Crystal and Molecular Structures of t-Butyl Isocyanide-Undecacarbonyl-Tetrahydrido-Tetraruthenium, Ru4(µ-H)4(CO)11(CNBu t )

1997 ◽  
Vol 50 (9) ◽  
pp. 879 ◽  
Author(s):  
Michael I. Bruce ◽  
Michael Schulz ◽  
Edward R. T. Tiekink
Keyword(s):  
Direct Methods ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Crystal And Molecular Structures

The crystal and molecular structures of Ru4(µ-H)4(CO)11(CNBut) (2), obtained with Ru4(µ- H)4(CO)10(CNBut)2 by hydrogenation of Ru5(µ5-CNBut)(CO)14(CNBut) (1), have been determined. Crystals of (2) are monoclinic, space group P 21/c, with a 12·349(1), b 11·627(3), c 17·0222(7) Å, β 105·785(4)°, V 2351·9(6) Å3 and Z 4. The structure was solved by direct methods and refined using 4478 reflections to final R 0·028(Rw0·033). An improved procedure for the preparation of (1) in 35–40% yields is also described.

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.

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.

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.

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.

Aromatic aldonitrones of 2-(hydroxyamino)benzyl alcohol and their cyclic isomers. Crystal and molecular structures of a 1-hydroxy-1,2-dihydro-4H-3,1-benzoxazine, a boron chelate, and its parent nitrone ligand

1998 ◽  
Vol 76 (4) ◽  
pp. 389-399 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Jörg Metge ◽  
Steven J Rettig ◽  
James Trotter
Keyword(s):  
Least Squares ◽  
Benzyl Alcohol ◽  
Crystal Structures ◽  
Direct Methods ◽  
Molecular Structures ◽  
Full Matrix ◽  
Space Group ◽  
Crystal And Molecular Structures ◽  
Independent Molecules ◽  
Boron Chelate

The synthesis of a series of C-aryl-N-[2-(hydroxymethyl)phenyl]nitrones, 5 (that can also exist under certain conditions as isomeric 1-hydroxy-2-aryl-1,2-dihydro-4H-3,1-benzoxazines, 8), via 2-(hydroxyamino)benzyl alcohol, 4, and their subsequent reactions with oxybis(diphenylborane), (Ph2B)2O, leading to the 5-(arylmethylene)-7,7-diphenyl-6,8-dioxa- 5-azonia-7-borata-5H-6,7,8,9-tetrahydrobenzocyclo- heptenes 6 are described. Crystals of 1-hydroxy-2- (4-methoxyphenyl)- 1,2-dihydro-4H-3,1-benzoxazine, 8b, are monoclinic, a = 9.379(2), b = 10.699(2), c = 12.9392(7) Å, β = 99.916(2)°, Z = 4 (two independent molecules), space group Pa; those of C-[4-(dimethylamino)phenyl]-N-[(2-hydroxymethyl)phenyl]nitrone, 5c, are monoclinic, a = 7.687(1), b = 7.891(1), c = 11.5053(9) Å, β = 92.781(9)°, Z = 2, space group P21; and those of 5-[4-(dimethylamino)phenylmethylene]-7,7-diphenyl-6,8-dioxa-5-azonia-7-borata-5H-6,7,8,9- tetrahydro-benzocycloheptene, 6a, are monoclinic, a = 10.771(1), b = 13.1057(9), c = 16.8724(7) Å, β = 90.005(5)°, Z = 4, space group P21/n. The structures were solved by direct methods and refined by full-matrix least-squares procedures to R(F2) = 0.120 (Rw(F2) = 0.135) for all 3149 reflections (R(F) = 0.071, Rw(F) = 0.063 for 1500 reflections with I >3 σ (I)) for 8b and R(F) = 0.035 and 0.036 (Rw(F) = 0.031 and 0.038) for 1071 and 3594 reflections with I >3 σ (I), respectively, for 5c and 6a. Compound 8b is the first structurally characterized 1-hydroxy-1,2-dihydro-4H-3,1-benzoxazine derivative and 6a features a relatively rare seven-membered boron-containing heterocycle.Key words: C-aryl-N-[2-(hydroxymethyl)phenyl]nitrones, 1-hydroxy-2-aryl-1,2-dihydro-4H-3,1-benzoxazines, organoboron compounds, crystal structures

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)�.

Structural studies of organoboron compounds. XV. Crystal and molecular structures of (3-aminopropanolato)diphenylboron, (2-N,N-dimethylaminoethanolato)diphenylboron, and (2-N,N-dimethylaminoethanolato)diphenylboron – diphenylborinic acid (1:1)

1983 ◽  
Vol 61 (10) ◽  
pp. 2334-2340 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Least Squares ◽  
Boron Atom ◽  
Direct Methods ◽  
Molecular Structures ◽  
Structural Studies ◽  
Organoboron Compounds ◽  
Full Matrix ◽  
Space Group ◽  
Crystal And Molecular Structures

Crystals of (3-aminopropanolato)diphenylboron are monoclinic, a = 9.6717(13). b = 9.8867(6), c = 14.452(2) Å, β = 99.500(7)°, Z = 4, space group P21/n: those of (2-N,N-dimethylaminoethanolato)diphenylboron are monoclinic, a = 7.0721(4), b = 16.8829(4), c = 12.0975(8) Å, β = 97.875(3)°, Z = 4, space group Cc; and those of (2-N,N-dimethylaminoethanolato)diphenylboron – diphenylborinic acid (1:1) are monoclinic. a = 11.3231(10). b = 19.3190(12). c = 12.2451(11) Å, β = 109.321(4)°, Z = 4, space group P21/n. All three structures were solved by direct methods and were refined by full-matrix least-squares procedures to final R values of 0.038. 0.031, and 0.040 for 1522, 1649, and 2420 reflections with I ≥ 3σ(I) respectively. Each structure contains a tetrahedrally coordinated boron atom. The libration-corrected B—O, B—N, and mean B—C distances are: 1.481(2), 1.643(3), and 1.623(3) Å for (3-aminopropanolato)diphenylboron; 1.476(2), 1.691 (2), and 1.625(7) Å for (2-N,N-dimethylaminoethanolato)diphenylboron. The Ph2BOH molecule contains a trigonal-planar boron atom with B—O = 1.354(3) Å and mean B—C = 1.572(3) Å.

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