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).

Darstellung und Kristallstruktur von Zinkazid · 4-Methylpyridin / Preparation and Crystal Structure of Zinc Azide · 4-Methylpyridine

1988 ◽  
Vol 43 (3) ◽  
pp. 253-256 ◽  
Author(s):  
Franz A. Mautner ◽  
Harald Krischner ◽  
Christoph Kratky
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Single Crystal ◽  
Zinc Atom ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

Zinc azide · 4-methylpyridine (1) is formed by the reaction of zinc azide with the corresponding pyridine in aqueous solution. The crystal structure was determined by single crystal X-ray diffraction methods. The crystals of 1 are monoclinic, space group C2/c, Z = 4, a = 1085.5(2), b = 1692.7(11), c = 619.7(6) pm, β = 113.47(5)°. Each zinc atom is surrounded by five nitrogen atoms (four from azide groups and one from the pyridine adduct) in a distorted trigonal bipyramidal fashion. The ZnN5-polyhedra share common edges to form chains along the crystallographic c-axis.

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.

Reaktion der Alkoxo-oxovanadium(V)-dichloride mit Bis(tert-butylamino)-dimethylsilan/ Reaction of Alkoxo Oxovanadium(V) Dichlorides with Bis(tert-butylamino) Dimethylsilane

1985 ◽  
Vol 40 (8) ◽  
pp. 1040-1044 ◽  
Author(s):  
Fritz Preuss ◽  
Edith Fuchslocher ◽  
William S. Sheldrick
Keyword(s):  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
Vanadium Complex ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

AbstractThe iminovanadium (V) com pounds tC4H9N = V(NtC4H9-SiMe2-NHtC4H9)Cl2 (3) and [VCl(μ-Cl)(NtC4H9)(NHtC4H9)(NH2tC4H9)]2 have been prepared by reaction of Me2Si(NHtC4H9)2 with VO(OC2H5)Cl2 and VO(O tC3H7)Cl2, respectively. 3 was investigated by 1H , 51V NMR spectroscopy and X-ray diffraction analysis; the structure has been found to be a mononuclear vanadium complex with a distorted trigonal bipyramidal arrangement of the ligands.

Tris(tert-butoxo)silylthiolato-Komplexe des Vanadiums(V, IV, III) / Tris(tert-butoxo)silylthiolato Complexes of Vanadium(V, IV, III)

1990 ◽  
Vol 45 (12) ◽  
pp. 1618-1624 ◽  
Author(s):  
Fritz Preuss ◽  
Martina Steidel ◽  
Reiner Exner
Keyword(s):  
Diffraction Analysis ◽  
Esr Spectroscopy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Thiolate Ligands ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

The complexes ′C4H9N = V(O′C4H9)3-n[SSi(O′C4H9)3]n, O = V(O′C4H9)3-n[SSi(O′C4H9)3]n, O=V[SSi(O′C4H9)3]2 (9) and VCl[SSi(O′C4H9)3]2 have been prepared by reaction of chlorovanadium compounds with LiSSi(O′C4H9)3. All complexes are characterized by NMR (1H, 51V) and ESR spectroscopy. 9 has been found by X-ray diffraction analysis to be a distorted trigonal bipyramidal complex with bidentate thiolate ligands.

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.

Iodomanganate(II): Darstellung und Kristallstrukturen von (Ph4P)MnI3L, MnI2 L3, [MnIL5]I3 und [MnL6](I3)2 (L = Tetrahydrofuran) / Iodomanganates(II): Synthesis and Crystal Structures of (Ph4P)MnI3L, MnI2L3, [MnIL5]I3 and [MnL6](I3)2

1988 ◽  
Vol 43 (2) ◽  
pp. 175-181 ◽  
Author(s):  
Peter Stolz ◽  
Siegfried Pohl
Keyword(s):  
Characteristic Feature ◽  
Single Crystal ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

The compounds (Ph4P)MnI3L (1), MnI2L3 (2), [MnIL5]I3 (3), and [MnL6](I3)2 (4) (L = C4 H8O, thf) were prepared in thf solution and their structures determined from single crystal X-ray diffraction data. 1 crystallizes in the monoclinic space group C2/c with a = 1743.6(1), b = 1985.8(1), c = 1806.7(1) pm, β = 98.74(1)°, Z = 8. The structure of 1 exhibits tetrahedral anions. The Mn-I distance was found to be 268.0 pm (mean). 2: monoclinic, C2/c with a = 1252.3(2), b = 1255.0(3), c = 1271.8(3) pm β = 113.88(2)°, Z = 4. The characteristic feature of the structure of 2 is the existence of neutral MnI2L3 molecules with a distorted trigonal bipyramidal geometry and the iodine atoms in equatorial positions (Mn-I: 271.1 pm). The compound crystallizes from a solution of Mnl2 in tetrahydrofuran. 3: monoclinic, C2/c with a = 1695.3(1), b = 1123.1(1), c = 1646.2(1̱) pm, β = 96.91(1)°, Z = 4. The preparation of 3 from 2 and iodine yields octahedral MnIL+5 cations (Mn-I: 278.8̄ pm) and triiodide anions. 4: monoclinic, P21/n with a = 1005.5(1). b = 1056.8(1), c =1835.6(2) pm, β = 91.16(1)°, Z = 2. 4 is prepared from 3 and iodine in thf solution, and shows octahedral MnL62+ cations and triiodide anions

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.

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.

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