The synthesis, crystal and molecular structures of triphenyl(phenylthio)silane, Ph3SiSPh, and of bis(μ-thiophenolato)bis[tetracarbonyltungsten(I)], [W(CO)4(SPh)]2

1987 ◽  
Vol 65 (4) ◽  
pp. 898-902 ◽  
Author(s):  
C. Robert Lucas ◽  
Michael J. Newlands ◽  
Eric J. Gabe ◽  
Florence L. Lee
Keyword(s):  
Bond Length ◽  
Phenyl Ring ◽  
Close Approach ◽  
Molecular Structures ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Structure Determinations

Preparations and X-ray structure determinations are described for Ph3SiSPh and [W(CO)4(μ-SPh)]2. The compound Ph3SiSPh crystallizes in space group Pcab with a = 15.260 Å, b = 15.968 Å, c = 16.757 Å, Z = 8, dcalc = 1.20 g cm−3 (MoKα1, λ = 0.70930 Å). The structure was solved with MULTAN and refined to the final R = 0.050 for 1933 significant reflections. The molecule has an unusual C—S—Si angle of 99.5° and a short Si—S bond length of 2.156 Å. The compound [W(CO)4(μ-SPh)]2 crystallizes in the space group P21/c with a = 9.164 Å, b = 12.054 Å, c = 11.163 Å, β = 111.63°, Z = 2, dcalc = 2.35 g cm−3 (MoKα1, λ = 0.70930 Å). The structure was solved with MULTAN and refined to the final R = 0.062 for 2748 significant reflections. The molecule is a dimer with a crystallographic center of symmetry. There is a short W—W distance (2.972 Å), a wide S—W—S′ angle (106.3°), a compressed W—S—W′ angle (73.67°) and there is distortion of a CO on each W due to the close approach of an ortho-H in a phenyl ring.

The Crystal and Molecular Structures of Bis(diethyldithiocarbamato)platinum(II) and Bis[di(2-hydroxyethyl)dithiocarbamato]platinum(II)

1992 ◽  
Vol 45 (2) ◽  
pp. 429 ◽  
Author(s):  
AT Baker ◽  
MT Emett
Keyword(s):  
Single Crystal ◽  
Bond Length ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Crystal And Molecular Structures

The structures of [Pt(S2CN(C2H5)2)2] (1) and [Pt(S2CN(C2H4OH)2)2] (2) have been determined by single-crystal X-ray diffractometry. Compound (1) crystallizes in the tetragonal space group P42/n, a 16.4692(10),c 6.2160(6) � (Z = 4); R was 0.029 for 1012 observed reflections. Compound (2) is monoclinic, space group Pc, a 6-0663(11), b 1.1784(15), c 12.5740(21) � ,β92.569(8)� (Z = 2); R was 0.019 for 1573 observed reflections. The presence of electron-withdrawing groups in the ligands of (2) appears to have little effect on the Pt-S distances but causes an increase in the C-N bond length, with the C-N bond lengths being significantly different at the 2 σ level.

Synthesis and resolution of an asymmetric arsonium cation. Crystal and molecular structures of (R)-Benzyl(methyl)(4-methylphenyl)(naphthalen-1-yl)- arsonium bromide and hexafluorophosphate

1984 ◽  
Vol 37 (6) ◽  
pp. 1171 ◽  
Author(s):  
DG Allen ◽  
CL Raston ◽  
BW Skelton ◽  
AH White ◽  
SB Wild
Keyword(s):  
Ion Exchange ◽  
Absolute Configuration ◽  
Optically Active ◽  
Molecular Structures ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Ion Exchange Column ◽  
Optically Pure

