Raman and far-infrared spectra of triphenyltin isochalcocyanates and their adducts with O- and N-donor ligands: the crystal and molecular structure of isocyanato-triphenyl (pyridine-N-oxide) tin

1987 ◽  
Vol 65 (3) ◽  
pp. 639-647 ◽  
Author(s):  
Ivor Wharf ◽  
Lars Piehler ◽  
Bruce M. Sailofsky ◽  
Mario Onyszchuk ◽  
Michel G. Simard
Keyword(s):  
Direct Method ◽  
Far Infrared ◽  
Triphenylphosphine Oxide ◽  
Donor Ligands ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Phenyl Rings ◽  
Distorted Trigonal Bipyramidal Coordination ◽  
Far Infrared Spectra ◽  
Distorted Trigonal Bipyramidal

Solid state infrared and Raman data (350–100 cm−1) are reported for Ph3SnNCY (Y = O, S, Se) and their 1:1 adducts with hexamethylphosphoramide (HMPA), pyridine-N-oxide (pyO), 4-picoline-N-oxide (4-picO), triphenylphosphine oxide (Ph3PO), and pyridine (py), as well as for Ph3SnNCSe•L where L = β-pic (β-picoline) or γ-pic (γ-picoline), and assignments are given. The crystal structure of Ph3SnNCO•pyO was determined by single crystal X-ray analysis. The compound crystallizes in space group Pbca with a = 14.443(3), b = 16.676(4), c = 17.523(6) Å (−110 °C); Z = 8. The structure was solved by the direct method and refined by full-matrix least-squares methods to R = 0.024 for 2086 observed reflections. The tin atom has distorted trigonal bipyramidal coordination with the isocyanate group and pyridine-N-oxide at the apices of the bipyramid and phenyl rings in the equatorial positions. Changes in v(Sn—NCY) on adduct formation are correlated with either increased coordination at tin (Y = O) or breaking of strong chalcocyanate bridges with tin remaining five-coordinate (Y = S, Se).

scholarly journals Five-Coordinated Geometries from Molecular Structures to Solutions in Copper(II) Complexes Generated from Polydentate-N-Donor Ligands and Pseudohalides

Molecules ◽  
2020 ◽  
Vol 25 (15) ◽  
pp. 3376 ◽  
Author(s):  
Franz A. Mautner ◽  
Roland C. Fischer ◽  
Ana Torvisco ◽  
Maher M. Henary ◽  
Febee R. Louka ◽  
...  
Keyword(s):  
Structural Parameters ◽  
Molecular Structures ◽  
Donor Ligands ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Vis Spectroscopy ◽  
Amine Ligands ◽  
Ethyl Amine ◽  
Chelate Ring Size ◽  
Distorted Trigonal Bipyramidal

A novel series of mononuclear five-coordinated pseudohalido-Cu(II) complexes displaying distorted square bipyramidal: [Cu(L1)(NCS)2] (1), [Cu(L2)(NCS)2] (2) and [Cu(L3)(NCS)]ClO4 (5) as well as distorted trigonal bipyramidal: [Cu(isp3tren)(N3)]ClO4 (3), [Cu(isp3tren)(dca)]ClO4 (4) and [Cu(tedmpza)(dca)]ClO4·0.67H2O (6) geometries had been synthesized and structurally characterized using X-ray single crystal crystallography, elemental microanalysis, IR and UV-vis spectroscopy, and molar conductivity measurements. Different N-donor amine skeletons including tridentate: L1 = [(2-pyridyl)-2-ethyl)-(3,4-dimethoxy)-2-methylpyridyl]methylamine and L2 = [(2-pyridyl)-2-ethyl)-(3,5-dimethyl-4-methoxy)-2-methyl-pyridyl]methylamine, and tetradentate: L3 = bis(2-ethyl-di(3,5-dimethyl-1H-pyrazol-1-yl)-[2-(3,4-dimethoxy-pyridylmethyl)]amine, tedmpza = tris[(2-(3,5-dimethyl-1H-pyrazol-1-yl)ethyl]amine and isp3tren = tris[(2-isopropylamino)ethyl)]amine ligands were employed. Molecular structural parameters such as nature of coligand, its chelate ring size and steric environment incorporated into its skeleton, which lead to adopting one of the two limiting geometries in these complexes and other reported compounds are analyzed and correlated to their assigned geometries in solutions. Similar analysis were extended to other five-coordinated halido-Cu(II) complexes.

