Tetraorganodichalcogenoimidodiphosphinato derivatives of dimethyltellurium(IV) compounds. Crystal structures of Me2Te[(SPPh2)2N]2, Me2TeCl[(SPPh2)2N], Me2TeI[(SPPh2)2N], and Me2TeCl[(OPPh2)(SPPh2)N]

1999 ◽  
Vol 77 (3) ◽  
pp. 356-366 ◽  
Author(s):  
John E Drake ◽  
Robert J Drake ◽  
Anca Silvestru ◽  
Jincai Yang
Keyword(s):  
Sulfur Atom ◽  
Lone Pair ◽  
Axial Position ◽  
Equatorial Position ◽  
X Ray Diffraction ◽  
Cell Parameters ◽  
Distorted Octahedral ◽  
Multinuclear Nmr Spectroscopy ◽  
Distorted Trigonal Bipyramid ◽  
Derivatives Of

Isolation of Me2Te[(SPPh2)2N]2, Me2Te[(OPPh2)(SPPh2)N]2, and the halo derivatives Me2TeX[(SPPh2)2N] and Me2TeX[(OPPh2)(SPPh2)N], where X = Cl, Br, I, was attempted. Four of these were characterized by single crystal X-ray diffraction, while the formation of the others was confirmed by multinuclear NMR spectroscopy. Me2Te[(SPPh2)2N]2, 1; P21/n (No. 14) with cell parameters a = 14.908(3) Å, b = 11.122(5) Å, c = 30.384(6) Å, β = 92.67(2)°, V = 5032(2) Å3, Z = 4, R = 0.0661, Rw = 0.0696. Me2TeCl[(SPPh2)2N], 2; P[Formula: see text] (No. 2) with cell parameters a = 10.553(2) Å, b = 15.512(2) Å, c = 8.769(3) Å, α = 103.19(2)°, β = 94.27(2)°, γ = 85.76(2)°, V = 1391.3(7) Å3, Z = 2, R = 0.0377, Rw = 0.0328. Me2TeI[(SPPh2)2N], 4; P[Formula: see text] (No. 2) with cell parameters a = 10.954(3) Å, b = 15.580(3) Å, c = 8.751(3) Å, α = 103.49(2)°, β = 93.11(3)°, γ = 87.33(2)°, V = 1449.3(7) Å3, Z = 2, R = 0.0586, Rw = 0.0613. Me2TeCl[(OPPh2)(SPPh2)N], 6; P21/c (No. 14) with cell parameters a = 10.441(9) Å, b = 13.672(10) Å, c = 19.521(9) Å, β = 97.16(6)°, V = 2764(3) Å3, Z = 4, R = 0.0546, Rw = 0.0572. The immediate environment about Te is that of a sawhorse structure in which the lone pair is apparently stereochemically active and occupying an equatorial position in a distorted trigonal bipyramid. In 1, 2, and 4, one sulfur atom of (SPPh2)2N occupies an axial position. If the second sulfur atom is included in the coordination sphere, then the environment about Te becomes distorted octahedral, for 1, and square pyramidal, for 2 and 4. By contrast, in Me2TeCl[(OPPh2)(SPPh2)N], 6, the oxygen atom, rather than sulfur, is bound to tellurium in the axial position, with the S atom, at best, having a very weak interaction with Te.Key words: structure, tellurium, methyl, tetraphenyldichalogenoimidodiphosphinates.

Dimethyltellurium(IV) derivatives with mixed 1,1-dithio ligands. Crystal structures of Me2Te[S2CNMe2][S2COEt] and Me2Te[S2CNEt2][S2COMe]

1999 ◽  
Vol 77 (7) ◽  
pp. 1262-1273 ◽  
Author(s):  
John E Drake ◽  
Layla N Khasrou ◽  
Anil G Mislankar ◽  
Raju Ratnani
Keyword(s):  
Lone Pair ◽  
Mixed Ligand ◽  
Equatorial Position ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
Secondary Interactions ◽  
Infrared And Raman Spectroscopy ◽  
Distorted Trigonal Bipyramid ◽  
Derivatives Of

