazolidine are monoclinic, a = 8.4977(4), b = 9.0617(5), c = 7.0105(3) Å, β = 111.627(3)°, Z = 2, space group P21. The structure was solved by direct methods and was refined by full-matrix least squares procedures to a final R of 0.040 for 967 reflections with I ≥ 3σ(I). The bond lengths involving nonhydrogen atoms have been corrected for thermal motion. Bond lengths are: B—O, 1.460(3) and 1.474(3), B—N, 1.666(3), B—C, 1.613(3), C—O, 1.411(3) and 1.419(3), C—N, 1.485(3) and 1.486(3), C(sp3)—C(sp3), 1.514(4) and 1.524(4), C—C(ar), 1.384–1.400(4–6), mean C—H, 0.98(4), and N—H, 0.87(5) Å. The crystal structure consists of discrete molecules of B-phenyl-diptychboroxazolidine each linked to two others by N—H … O hydrogen bonds (O … N = 2.914(3) Å) to form continuous spirals along b.

scholarly journals Crystal structure ofcatena-poly[silver(I)-μ-L-tyrosinato-κ2O:N]

2015 ◽  
Vol 71 (3) ◽  
pp. m50-m51
Author(s):  
Aqsa Yousaf ◽  
Muhammad Nawaz Tahir ◽  
Abdul Rauf ◽  
Shafique Ahmad Awan ◽  
Saeed Ahmad
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Double Layer ◽  
Title Compound ◽  
Bond Angle ◽  
Symmetry Code ◽  
Linear Arrangement ◽  
Bond Lengths ◽  
Polymeric Network ◽  
Polymeric Chains

The title compound, [Ag(C9H10NO3)]n, is a polymeric silver(I) complex of L-tyrosine. The AgIatom is connected to N and O atoms of two different L-tyrosine ligands in an almost linear arrangement, with an Ni—Ag—O1 bond angle of 173.4 (2)° [symmetry code: (i)x + 1,y,z]. The Ag—Niand Ag—O bond lengths are 2.156 (5) and 2.162 (4) Å, respectively. The polymeric chains extend along the crystallographicaaxis. Strong hydrogen bonds of the N—H...O and O—H...O types and additional C—H...O interactions connect these chains into a double-layer polymeric network in theabplane.

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