scholarly journals Synthesis and Structure Features of Tetraphenylantimony 2,3-Difluoro- and 2,3,4,5,6-Pentafluorobenzoate

2020 ◽  
Vol 12 (4) ◽  
pp. 51-62
Author(s):  
A. Efremov ◽  
Keyword(s):  
Diffraction Analysis ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Trigonal Bipyramidal ◽  
Cambridge Crystallographic Data Center ◽  
Redistribution Reaction ◽  
Distorted Trigonal Bipyramidal Coordination ◽  
Distorted Trigonal Bipyramidal

Tetraphenylantimony 2,3-difluorobenzoate (1) and tetraphenylantimony 2,3,4,5,6-pentafluorobenzoate (2) was obtained by the interaction of pentaphenylantimony with 2,3-difluorobenzoic and 2,3,4,5,6-pentafluorobenzoic acids in benzene with a yield of up to 98 %. The compounds were also synthesized by the ligand redistribution reaction between pentaphenylantimony and triphenylantimony dicarboxylates. The compounds have been identified by IR spectroscopy and X-ray diffraction analysis. According to the X-ray diffraction data, the antimony atoms in compounds 1 and 2 have a distorted trigonal-bipyramidal coordination with the oxygen atom in axial positions. X-ray diffraction analysis was performed on a D8 QUEST diffractometer (Bruker). The crystallographic parameters of the unit cell of the compounds: 1 space group Р1 ̅, а = 9.857(5), b = 10.154(7), c = 14.362(11) Å, α = 83.74(4)°, β = 82.59(3), γ = 68.34(2)°, V = 1321.9(16) Å3, ρcalc = 1.475 g/cm3, Z = 2; 2 space group Р21/с, а = 16.186(9), b = 8.771(6), c = 20.413(13) Å, α = 90.00°, β = 113.073(17), γ = 90.00°, V = 2666(3) Å3, ρcalc = 1.597 g/cm3, Z = 4. The OSbO axial angles are slightly different and amount to 177.90(5)º in 1 and 179.00(5)º in 2. The sums of the CSbC equatorial angles are 356.89(9)º (1), 355.85(7)º (2). The Sb–Ceq distances in compounds 1 and 2 are 2.116(2), 2.119(2), 2.118(2) and 2.1073(17), 2.1158(18), 2.1152(19) Å respectively, which are significantly shorter than the Sb–Сax bond lengths (2.169(2) and 2.1617(19) Å). The organization of molecules in the crystals of compounds is due to hydrogen bonds and CHπ-interactions of the aryl and carboxyl ligands. The main difference between structures 1 and 2 is the different Sb–O bond lengths (2.2864(18) and 2.3168(18) Å), which is due to an increase in the electronegativity of the carboxyl ligand in 2, caused by the presence of five electronegative fluorine atoms in the benzoate substituent. Complete tables of atom coordinates, bond lengths and valence angles are deposited at the Cambridge Crystallographic Data Center (No. 1980908 (1); 1977189 (2); [email protected]; http://www.ccdc.cam.ac.uk/data_request/cif).

Thiophenophane metal complexes. III. Preparation, X-ray structure, and properties of 2,5,7,10-tetrathia[12] (2, 5) thiophenophane, L, and [Ag2L2]2+, its dinuclear silver complex cation

1990 ◽  
Vol 68 (4) ◽  
pp. 644-649 ◽  
Author(s):  
C. Robert Lucas ◽  
Shuang Liu ◽  
Michael J. Newlands ◽  
Jean-Pierre Charland ◽  
Eric J. Gabe
Keyword(s):  
Mass Spectra ◽  
Fast Atom Bombardment ◽  
Complex Cation ◽  
Ligand Molecule ◽  
Space Group ◽  
X Ray ◽  
H Nmr ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal Coordination ◽  
Distorted Trigonal Bipyramidal

