The Structures of Bis(O-Benzylxanthato)Nickel(II) and the Benzene Clathrate of Its 1,10-Phenanthroline Adduct

1986 ◽  
Vol 39 (12) ◽  
pp. 1983 ◽  
Author(s):  
AJ Edwards ◽  
BF Hoskins ◽  
G Winter
Keyword(s):  
Unit Cell ◽  
Molecular Structures ◽  
Space Group ◽  
Crystal And Molecular Structures ◽  
Benzene Clathrate

The crystal and molecular structures of bis (O- benzylxanthato )nickel(II), Ni( bzxa )2, and the benzene clathrate of its 1,10-phenanthroline adduct, Ni( bzxa )2( phen ).C6H6, are reported. Crystals of Ni( bzxa )2 are orthorhombic, with the space group P bca. There are four molecules per unit cell, which has dimensions a 6.961(1), b 35.008(8), c 7.277(2)Ǻ. The refinement converged with R 0.031 and Rw 0.037 after use of 1732 independent reflections for which I ≥ 2σ(I). Asymmetry of the nickel-sulfur bonds is observed. The adduct crystallizes in the space group C2/c. There are four molecules each of the adduct and benzene per unit cell, which has dimensions a 7.133(3), b 18.196(5), c 24.282(5)Ǻ, β 97.01(2)°. The refinement converged with R 0.064 and Rw 0.052 after use of 1123 independent reflections for which I ≥ 2σ(I). The packing clearly indicates that this host-guest compound is of the clathrate type.

Reaktionen von Oxo-Rhenium(VII und V)-Verbindungen mit Thiobenzoylhydrazin. Kristall- und Molekülstrukturen von Re(NHNC(S)Ph)3 · DMF, Re(NHNC(S)Ph)3 · OPPh3 und [Re(NHNC(S)Ph)(NHNHC(S)Ph)2]Cl · 1/3 C2H5OH · 1/3 H2O / Reactions of Oxorhenium(VII and V) Complexes with Thiobenzoylhydrazine. Crystal and Molecular Structures of Re(NHNC(S)Ph)3 · DMF, Re(NHNC(S)Ph)3 · OPPh3 and [Re(NHNC(S)Ph)(NHNHC(S)Ph)2]Cl · 1/3 C2H5OH · 1/3 H2O

1990 ◽  
Vol 45 (8) ◽  
pp. 1167-1176 ◽  
Author(s):  
Alfons Möhlenkamp ◽  
Rainer Mattes
Keyword(s):  
Unit Cell ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Chelating Ligands ◽  
Rhenium Atom ◽  
Coordination Polyhedra ◽  
Space Group ◽  
Crystal And Molecular Structures ◽  
Ligand Structure

The reaction of NaReO4 with thiobenzoylhydrazine yields Re(NHNC(S)Ph)3- DMF (1). With ReOCl3(PPh3)2 thiobenzoylhydrazine reacts to give Re(NHNC(S)Ph)3 · OPPh3 (2) and in the presence of HCl to yield [Re(NHNC(S)Ph)(NHNHC(S)Ph),]Cl · 1/3 C2H5OH -1 /3 H2O (3). The structures of 1-3 have been determined. 1: monoclinic, space group P2,/c, a = 1150.1(9), b = 2050.0(9), c = 1181.0(8) pm, β = 109.62(5)°, Z = 4, 2980 reflections, R = 0.055; 2: trigonal, space group R 3, a = 1399.8(1), c = 1684.0(1) pm, Z = 3, 1419 reflections, R = 0.033; 3: monoclinic, space group P2,/c, a = 1446.8(3), b = 3220.7(5), c = 1727.1(4) pm, β = 108.42(2)°, Z = 12, 6112 reflections, R = 0.062. In 1 and 2 three N,S-chelating ligands NHNR (R = C(S)Ph) are coordinated to the central rhenium atom. The ligand structure is intermediate between a diazene and a hydrazido(2–) structure. In 3 each rhenium atom is coordinated by one NHNR and two NHNHR ligands, all N,S-chelating. The latter can be considered as protonated diazene ligands. The unit cell contains three isomeric coordination polyhedra.

