Crystal and Molecular Structure of Tris(Ethane-1,2-Diamine)Osmium(III) Trifluoromethanesulfonate Monohydrate

1987 ◽  
Vol 40 (7) ◽  
pp. 1267 ◽  
Author(s):  
PA Lay ◽  
GM Mclaughlin ◽  
AM Sargeson
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Oxidation State ◽  
Bond Order ◽  
Crystal And Molecular Structure ◽  
Single Bond ◽  
Bond Lengths ◽  
Formal Oxidation State ◽  
Bite Angle ◽  
Diamine Ligands

The crystal and molecular structure of racemic [Os(en)3] (CF3SO3)3.H2O has been determined. The [Os(en)3]3+ ion adopts a le ξob configuration and has approximate C2 symmetry with an Os-N(av.) bond length of 2.11 � and a bite angle for the chelate of - 82�. The previously recorded structure of the [Os(en-H)2(en)]2+ ion in which two deprotonated ethane-1,2-diamine ligands adoptoa cis configuration of the two amido donors, and in which the OsIV -N( amido ) bonds (1.90 �) are much shorter than the Os-N(amine) bonds, 2.11 ( cis ), 2.19 (trans), along with the present structure indicates a bond order > 1 for the osmiumo amido bond. The normal Os-N bond lengths fall into well defined ranges OS-NR3 (2.11-2.14 �), Os=NR2- (~1.90 �),Os=NR2 (- 1.70 �) and Os=N3-(- 1.58-1.63 �). These single bond lengths are more affected by trans effects than the formal oxidation state of the osmium centre.

Kristall-und Molekülstruktur von N-(TricHorgermyl)-trimethylphosphinimin [Cl3Ge-N=PMe3]n, n = 1 und 2 / Crystal and Molecular Structure of N-(Trichlorogermyl)-trimethylphosphinimine [Cl3Ge-N=PMe3]n, n= 1 and 2

1978 ◽  
Vol 33 (5) ◽  
pp. 493-497 ◽  
Author(s):  
W. S. Sheldrick ◽  
D. Schomburg ◽  
W. Wolfsberger
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
Centrosymmetric Dimer ◽  
Triclinic Space Group ◽  
Bond Lengths ◽  
Axial Ligands ◽  
Trigonal Bipyramidal ◽  
Coordinate Bond

Abstract N-(Trichlorogermyl)trimethylphosphinimine crystallizes in the triclinic space group P1̅ with a = 12.49(2), b = 12.54(3), c = 6.66(1) Å,a = 100.96(10),β = 91.45(14), γ = 102.77(15)°. The structure was solved by Patterson and difference syntheses and refined to R = 0.063 for 2867 independent reflections. In the unit cell there are two symmetry related monomers containing tetracoordinated Ge and one crystallographically centrosymmetric dimer with a planar four-membered [GeN]2 ring exhibiting trigonal-bipyramidal pentacoordinated Ge and trigonal N. Significant differences are observed in the bond lengths from pentacoordinated Ge to its equatorial and axial ligands: Ge-Neq 1.837(7), Ge-Nax 1.972(7), Ge-Cleq 2.176(2) and 2.170(2), Ge-Clax 2.345(3) Å. The Ge-Neq distance is similar to that observed in tetracoordinated derivatives [1.81-1.87 Å], whereas the Ge-Nax distance is 0.22 Å shorter than that observed for the axial N→Ge coordinate bond in hitherto known pentacoordinated derivatives [2.19-2.24 Å]. The very short Ge-N bond length of 1.737(8) Å in the monomer which is 0.07 Å shorter than in other tetracoordinated derivatives may be indicative of the involvement of a (p→d)π component.

The crystal and molecular structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, a phosphorus–silicon heterocycle

1979 ◽  
Vol 57 (2) ◽  
pp. 174-179 ◽  
Author(s):  
A. Wallace Cordes ◽  
Paul F. Schubert ◽  
Richard T. Oakley
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Monoclinic Space Group ◽  
Single Bond ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Bond Lengths