Mixed ligand derivatives of Me2TeLL'2, where L = N,N-dialkyl dithiocarbamate or O,O-alkylene dithiophosphate and L' = O-alkyl dithiocarbonate, have been synthesized and characterized by elemental analysis, 1H, 13C, 31P, and 125Te NMR spectroscopy and infrared and Raman spectroscopy, and X-ray crystallography. Me2Te[S2CNMe2][S2COEt], 8: P[Formula: see text] (no. 2), with cell parameters a = 10.073(3) Å, b = 10.139(2) Å, c = 9.108(2) Å, α = 92.36(2)°, β = 115.55(2)°, γ = 111.19(2)°, V = 760.7(4) Å3, Z = 2, R = 0.0343, Rw = 0.0296. Me2Te[S2CNEt2][S2COMe], 9: P21/c (no. 14) with cell parameters a = 9.881(4) Å, b = 17.671(3) Å, c = 10.149(4) Å, β = 113.65(3)°, V = 1623.3(10) Å3, Z = 4, R = 0.0567, Rw = 0.0514. The immediate environment about tellurium in both molecules is essentially that of a saw-horse structure in which the lone pair is apparently stereochemically active and occupying an equatorial position in a distorted trigonal bipyramid. The S-Te-S angles in the two molecules are 166.87(6)° and 162.0(1)° for 8 and 9, respectively. In both molecules, the Te—S bonds to the dithiocarbamate groups are slightly shorter than those to dithiocarbonates. The dithiocarbamate groups are oriented to give secondary interactions involving the apparently terminal sulfur atoms resulting in Te—S distances of 3.205(2) and 3.277(4) Å, respectively, in 8 and 9. However, only in 9 is there a similar Te—S distance of 3.346(5) Å involving the S2COMe group because in 8, the OEt group of S2COEt, rather than the terminal S atom, is oriented toward Te. Key words: structure, tellurium, methyl, dithiocarbamates, dithiocarbonates, dithiophosphates.

Synthesis, spectroscopic and structural studies of O-methyl and O-isopropyl monothiocarbonate (monoxanthate) derivatives of dimethyl-and diphenyltellurium(IV). Crystal structures of Me2Te[SCO2(i-Pr)]2, Ph2Te[SCO2(i-Pr)]2, Me2TeCl[SCO2Me], and Me2TeBr[SCO2(i-Pr)]

1996 ◽  
Vol 74 (11) ◽  
pp. 1968-1982 ◽  
Author(s):  
John E. Drake ◽  
Robert J. Drake ◽  
Layla N. Khasrou ◽  
Anil G. Mislankar ◽  
Raju Ratnani ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Key Words ◽  
Lone Pair ◽  
Supramolecular Interactions ◽  
Equatorial Position ◽  
Structural Studies ◽  
Cell Parameters ◽  
Distorted Trigonal Bipyramid ◽  
Derivatives Of ◽  
Oxygen Atoms

Monothiocarbonate derivatives of diorganotellurium(IV), R2Te[SCO2R′]2, and R2TeX[SCO2R′], where R = Me, Ph; R′ = Me, i-Pr; X = Cl, Br, and I, have been prepared and characterized by vibrational and 1H, 13C, and 125Te NMR spectroscopy. Me2Te[SCO2(i-Pr)]2 (2): P21/n (No. 14) with cell parameters a = 6.942(6) Å, b = 25.599(3) Å, c = 9.404(6) Å, β = 94.48(6)°, V = 1666(1) Å3, Z = 4, R = 0.0648, Rw = 0.0624; Ph2Te[SCO2(i-Pr)]2 (4): P21/n (No. 14) with a = 12.360(4) Å, b = 12.277(3) Å, c = 15.066(3) Å, β = 102.82(2)°, V = 2229.1(9) Å3, Z = 4, R = 0.0368, Rw = 0.0312; Me2TeCl[SCO2Me] (5); P21/c (No. 14) with a = 5.193(2) Å, b = 18.118(4) Å, c = 9.613(5) Å, β = 91.31(6)°, V = 904.2(6) Å3, Z = 4, R = 0.0396, Rw = 0.0361; and Me2TeBr[SCO2(i-Pr)] (8): P21/n (No. 14) with a = 11.701(2) Å, b = 6.250(2) Å, c = 16.152(2) Å, β = 98.43(1)°, V = 1168.4(4) Å3, Z = 4, R = 0.0369, Rw = 0.0325. In all molecules, the immediate environment about tellurium is that of the saw-horse structure in which the lone pair is assumed to be stereochemically active and occupying an equatorial position in a distorted trigonal bipyramid. In 2 and 5, the terminal oxygen atoms are oriented toward tellurium, whereas in 4, one O(i-Pr) group is oriented toward tellurium, as it is in 8. In the latter cases, the terminal oxygen atoms act as weak bridges to form a pseudo dimeric species in 4 and a pseudo polymer in 8. Supramolecular interactions in 2 and 5 lead to a sulfur-bridged dimer in the former and a chlorine-bridged polymer in the latter. Key words: structure, tellurium, dimethyl, diphenyl, monothiocarbonates.