Organolanthanoids. XI. The Crystal and Molecular Structures of Two Tris(η5-cyclopentadienyl)(pyridine) lanthanoid(III) Compounds

1987 ◽  
Vol 40 (5) ◽  
pp. 907 ◽  
Author(s):  
GB Deacon ◽  
BM Gatehouse ◽  
SN Platts ◽  
DL Wilkinson
Keyword(s):  
Crystal Structures ◽  
Coordination Number ◽  
Unit Cell ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Crystal And Molecular Structures

The crystal structures of tris (η5-cyclopentadienyl) (pyridine) samarium(III), monoclinic, space group P21/c, a 10.906(4), b 8.636(2), c 17.825(3) �, β 96.44(2)�, Z 4, R 0.027 and Rw 0.032 for 3619 'observed' reflections, and tris (η5-cyclopentadienyl)(pyridine)neodymium(III), monoclinic, space group P21 / c, a 14-206(4), b 8.619(2), c 15.190(7) �, β 107.38(2)�, Z 4, R 0.035 and R, 0.039 for 2677 'observed' reflections have been determined. Both compounds have pseudotetrahedral geometry with a coordination number of 10 for the lanthanoid metal but there is a difference in the coordination of pyridine and in unit cell packing between the two structures.

The crystal and molecular structures of the ligand (E)-Pyridine-2-carbaldehyde Pyridin-2'-ylhydrazone and the palladium(II) complex Chloro[(E)-pyridine-2-carbaldehyde pyridin-2'-ylhydrazonato]palladium(II) which involves the coordination of the ligand in its anionic form

1984 ◽  
Vol 37 (4) ◽  
pp. 739 ◽  
Author(s):  
AT Casey ◽  
BF Hoskins ◽  
IP Traverso
Keyword(s):  
Least Squares Method ◽  
Complex Structure ◽  
Lone Pair ◽  
Unit Cell ◽  
Molecular Structures ◽  
Thermal Parameters ◽  
Anionic Form ◽  
Hydrogen Atoms ◽  
Space Group ◽  
Crystal And Molecular Structures

The crystal and molecular structures of the ligand (E)-pyridine-2-carbaldehyde pyridin-2'-ylhydrazone hydrate and its complex chloro[(E)-pyridine-2-carbaldehyde pyridin-2'-ylhydrazonato]palladium(II) have been determined by single-crystal three-dimensional X-ray diffraction techniques. Crystals of the ligand are monoclinic with space group P 21/c. The unit cell, which contains four molecules of ligand together with approximately ten disordered water molecules, has the dimensions a 17.762(4), b 3,8717(11), c 18.503(4) Ǻ and β 107.99(2)°. Crystals of the complex are triclinic with space group P1, and the unit cell has the dimensions a 6.9721(3), b 9.0739(11), c 9.1304(9) Ǻ, α81.116(9), β 88.778(8) and γ 81.392(8)°; Z = 2. The ligand structure was solved by direct methods and refined with anisotropic thermal parameters for all non-hydrogen atoms and isotropic thermal parameters for hydrogen and solvent atoms. The complex structure was solved by conventional Fourier methods and refined with anisotropic thermal parameters for all non-hydrogen atoms. A full-matrix least-squares method was employed for both structures based on 1295 and 2224 statistically significant reflections giving final values of R 0.061, Rw 0.068 and R 0.028, Rw 0.030 for the ligand and complex respectively. The structure analysis of the ligand shows definite evidence of delocalization of lone pair electrons in the hydrazine moiety. The ligand in its anionic form coordinates in a tridentate manner to the palladium atom in the complex through the two pyridine nitrogen atoms and the distal nitrogen of the hydrazine residue. A square-planar array is formed by a chlorine atom occupying the fourth position. Molecular dimensions suggest that the lone pair on the proximal nitrogen is delocalized over the entire molecule. Standard valence-bond and 'increased valence' methods have been applied in order to determine resonance schemes consistent with the observed structures of both the ligand and its complex.

Studies of Some Cadmium(II) and Mercury(II) Complexes With Dicyclohexylphosphino-N-Phenylthioformamide, LH: Crystal and Molecular-Structures of [Cdl2(LH)]2, ([HgCl2(LH)]2.CH2Cl2) And HgCl2(LH)2

1986 ◽  
Vol 39 (4) ◽  
pp. 547 ◽  
Author(s):  
SW Cowan ◽  
D Dakternieks ◽  
RW Gable ◽  
BF Hoskins ◽  
CL Rolls ◽  
...  
Keyword(s):  
Unit Cell ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Tetrahedral Geometry ◽  
Triclinic Space Group ◽  
Space Group ◽  
Mercury Compounds ◽  
Crystal And Molecular Structures ◽  
Tetrahedral Environment