Preparations of the thiophenophane C12H18S5(L3), and its binuclear silver(I) complex cation [Ag2(L3)2]2+ are described. The 13C and 1H nmr spectra of L3 and the ir and fast atom bombardment mass spectra of the complex are reported. X-ray structures of L3 and [Ag2(L3)2](ClO4)2 have been determined. For L3: space group P21/n, a = 10.8866(2), b = 9.4419(4), c = 14.9608(2) Å, β = 97.132(1)°, Z = 4, Rf = 0.057, Rw = 0.045. For [Ag2(L3)2] [ClO4]2: space group P21/n,a = 9.2717(3), b = 19.8697(2), c = 10.2654(4) Å, β = 100.592(2)°, Z = 2, Rf = 0.036, Rw = 0.030. The effect of structure on the ligand's ability to form complexes is discussed. The centrosymmetric dinuclear cation has slightly distorted trigonal bipyramidal coordination geometry about each silver. The silver atoms are linked by one bridging thioether sulfur from each ligand. The remaining three sites on each silver are occupied by two terminal thioether sulfurs from one ligand molecule and one from the other ligand molecule. The complex is remarkably stable photochemically and chemically but under certain specific conditions reacts with loss of ligand. This stability is discussed with respect to structure. Keywords: binuclear silver(I) thiophenophane complex.

The synthesis, and molecular and crystal structure of diphenyl(2-oxidonaphthylmethyl-iminoacetato)tin(IV)

1996 ◽  
Vol 74 (11) ◽  
pp. 2041-2047 ◽  
Author(s):  
Frank. E. Smith ◽  
Lian Ee Khoo ◽  
Ngoh Khang Goh ◽  
Rosemary C. Hynes ◽  
George Eng
Keyword(s):  
Crystal Structure ◽  
Elemental Analysis ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Trigonal Bipyramidal ◽  
Intermolecular Contacts ◽  
Distorted Trigonal Bipyramidal Coordination ◽  
Distorted Trigonal Bipyramidal

The new diorganotin complex ((C6H5)2Sn(OC10H6CH=NCH2COO)) was prepared and characterized by 1H NMR, IR, elemental analysis, and a single crystal X-ray diffraction study. The crystals are monoclinic, space group P21/a with a = 16.9167(9) Å, b = 19.1276(16) Å, c = 26.538(2) Å, β = 100.534(6)°, V = 8442.5(11) Å3, Z = 16, and Dcalc = 1.574 Mg m−3. The final discrepancy factors are RF = 0.030, and RW = 0.021 for 6524 significant reflections. The tin atom has a distorted trigonal bipyramidal coordination, with no short intermolecular contacts. The two axial Sn—O bonds of 2.12 Å and 2.09 Å and the equatorial Sn—N bond of 2.14 Å are among the shortest found in related complexes. Key words: diorganotin(IV), bicycloazastannoxide, trigonal bipyramidal, antitumour.

Simple Synthesis, Characterization and Structure of Diorganotin(IV) Complexes Containing the N-(2-Salicylidene)-N'-benzoylhydrazone Ligand

2003 ◽  
Vol 58 (4) ◽  
pp. 336-344 ◽  
Author(s):  
Dilip Kumar Dey ◽  
Brajagopal Samanta ◽  
Antonin Lycka ◽  
Lutz Dahlenburg
Keyword(s):  
Schiff Base ◽  
Nitrogen Atom ◽  
Elemental Analysis ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal Coordination ◽  
Distorted Trigonal Bipyramidal

Two diorganotin(IV) complexes of general formula R2Sn[2-OC6H4CH=NDN=C(O)Ph] (R = Ph, 1; R = Me, 2) have been synthesized from the corresponding diorganotin(IV) dichloride and the Schiff base derived from salicylaldehyde and benzoyl hydrazide. The two compounds have been characterized by elemental analysis, IR and NMR (1H, 13C, 15N, 119Sn) spectra, and their structures have been confirmed by single crystal X-ray structure analysis. Crystals of complex 1 re triclinic, space group P1̄ , a = 11.1631(5), b = 13.462(2), c = 16.511(1) Å , α = 106.193(9), β = 106.379(8), γ = 94.932(8)°, Z = 4, R1 = 0.0461, wR2 = 0.0939 for 13194 unique reflections. Crystals of 2 are monoclinic, space group P21, a = 10.2073(5), b = 14.645(2), c = 10.411(3) Å, β = 92.572(9)°, Z = 4, R1 = 0.0395, wR2 = 0.0835 for 5050 unique reflections. The central tin atom of either complex adopts a distorted trigonal bipyramidal coordination with two ligand oxygen atoms in axial positions, the nitrogen atom of the ligand and two organic groups on tin occupying equatorial sites. The δ(119Sn) values for the complexes 1 and 2 are -329.2 and -150.3, respectively, thus indicating penta-coordinated tin centres.