The (�)-benzyl(methyl)(4-methylphenyl)(naphthalen-1-yl)arsonium cation has been synthesized and subsequently resolved by fractional crystallization of monohydrogen [R-(R*,R*)]-2,3-bis(benzoyloxy)- butanedioate salts. The separated diastereoisomers were converted into the corresponding optically active arsonium bromides by ion-exchange column chromatography. The absolute configuration of the arsonium cation exhibiting a positive rotation at 589 nm (sodium D line) has been established as (R) by single-crystal X-ray analysis of both the bromide and hexafluorophosphate salts. The arsonium bromide with [α]D + 54.8�(c, 0.62 in CH2Cl2) crystallizes in the orthorhombic space group P212121 (D24, No.19) with a 22.472(8), b 15.724(7), c 12.585(5) � and U 4447(3) �3. The corresponding hexafluorophosphate with [α]D + 19.3� (c, 0.5 in CH2Cl2) crystallizes in the same space group with a 23.56(2), b 16.40(1), c 13.12(1) � and U 5067(6) � 3. Benzylidene transfer to benzaldehyde from the arsonium ylide derived from either of the arsonium salts produced optically pure (–)-(S)-methyl(4-methylphenyl)(naphthalen-1-yl)arsine, [α]D - 115.9� (c, 0.593 in CHCl3), and partly resolved [R-(R*,R*)]-2,3-diphenyloxiran.

Arsenic(III), Antimony (III) and Bismuth(III) Thiobenzoates: Crystal and Molecular Structures of M(SOCR)3 and PhSb(SOCPh)2

1998 ◽  
Vol 53 (12) ◽  
pp. 1475-1482 ◽  
Author(s):  
Prit Singh ◽  
Sudha Singh ◽  
Vishnu D. Gupta ◽  
Heinrich Nöth
Keyword(s):  
Crystal Structure ◽  
Molecular Structures ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Covalently Bonded ◽  
Bismuth Complex ◽  
Group 15 ◽  
Structure Determinations ◽  
Trigonal Pyramid ◽  
Trigonal Prisms

Abstract Tris-thiobenzoates, Arsenic, Antimony, Bismuth Tris-thiobenzoates of arsenic, antimony and bismuth, M(SOCR)3 have been obtained from their oxides and characterized. In the X-ray crystal structure determinations of these, the group 15 atom and the three covalently bonded sulfur atoms are found to constitute a trigonal pyramid, the central atoms lie at a C3 axis. In the bismuth complex the thiobenzoate ligand tends to chelate. However, three comparatively short intermolecular M···S interactions are significant features for these molecules resulting in stacking of trigonal prisms providing an essentially six coordinate environment around arsenic and antimony and a nine-coordinate one for bismuth. The structure of PhSb(SOCPh)2 can be considered

The crystal and molecular structures of the bispyridine and 1,10-phenanthroline adducts of Bis(ethyl 3-mercaptobut-2-enoato)nickel(II)

1982 ◽  
Vol 35 (2) ◽  
pp. 331 ◽  
Author(s):  
J Sachinidis ◽  
MF Mackay ◽  
MW Grant
Keyword(s):  
Thermodynamic Data ◽  
Molecular Structures ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Crystal And Molecular Structures ◽  
Distorted Octahedral ◽  
In Cis ◽  
Oxygen Atoms

X-ray analyses of monoclinic crystals of the bispyridine and 1,10-phenanthroline adducts of the monothioacetylacetonate complex bis(ethyl 3-mercaptobut-2-enoato)nickel(n), Ni(eosm)2,* have defined their structures. Crystals of the bispyridine adduct Ni(eosm)2,py2, C22H28N2NiO4S2, belong to the space group P21/c with a 8.865(6), b 15.758(4), c 9.136(3)Ǻ, β 109.18(4)°, Z 2. Crystals of the 1,10-phenanthroline adduct Ni(eosm)2,phen, C24H26N2NiO4S2, belong to the space group P21c with a 12.451(2), b 16.949(1), c 15 5921(2) Ǻ, β 130.97(1)°, Z 4. The structures were refined with diffractometer data measured with Cu Ka radiation to R 0.047 (1962 terms) for the bispyridine adduct and R 0.061 (3115 terms) for the phenanthroline adduct. The geometry about the nickel in each complex is distorted octahedral. The molecule of the bispyridine adduct has exact rn symmetry with the two sulfur atoms cis-equatorial and the nitrogen atoms axial. In the phenan- throline adduct, pairs of sulfur, nitrogen and oxygen atoms are in cis configurations. In the bis-pyridine adduct, the Ni-N bond lengths, 2.153(3) and 2.182(4) Ǻ, are significantly longer than those in other bispyridine adducts of nickel(II) species. It is suggested that the long Ni-N distances reflect the relative instability of the bispyridine adduct, and thermodynamic data are presented to support this.