The crystal structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, (PhPSi2Me4)2, has been determined by single crystal X-ray diffraction. The crystals are monoclinic, space group P21/c, with a = 9.866(1), b = 11.921(1), and c = 11.324(2) Å, β = 104.31(1)°, Z = 2, and ρcalcd = 1.15 g/cm3. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.060 and Rw of 0.078, for 1173 reflections with intensities greater than 3σ. The (PhPSi2Me4)2 molecule lies on a crystallographic centre of symmetry, and the six-membered P2Si4 ring has a chair conformation with equatorial phenyl groups. The endocyclic angles at P (104.4(1)°) and Si (104.9(2)°) are intermediate between those found in cyclic hexaphosphine and hexasilane molecules, and the Si—Si and P—Si distances of 2.345(3) and 2.252(4) Å, respectively, correspond to single bond lengths, with no appreciable evidence for secondary pπ → dπ bonding between phosphorus and silicon. The Si—C (1.867(8) Å) and P—C (1.828(7) Å) bond lengths are also normal. The variations in the Si—P—C (101.6(2)°, 108.6(2)°), P—Si—C (range 106.2(3)–120.0(3)°), and Si—Si—C (range 105.8(3)–113.7(3)°) angles indicate that the positions of the exocyclic methyl and phenyl groups are influenced by both intra- and intermolecular steric forces.

scholarly journals Crystal and molecular structure of 2,2,4,6,6-pentamethyl-5-benzoyl-4-(N-methylbenzamido)-1,3-diaza-2,4,6(Pv)-triphosphorin

1977 ◽  
Vol 55 (13) ◽  
pp. 2534-2539 ◽  
Author(s):  
Richard T. Oakley ◽  
Norman L. Paddock ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Full Matrix ◽  
Bond Lengths ◽  
Benzoyl Group ◽  
Electron Withdrawal ◽  
Related Compounds ◽  
Twist Boat

Crystals of 2,2,4,6,6-pentamethyl-5-benzoyl-4-(N-methylbenzamido)-1,3-diaza-2,4,6(Pv)-tri-phosphorin are triclinic, a = 13.375(1), b = 11.313(1), c = 7.925(1) Å, α = 107.72(1), β = 98.23(1), γ = 87.00(1)°, Z = 2, space group [Formula: see text]. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares procedures to a final R of 0.067 and Rw of 0.089 for 3954 reflections with. I ≥ 3σ(I) The P3N2C ring is nearly planar and has a conformation corresponding to a flattened version of the chair – twist boat. Bond lengths in the azaphosphorin ring, P—N, 1.579–1.614(2), and P—C, 1.752(3) and 1.777(3) Å, indicate conjugation with the C-benzoyl group. The exocyclic P—N bond length, 1.742(3) Å, is longer than those in related compounds as a result of competitive electron withdrawal from the N-benzoyl group. Other bond lengths (corrected for libration) are: mean P—Me, 1.796(4); C=O, 1.242(3) and 1.247(4); C—N, 1.472(3) and 1.369(4); mean C—C(phenyl), 1.391(10); other C(sp2)—C(sp2); 1.417–1.518(4) Å.

The Crystal and Molecular Structure of the Dihydrochloride of 2-trans-6-Diethyl-2,4,4,6,8,8-hexamethylcyclotetraphosphazene

1975 ◽  
Vol 53 (16) ◽  
pp. 2413-2418 ◽  
Author(s):  
Harry P. Calhoun ◽  
Richard T. Oakley ◽  
Norman L. Paddock ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Crystal And Molecular Structure ◽  
Chair Conformation ◽  
Electrostatic Repulsion ◽  
Electron Localization ◽  
Full Matrix ◽  
X Ray ◽  
Bond Lengths ◽  
The Mean

Octamethylcyclotetraphosphazene is deprotonated by methyllithium to form carbanions, which react with methyl iodide to give ethyl derivatives N4P4Me8−nEtn, [Formula: see text] the structure of the dihydrochloride of the diethyl derivative, N4P4Me6Et2•2HCl has been determined. Its crystals are monoclinic, a = 9.928(5), b = 15.482(6), c = 6.329(2) Å, β = 103.29(2)°, space group P21/n. The structure was determined from diffractometer X-ray data and refined by full-matrix least squares methods to R 0.079 for 715 observed reflections. The N4P4Me6Et2H22+ ion lies on a crystallographic center of symmetry and the eight-membered phosphazene ring has the "chair" conformation. There are two significantly different P—N bond lengths, 1.665(6) and 1.572(7) Å, and two significantly different P—N—P angles, 126.7(6) and 139.8(6)°. The mean P—C bond length is 1.801(7) Å, and the mean N—P—N and C—P—C angles are 112.2(4) and 107.6° respectively. Bond lengths and angles in the phosphazene ring show the characteristic effects of π-electron localization found in other protonated phosphazene derivatives. The two ethyl groups are in tran-antipodal positions, corresponding to the least intramolecular electrostatic repulsion in the carbanion.