The crystal and molecular structures of the title compounds, [CdI2(LH)]2, (1), [HgCl2(LH)]2.CH2Cl2(2), and HgCl2(LH)2(3)[where LH = dicyclohexylphosphino-N-phenyl-thioformamide,* (c-C6H11)2PC(S)N(H)Ph] have been determined by single-crystal X-ray diffraction techniques. Crystals of (1) are monoclinic, space group P21/n, a 13.051(2), b 10.183(1), c 18.106(1)Ǻ and β 101.55(8)° with Z 2; R and Rw were 0.047 and 0.044 respectively for 2320 unique, observed reflections. The unit cell contains two equivalent centrosymmetric, halogen-bridged cadmium dimers. Crystals of (2) are triclinic, space group Pī, with a 10.668(4), b 14.978(3), c 16.838(4)Ǻ, and α 111.80(2), β 101.03(2), γ 92.06(2)° with Z 2; R and Rw were 0.069 and 0.067 respectively for 3379 unique observed reflections. The structure shows two independent centrosymmetric halogen-bridged dimers within the unit cell. Crystals of (3) are monoclinic, space group C2/c, a 24.719(6), b 12.247(3), c 26.818(6) Ǻ, and β 94.62(2)° with Z 8; R and Rw were 0.075 and 0.071 respectively for 2698 unique, observed reflections. The structure shows the complex to be monomeric. In all three compounds the metal atom is in an approximately tetrahedral environment with the potentially multidentate ligand, LH, coordinating only through the phosphorus atom. The mercury compounds show a much larger deviation from ideal tetrahedral geometry than does the cadmium compound.

Metallacyclohexasulfanes: the crystal and molecular structures of (η5-C5H5)2MS5, M = Zr and Hf

1987 ◽  
Vol 65 (7) ◽  
pp. 1676-1680 ◽  
Author(s):  
Alan Shaver ◽  
James M. McCall ◽  
Victor W. Day ◽  
Sarah Vollmer
Keyword(s):  
Single Crystal ◽  
Unit Cell ◽  
Molecular Structures ◽  
Equatorial Position ◽  
Ring Inversion ◽  
Space Group ◽  
Crystal And Molecular Structures ◽  
Monoclinic Unit Cell ◽  
Coordination Spheres

The crystal and molecular structures of (η5-C5H5)2ZrS5, 2, and (η5-C5H5)HfS5, 3, have been determined by single crystal diffractometry methods. Both compounds crystallized with four molecules in a monoclinic unit cell of dimensions: a = 8.984(3) Å, b = 13.336(4) Å, c = 11.421(2), β = 93.10(2)° for 2, and a = 9.012(2) Å, b = 13.291(2) Å, c = 11.381(2) Å, β = 93.25(1)° for 3; the space group is P21/n for both. These crystals of 2 and 3 are thus isomorphous with those of (C5H5)2TiS5, 1, studied by Epstein etal. (3a). The structures of all three complexes are very similar consisting of a cyclohexane-like six-membered MS5 ring with two C5H5 rings attached to the metals in an axial and equatorial position. The coordination spheres of 2 and 3 are less crowded than that of 1. The consequences of this are discussed with respect to the barriers to ring inversion in these complexes.

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.

Synthesis of C-aryl-N-(2-hydroxyphenylmethyl)-nitrones and their reaction with diphenylborinic or carboxylic acid derivatives. Crystal and molecular structures of a free nitrone ligand and its diphenyl–boron chelate

1997 ◽  
Vol 75 (12) ◽  
pp. 1830-1843 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Jörg Metge ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Carboxylic Acid ◽  
Electron Distribution ◽  
Direct Methods ◽  
Molecular Structures ◽  
State Structure ◽  
Space Group ◽  
Crystal And Molecular Structures ◽  
New Type ◽  
Boron Chelate ◽  
Diphenylboron Chelate

The syntheses of a number of aromatic aldonitrones of N-(2-hydroxyphenylmethyl)hydroxylamine and their subsequent reactions with diphenylborinic or carboxylic acid derivatives are reported. Crystals of 8-(4-dimethylaminophenylmethylene)-6,6-diphenyl-5,7-dioxa-8-azonia-6-borata-5H-6,7,8,9-tetrahydrobenzocycloheptene, 2b, are triclinic, a = 10.6802(8), b = 11.1809(4), c =10.1520(3) Å, α = 105.847(3)°, β = 92.567(4)°, γ = 84.610(5)°, Z = 2, space group PĪ, and those of C-(4-dimethylaminophenyl)-N-(2-hydroxyphenylmethyl)nitrone, 6e, are monoclinic, a = 12.2319(8), b = 7.071(1), c = 17.2005(9) Å, β = 107.520(4)°, Z = 4, space group P21/a. The structures were solved by direct methods and refined by full-matrix least-squares procedures to R = 0.035 and 0.032 (Rw = 0.036 and 0.032) for 3379 and 1800 reflections with I ≥ 3σ(I), respectively. Compound 2b is representative of a new type of heterocyclic B,N-betaine. The solid state structure of 6e (the precursor to 2b) shows that only small topological changes, but significant changes in the electron distribution, occur upon the formation of the diphenylboron chelate. Keywords: aromatic aldonitrones, organoboron compounds, crystal structures.