Copper complexes of Picloram: The crystal and molecular structures of Bis(4-amino-3,5,6-trichloropyridine-2-carboxylato)aquacopper(II) dihydrate and Bis(4-amino-3,5,6-trichloropyridine-2-carboxylato)bis(pyrimidin-2-amine)copper(II)

1983 ◽  
Vol 36 (1) ◽  
pp. 183 ◽  
Author(s):  
EJ O'Reilly ◽  
G Smith ◽  
CHL Kennard ◽  
AH White
Keyword(s):  
Copper Complexes ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Trigonal Bipyramidal ◽  
Distorted Octahedral ◽  
A Cell ◽  
Amine Ligands

The crystal structures of two copper(II) complexes of the herbicide Picloram (4-amino-3,5,6-trichloro- pyridine-2-carboxylic acid) have been determined by single-crystal X-ray diffractometry. Bis(4-amino- 3,5,6-trichloropyridine-2-carboxylato)aquacopper(II) dihydrate (1) is monoclinic, space group C2/c, with Z 4 in a cell of dimensions a 15.593(6), b 7.940(6), c 16.983(6) �, β 107.58(3)�. The structure was refined to a residual R 0.046 for 905 'observed' reflections. Complex (1) is trigonal bipyramidal with the trigonal plane consisting of oxygens from two picolinate ligands [Cu-O 1.995(5) �] and a water molecule [Cu-O 2.080(5) �]. The apical positions are occupied by pyridine ring nitrogens from the Picloram ligands [Cu-N 2.021(5) �]. Bis(4-amino-3,5,6-trichloropyridine- 2-carboxylato)bis(pyrimidin-2-amine)copper(II) (2) is monoclinic, space group P2,/c, with Z 4 in a cell of dimensions a 12.3 11(5), b 15.435(5), c 15.320(6) �, β 115.95(3)�, and gave a final R 0.059 for 2429 'observed' reflections. In complex (2), the copper(II) atom has a tetragonally distorted octahedral stereochemistry with the Picloram ring nitrogens once again occupying the two axial positions [Cu-N 2.586(7) and 2.611(7) �]. The square plane consists of two carboxylato oxygens [Cu-O 1.941(6) and 1.960(7) �] and two hetero-nitrogens from pyrimidin-2-amine ligands [Cu-N 2.048(6) and 2.054(6) �].

Bisphenol flukicides. VI. The crystal and molecular structures of 2,2'-(Phenoxymethylene)bis(4-chloro-6-nitrophenol) and a triethylamine adduct of 2,2'-(Benzyloxymethylene)bis(4-chloro-6-nitrophenol)

1982 ◽  
Vol 35 (2) ◽  
pp. 341 ◽  
Author(s):  
DG Hay ◽  
MF Mackay
Keyword(s):  
Molecular Structures ◽  
Dihedral Angles ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures

X-ray crystallographic analyses have defined the conformational detail in the title compounds. Crystals of 2,2'-(phenoxymethylene)bis(4-chloro-6-nitrophenol) (1), Cl9H12Cl2N2O7, are monoclinic: space group P21/n, a 8.616(1), b 16.214(1), c l3.727(1) �, β 92.13(1)� and Z 4. The triethylamine adduct of 2,2'-(benzyloxymethylene)bis(4-chloro-6-nitrophenol) (2),Et3N, C20H14Cl2N2O7,C6H15N, crystallizes in the monoclinic space group P21/c with a 9.454(1), b 11.911(2), c 25.392(2) �, ββ 109.96(1)� and Z 4. The structures were refined with diffractometer data measured with Cu Kα radiation to R 0.061 (1761 terms) for (1) and R 0.063 (1230 terms) for (2),Et3N. The methylenebisphenol moieties in the molecules of (1) and (2) adopt twist and butterfly conformations respectively. In (1), the dihedral angles between the perpendiculars to the plane of the C-C-C bridge and the phenol rings are 61.1(4) and 71.6(4)�; in (2), these angles have values of 88.0(8) and 85.6(7)�.