scholarly journals Über Verbindungen subvalenter Hauptgruppenmetallkationen mit Dithiolaten, 4. Mitteilung [1] Die Kristallstrukturen der Verbindungen Pb[S(CN)C=C(CN)S] und (AsPh4)2{Pb[S(CN)C=C(CN)S]2} / Compounds of Subvalent Main Group Metal Cations with Dithiolates, Part 4 [1] Crystal Structures of Pb[S(CN)C=C(CN)S] and (AsPh4)2{Pb[S(CN)C=C(CN)S]2}

1989 ◽  
Vol 44 (12) ◽  
pp. 1531-1537 ◽  
Author(s):  
Hans-Ulrich Hummel ◽  
Hermann Meske
Keyword(s):  
Crystal Structures ◽  
Complex Anion ◽  
Lone Pair ◽  
Equatorial Position ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Main Group Metal ◽  
Distorted Trigonal Bipyramid

The crystal structures of Pb[S(CN)C=C(CN)S] and (AsPh4)2{Pb[S(CN)C=C(CN)S]2} have been determined by X-ray diffraction. PbS2C4N2, crystallizes in the non-centrosymmetric space group P21 with a = 7.292(3), b = 7.420(3), c = 5.789(2) Å, β = 95.47(5)° and Ζ = 2. The lead atom is coordinated by three S atoms of dithioligands. The coordination sphere around Pb includes a stereochemically active lone-pair and is described as a distorted tetrahedron. (AsPh4)2[Pb(S2C4N2)2] crystallizes in the triclinic space group P1 with a = 17.205(3), b = 13.342(3), c = 12.059(2) Å, α = 106.15(7), β = 102.92(6), γ = 79.50(3)° and Z = 2. In the complex anion {Pb[S(CN)C=C(CN)S]2}2- the Pb-atom is located at a centre of a distorted trigonal bipyramid with a stereochemically active lone-pair in an equatorial position.

scholarly journals Synthesis and Crystal Structure of the Bioinorganic Complex [Sb(Hedta)]·2H2O

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Di Li ◽  
Guo-Qing Zhong
Keyword(s):  
Crystal Structure ◽  
Ethylenediaminetetraacetic Acid ◽  
Raw Materials ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Cell Parameters ◽  
Composition And Structure ◽  
Decomposition Processes ◽  
Distorted Trigonal Bipyramid

The antimony(III) complex [Sb(Hedta)]·2H2O was synthesized with ethylenediaminetetraacetic acid (H4edta) and antimonous oxide as main raw materials in aqueous solution. The composition and structure of the complex were characterized by elemental analysis, infrared spectra, single crystal X-ray diffraction, X-ray powder diffraction, thermogravimetry, and differential scanning calorimetry. The crystal structure of the antimony(III) complex belongs to orthorhombic system, space group Pna2(1), with cell parameters ofa=18.4823(18) Å,b=10.9408(12) Å,c=7.3671(5) Å,V=1489.7(2) Å3,Z=4, andDc=1.993 g cm−3. The Sb(III) ion is five-coordinated by two amido N atoms and three carboxyl O atoms from a single Hedta3−ligand, forming a distorted trigonal bipyramid geometry. The thermal decomposition processes of the complex include dehydration, oxidation, and pyrolysis of the ligand, and the last residue is Sb2O3at the temperature of 570°C.