Kristall- und Molekülstruktur von As2P2S7/ Crystal and Molecular Structure of As2P2S7

1984 ◽  
Vol 39 (8) ◽  
pp. 1088-1091 ◽  
Author(s):  
Wolfgang Hönle ◽  
Claus Wibbelmann ◽  
Wolfgang Brockner
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Bond Length ◽  
Crystal And Molecular Structure ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Group V ◽  
X Ray ◽  
Bond Lengths ◽  
Crystal And Molecular Structures

AbstractThe crystal and molecular structures of As2P2S7 has been determined by single crystal X-ray diffraction (space group V 21/c; Z = 4; a = 1174.6(16) pm; b = 823.9(7) pm; c = 1140.1(10) pm; β - 94.43(9)°; R = 0.073. The molecule is isosteric to P4S7 and possesses C2v symmetry. Mean bond lengths are: d (As-As) = 250.9 pm; d (As-S ) = 225.7 pm; d(P - S) = 208.3 pm and d(P = S) = 193.2 pm. The observed As -As bond length agrees well with spectroscopic results

Crystal and Molecular Structure of N-(Trifluorosilyl)trimethylphosphinimine Dimer

1977 ◽  
Vol 32 (1) ◽  
pp. 22-25 ◽  
Author(s):  
W. S. Sheldrick ◽  
W. Wolfsberger
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Bond Lengths ◽  
Axial Ligands ◽  
Trigonal Bipyramidal ◽  
Pentacoordinate Silicon

N-(Trifluorosilyl)trimethylphosphinimine dimer crystallises in the monoclinic space group P21/n, Z = 2, with a= 6.314(2), b = 12.057(5), c = 10.936(4) Å, β = 95.45(2)°. The structure was solved by direct methods and refined to R 0.078 for 1117 independent reflections. The molecule is dimeric and centrosymmetric with an planar four-membered [SiN]2 ring containing trigonal-bipyramidal pentacoordinate silicon and trigonal nitrogen. Significant differences are observed in the bond lengths from silicon to its equatorial and axial ligands: Si-Neq 1.736(4), Si-Nax 1.857(4), Si-Feq1.606(4) and 1.607(3), Si-Fax 1.668(3) Å. The Si-Neq bond length is similar to that in tetracoordinate derivatives for which a (p →d) π bonding component has been postulated, while the Si-Nax distance is very much shorter than that observed in other pentacoordinate derivatives.

Crystal and Molecular Structure of the Copper(I)-thiolate-selenide Complex [Ph4P][Cu(SeS2CNC4H8)(S2CN2C4H8)] with an Unusual Se-S Bond

1999 ◽  
Vol 54 (10) ◽  
pp. 1313-1317 ◽  
Author(s):  
Qianfeng Zhang ◽  
Jinxi Chen ◽  
Maochun Hong ◽  
Xinquan Xin ◽  
Hoong-Kun Fun
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
Space Group ◽  
A Cell

Reaction of a DMF solution of Cu(S2CNC4H8) with [Ph4P]2[WSe4] affords [Ph4P]2[WSe4- (CuS2CNC4H8)3] (1) and [Ph4P][Cu(SeS2CNC4H )(S2CN2C4H8)] (2) in which a Se atom from the decomposition of the WSe42- anion has reacted with the pyrrolidyldithiocarbamate (C4H8dtc) ligand anion to form the new ligand anion SeS2CNC4H8⊖. Complex 2 crystallizes with four formula units in the monoclinic space group P21/c in a cell of dimensions a = 10.5824(2), b = 18.7575(3), c = 18.3268(4) Å and ß = 109.0980(10)°. 6055 independent reflections above background were measured with a diffractometer and the structure was refined anisotropically to R =0.073. The anion contains a three-coordinated copper(I) atom. The C4H8dtc⊖ ligand is bonded to the Cu+ cation in a terminal fashion, while SeS2CNC4H8⊖ chelates the Cu+ cation. The Se-S bond length is 2.231 (4) Å.

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