Preparation, crystal and molecular structures of Ph2CNSNSO and a comparison of the —SNSO and —SNSS chromophores

1985 ◽  
Vol 63 (5) ◽  
pp. 1063-1067 ◽  
Author(s):  
Tristram Chivers ◽  
Richard T. Oakley ◽  
Roger Pieters ◽  
John F. Richardson
Keyword(s):  
Thermal Decomposition ◽  
Molecular Structures ◽  
Structural Determination ◽  
Model Compounds ◽  
Excitation Energies ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Mndo Calculations

The sulphenyl chloride, Ph2CNSCl, prepared insitu from Ph2CNSiMe3 and sulphur dichloride, has been employed in the synthesis of Ph2CNSNSO and Ph2CNSNSNSNCPh2 by reaction with Me3SiNSO and Me3SiNSNSiMe3, respectively. An X-ray structural determination of Ph2CNSNSO shows it to consist of a planar cis-trans chain. The crystals are triclinic and belong to the space group[Formula: see text], a = 9.9078(8), b = 10.0967(9), c = 15.1682(14) Å, α = 78.646(7), β = 71.065(7), γ = 63.449(7)°, V = 1281.5(5) Å3, Z = 4. The final R and Rw values were 0.033 and 0.027, respectively. The π* → π* excitation energies for the RSNSO and RSNSS chromophores are compared for different R groups and discussed in the light of MNDO calculations on the model compounds HSNSX (X = S, O). The thermal decomposition of both Ph2CNSNSO and Ph2CNSNSNSNCPh2 produced S4N4 and Ph2CO or (Ph2CN)2S, respectively.

Crystal structures of 1-(m-nitrophenyl)-2,2-dicarboethoxy-3-phenyl-pyrrolidin-5-one (C22H22N2O7) (I) and 1-(p-chlorophenyl)-2,2-dicarboethoxy-3-phenyl-pyrrolidin-5-one (C22H22NO5Cl) (II)

1989 ◽  
Vol 189 (3-4) ◽  
Author(s):  
G. D. Nigam ◽  
G. Mattern ◽  
R. Fröhlich
Keyword(s):  
Crystal Structures ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures

AbstractThe crystal and molecular structures of 1-(m-nitrophenyl)-2,2-dicarboethoxy-3-phenyl-pyrrolidin-5-one (I) and 1-(p-chlorophenyl)-2,2-dicarboethoxy-3-phenyl-pyrrolidin-5-one (II) have been determined by X-ray diffraction methods. (I) crystallizes in the monoclinic space group

Two crystal structures of 10,10′-(l,4-phenylene-dimethylidene)-bis-9,10-H-anthracenone

1992 ◽  
Vol 200 (3-4) ◽  
Author(s):  
G. Dewald ◽  
M. Hanack ◽  
E.-M. Peters ◽  
L. Walz
Keyword(s):  
Crystal Structures ◽  
Diffraction Data ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures

AbstractThe crystal and molecular structures of dimorphic 10,10′-(1,4-phenylene-dimethylidene)-bis-9,10-H-anthracenone (1) have been determined using X-ray diffraction data. The compound crystallizes either in the monoclinic space groupSince all non-hydrogen atoms are of pure

Kristall- und Molekülstrukturen von zwei trans-1.2.4.5-Tetraza-3.6-diphospha-cyclohexan-3.6-disulfiden / Crystal and Molecular Structures of Two trans- 1,2,4,5-Tetraza-3,6-diphospha-cyclohexane-3,6-disulfides

1984 ◽  
Vol 39 (3) ◽  
pp. 269-274 ◽  
Author(s):  
Franz Dirschl ◽  
Heinrich Nöth
Keyword(s):  
Chair Conformation ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
Torsion Angles ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Twist Conformation

The crystal and molecular structures of two trans-1,2,4,5-tetraza-diphospha-3,6-cyclohexane- 3,6-disulfides, 2 and 3, have been determined by X-ray diffraction methods. The 3,6-diphenyl- 1,2,4,5-tetramethyl-derivative 2 crystallizes in the monoclinic system, space group C He. Its P2N 4 heterocycle adopts a twist conformation. In contrast, the hexamethyl derivative 3 is triclinic, space group P1̅, and its ring shows chair conformation. Torsion angles in these two compounds and similar ones reveal less interaction between lone pairs of electrons on adjacent N-atoms in the chair conformation but stronger interaction of those bound to phosphorus. It is suggested that the latter interaction is responsible for the larger N -P -N bond angle (107°) as compared to the smaller one (101°) in the P2N4 rings present in twist conformation.

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