Synthesis and Characterization of Cadmium and Mercury Saccharinate Complexes with 2-Dimethylaminoethanol: cis-[Cd(sac)2(dmea)2] and [Hg(sac)2(dmea)(H2O)]

2006 ◽  
Vol 61 (5) ◽  
pp. 555-559 ◽  
Author(s):  
Veysel T. Yilmaz ◽  
Vecdi Kars ◽  
Canan Kazak
Keyword(s):  
Three Dimensional ◽  
Carbonyl Oxygen ◽  
Supramolecular Network ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Octahedral ◽  
Distorted Trigonal Bipyramidal Coordination ◽  
Distorted Trigonal Bipyramidal

The new cadmium and mercury saccharinate (sac) complexes, cis-[Cd(sac)2(dmea)2] (1) and [Hg(sac)2(dmea)(H2O)] (2) (dmea = 2-dimethylaminoethanol), have been prepared and characterized by elemental analysis, IR spectroscopy, thermal analysis and single crystal X-ray diffraction. In complex 1, the cadmium(II) ion is coordinated by two neutral dmea ligands and two sac anions in a distorted octahedral CdN3O3 coordination geometry. The dmea ligand acts as a bidentate N, O chelate, while the sac ligands behave as an ambidentate ligands. One of them coordinates to the cadmium(II) ion through the carbonyl oxygen atom, while the other is N-bonded. In complex 2, the mercury(II) ion is coordinated by an aqua ligand, a chelating dmea ligand and two N-bonded sac ligands, forming a distorted trigonal bipyramidal coordination HgN3O2. The molecules interact with each other through O-H···O hydrogen bonds and aromatic π(sac)···π(sac) stacking interactions, leading to a three-dimensional supramolecular network.

The synthesis and structural characterization of a series of pentacoordinate diorganotin(IV) N-arylidene-α-amino acid complexes

1992 ◽  
Vol 70 (4) ◽  
pp. 1114-1120 ◽  
Author(s):  
F. E. Smith ◽  
Rosemary C. Hynes ◽  
T. T. Ang ◽  
L. E. Khoo ◽  
G. Eng
Keyword(s):  
Molecular Structure ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Intermolecular Contacts ◽  
Distorted Trigonal Bipyramidal Coordination ◽  
C Nmr ◽  
Distorted Trigonal Bipyramidal

Eight new diorganotin complexes formulated as R2Sn(OArCR″=NCHR′COO) were prepared and characterized by 1H and 13 C NMR, IR, and elemental analysis. A single crystal X-ray diffraction study of the dibutyltin N-salicylidenevaline complex, Bu2Sn(OC6H4CH=NCH(i-Pr)COO), determines the molecular structure. The crystals are orthorhombic, space group P212121 with a = 9.187(2) Å, b = 10.003(2) Å, c = 23.482(4) Å, V = 2157.8(6) Å3, Z = 4, and Dc = 1.392 g cm−3. The final discrepancy factors are RF = 0.040, and Rw = 0.021 for 1131 significant reflections. The tin atom has a distorted trigonal bipyramidal coordination, with no short intermolecular contacts. The two axial Sn—O bonds of 2.078(10) and 2.151(8) Å and the equatorial Sn—N bond of 2.158(8) Å are among the shortest found in related complexes. The fact that the closest intermolecular Sn—O distance is 4.511(8) Å indicates a nonbridging carbonyl group.

Xenon Trioxide Adducts of O-Donor Ligands; [(CH3)2CO]3XeO3, [(CH3)2SO]3(XeO3)2, (C5H5NO)3(XeO3)2, and [(C6H5)3PO]2XeO3

2018 ◽  
Author(s):  
Katherine Marczenko ◽  
James Goettel ◽  
Gary Schrobilgen
Keyword(s):  
Room Temperature ◽  
Triphenylphosphine Oxide ◽  
Donor Ligands ◽  
Mechanical Shock ◽  
X Ray Diffraction ◽  
X Ray ◽  
Oxygen Coordination ◽  
Xenon Trioxide ◽  
Distorted Octahedra ◽  
Coordination Spheres