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.

Cyclische Diazastannylene, XVIII [1]Zur Frage der Bindungsbeschreibung in Polyedern des Typs Sn4X3Y:Die Kristall-und Molekülstrukturen von Sn4(NtBu)4 und Sn4(NtBu)3O / Cyclic Diazastannylenes, XVIII [1]Bonding Description in Polyhedra of the Sn4X3Y-Type:The Crystal and Molecular Structures of Sn4(NtBu)4 and Sn4(NtBu)3O

1983 ◽  
Vol 38 (9) ◽  
pp. 1054-1061 ◽  
Author(s):  
M. Veith ◽  
O. Recktenwald
Keyword(s):  
Van Der Waals ◽  
Structural Data ◽  
Van Der Waals Forces ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Structural Elements ◽  
Triclinic Space Group ◽  
Space Group ◽  
O 213.2 ◽  
Crystal And Molecular Structures

Abstract Crystals of Sn4(NtBu)4 (1) are monoclinic, space group P21/c, with cell constants a = 1038.9(4), b = 1468.3(5), c = 1698.8(5) pm, β = 91.6(1)° and Z = 4, while those of Sn4(NtBu)3O (2) are triclinic, space group P 1̄, with dimensions a = 1293.0(5), b = 1027.1(5), c = 1716.7(9) pm, α = 90.9(1), β = 102.5(1), γ = 107.0(1)° and Z = 4. The molecules 1 are held together by van-der-Waals forces, whereas two molecules 2 interact in the crystal by weak 0→Sn donor bonds (290-332 pm) forming dimers. The outstanding structural elements of 1 and 2 are the Sn4N4 and Sn4N3O polyhedra, which can be described by two interpenetrating tetrahedra of tin atoms and of nitrogen or nitrogen and oxygen atoms forming a distorted cube, which approaches 4̄3 m symmetry in the case of 1 and 3m for 2. Characteristic distances are in 1: Sn-N 220.2 pm, in 2: Sn-N 221.3 pm and Sn-O 213.2 pm. An almost ionic bonding model and two covalent models are discussed on the basis of the structural data including Sn4(NtBu)3OAlMe3.

C-(2-Hydroxyaryl)-N-(2-hydroxyphenylmethyl)nitrones as regioselective bidentate ligands in boron chelate formation. Crystal and molecular structures of a diphenylboron complex and its parent ligand

1998 ◽  
Vol 76 (7) ◽  
pp. 1082-1092 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Jörg Metge ◽  
Steven J Rettig ◽  
James Trotter
Keyword(s):  
Direct Methods ◽  
Acid Anhydride ◽  
Molecular Structures ◽  
Bidentate Ligands ◽  
Full Matrix ◽  
Space Group ◽  
Crystal And Molecular Structures ◽  
Chelate Formation ◽  
Boron Chelate ◽  
Parent Ligand

The C-(2-hydroxyaryl)-N-(2-hydroxyphenylmethyl)nitrones 5 are synthesized by the condensation of variously substituted salicylaldehydes with N-(2-hydroxyphenylmethyl)-hydroxylamine. These nitrones react with diphenylborinic acid anhydride to form seven-membered diphenylboron chelates 6. Crystals of C-(4-diethylamino-2-hydroxyphenyl)-N-(2-hydroxyphenylmethyl)nitrone, 5d, are monoclinic, a = 6.911(2), b = 10.663(2), c = 22.951(1) Å, β = 97.33(1)°, Z = 4, space group P21/n, and those of 4-dimethylamino-8-(2-hydroxyphenylmethyl)-6,6-diphenyl-5,7-dioxa-8-azonia-6-borata-6,7-dihydro-5H-benzocycloheptene-ethanol, 6d·EtOH, are monoclinic, a = 9.069(2), b = 29.881(1), c = 11.1883(6) Å, β = 109.426(9)°, Z = 4, space group P21/n. The structures were solved by direct methods and refined by full-matrix least-squares procedures to R = 0.032 and 0.039 (R w = 0.031 and 0.036) for 2510 and 4162 reflections with I > 3σ(I), respectively. Key words : C-(2-hydroxyaryl)-N-(2-hydroxyphenylmethyl)nitrones, organoboron compounds, crystal structures.

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