Oxygen coordination to the Xe(VI) atom of XeO<sub>3</sub> was observed in its adducts with triphenylphosphine oxide, dimethylsulfoxide, pyridine-N-oxide, and acetone. The crystalline adducts were characterized by low-temperature, single-crystal X-ray diffraction and Raman spectroscopy. Unlike solid XeO<sub>3</sub>, which detonates when mechanically or thermally shocked, the solid [(C<sub>6</sub>H<sub>5</sub>)<sub>3</sub>PO]<sub>2</sub>XeO<sub>3</sub>, [(CH<sub>3</sub>)<sub>2</sub>SO]<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub>,<sub> </sub>and (C<sub>5</sub>H<sub>5</sub>NO)<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub> adducts are insensitive to mechanical shock, but undergo rapid deflagration when ignited by a flame. Both [(C<sub>6</sub>H<sub>5</sub>)<sub>3</sub>PO]<sub>2</sub>XeO<sub>3 </sub>and (C<sub>5</sub>H<sub>5</sub>NO)<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub> are air-stable whereas [(CH<sub>3</sub>)<sub>2</sub>SO]<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub> slowly decomposes over several days and [(CH<sub>3</sub>)<sub>2</sub>CO]<sub>3</sub>XeO<sub>3</sub> undergoes adduct dissociation at room temperature. The xenon coordination sphere of [(C<sub>6</sub>H<sub>5</sub>)<sub>3</sub>PO]<sub>2</sub>XeO<sub>3</sub> is a distorted square pyramid which provides the first example of a five-coordinate XeO<sub>3</sub> adduct. The xenon coordination spheres of the remaining adducts are distorted octahedra comprised of three Xe---O secondary contacts that are approximately trans to the primary Xe–O bonds of XeO<sub>3</sub>. Quantum-chemical calculations were used to assess the Xe---O adduct bonds, which are predominantly electrostatic σ-hole bonds between the nucleophilic oxygen atoms of the bases and the σ-holes of the xenon atoms.

Crystal and molecular structure of diorganoammonium oxalatotrimethylstannate, [R2NH2][Me3Sn(C2O4)] (R=i-Bu, cyclohexyl)

2011 ◽  
Vol 34 (5-6) ◽  
pp. 127-130 ◽  
Author(s):  
Yaya Sow ◽  
Libasse Diop ◽  
Kieran C. Molloy ◽  
Gabrielle Kociok-Köhn
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Diffraction Study ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Trans Complex ◽  
A Chain ◽  
Distorted Trigonal Bipyramidal

Abstract The title compounds [R2NH2][C2O4SnMe3](R=i-Bu, Cy), in which tin atoms adopt a distorted trigonal bipyramidal configuration, have been prepared and submitted to an X-ray diffraction study. These compounds have been obtained from the reaction of (Cy2NH2)2C2O4·H2O or (i-Bu2NH2)2C2O4 with SnMe3Cl. In both [R2NH2][C2O4SnMe3] compounds, the trans complex has an almost regular trigonal bipyramidal geometry around the tin atom. The SnMe3 residues are connected as a chain with bridging oxalate anions in a trans-SnC3O2 framework, the oxygen atoms being in axial positions. The cations connect linear adjacent chains through NH…O hydrogen bonds giving layered structures.

Chloridobis(1,10-phenanthroline-κ2 N,N′)copper(I) hexahydrate

2007 ◽  
Vol 63 (3) ◽  
pp. m826-m828 ◽  
Author(s):  
H. Zhong ◽  
X.-R. Zeng ◽  
X.-M. Yang ◽  
Q.-Y. Luo ◽  
S.-Z. Xiao
Keyword(s):  
Three Dimensional ◽  
Water Molecules ◽  
Stacking Interactions ◽  
Coordination Geometry ◽  
Rotation Axes ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal Coordination ◽  
Cl Atom ◽  
Phenanthroline Ligands ◽  
Distorted Trigonal Bipyramidal

The CuI atom in the title complex, [CuCl(C12H8N2)2]·6H2O, exists in a distorted trigonal-bipyramidal coordination geometry defined by one Cl atom and four N atoms of two 1,10-phenanthroline ligands. In the crystal structure, molecules are linked into a three-dimensional framework by O—H...O hydrogen bonds and π–π stacking interactions. Four water molecules lie on crystallographic twofold rotation axes.

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