The crystal structure of seeligerite, Pb3IO4Cl3, a rare Pb-I-oxychloride from the San Rafael mine, Sierra Gorda, Chile

2008 ◽  
Vol 72 (3) ◽  
pp. 771-783 ◽  
Author(s):  
L. Bindi ◽  
M. D. Welch ◽  
P. Bonazzi ◽  
G. Pratesi ◽  
S. Menchetti
Keyword(s):  
Crystal Structure ◽  
Lone Pair ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Coordination Polyhedra ◽  
X Ray ◽  
Cell Parameters ◽  
Square Planar ◽  
San Rafael ◽  
Cl Atoms

AbstractThe crystal structure of seeligerite, Pb3IO4Cl3, from the San Rafael mine, Sierra Gorda, Chile, was solved in the space group Cmm2, and refined to R = 3.07%. The unit-cell parameters are: a = 7.971(2), b = 7.976(2), c = 27.341(5) Å, V = 1738.3(6) Å3 and Z = 8. The crystal structure consists of a stacking sequence along [001] of square-net layers of O atoms and square-net layers of Cl atoms with Pb+ and I+ cations located in the voids of the packing. As is typical of cations with a stereoactive lone-pair of electrons, Pb2+ and I5+ adopt strongly-asymmetrical configurations. Pb2+ cations occur in a variety of coordination polyhedra, ranging from anticubes and monocapped anticubes to pyramidal ‘one-sided’ coordinations. I5+ is coordinated by a square of four oxygen atoms: I1 and I3 exhibit a ‘one-sided’ coordination, whereas I2 has square-planar coordination.The TEM investigation has revealed additional superlattice reflections (which were not registered by X-ray diffraction (XRD)) in the hk0 diffraction pattern of seeligerite based upon a 0.158 Å-1 square net, which can be interpreted as arising from a 20-cation super-sheet motif (12.6 Å x 12.6 Å), likely related to a further level of Pb-I order superimposed upon the 8-site motif identified by XRD.

scholarly journals Synthesis, Spectral and Thermal Studies, and Crystal Structure of cis-Bis(4-methylimidazole)bis(picolinato)copper(II) [Cu(pic)2(4-MeIm)2]

2006 ◽  
Vol 61 (10) ◽  
pp. 1217-1221 ◽  
Author(s):  
Zerrin Heren ◽  
Cem Keser ◽  
C. Cüneyt Ersanli ◽  
O. Zafer Yeşilel ◽  
Nazan Ocak
Keyword(s):  
Thermal Studies ◽  
X Ray Diffraction ◽  
Complex Molecules ◽  
Triclinic Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Distorted Octahedral ◽  
Ft Ir ◽  
In Cis ◽  
Hydrogen Bondings

The mixed-ligand picolinato (pic) complex of Cu(II) with 4-methylimidazole (4-MeIm), [Cu(pic)2(4-MeIm)2], was synthesized and characterized by elemental analysis, magnetic susceptibility, spectroscopic methods (UV/vis and FT-IR) and X-ray diffraction. In the slightly distorted octahedral cis-bis(4-methylimidazole)bis(picolinato)copper(II) complex, the pic ligands are coordinated to the Cu(II) ion as bidentate N,O-donors forming chelate rings. The 4-MeIm ligands are N-coordinated in cis positions. The complex crystallizes in the triclinic space group p̅1 with unit cell parameters a = 9.204(5), b = 9.498(5), c = 13.095(5) Å , α = 90.395(5), β = 101.687(5), γ = 112.291(5)° and Z = 2. Hydrogen bondings and C-H ··· π interactions occur between picolinato and methylimidazole ligands of neighboring complex molecules. The thermal decomposition of the complex is described.

scholarly journals Preparation and Structures of Ternary Copper(II) Complexes of ADP and ATP Models for Enzyme-Metal Ion-Nucleoside Polyphosphate Complexes

1982 ◽  
Vol 37 (7) ◽  
pp. 863-871 ◽  
Author(s):  
William S. Sheldrick
Keyword(s):  
Metal Ion ◽  
Basic Structure ◽  
Axial Position ◽  
Distorted Octahedral Geometry ◽  
X Ray Diffraction ◽  
Bidentate Coordination ◽  
X Ray ◽  
Ph Values ◽  
Distorted Octahedral ◽  
The Third Terminal

AbstractThe stable ternary copper(II) complexes of ATP and ADP, [Cu(H2ATP)(phen)]2 · 7 H2O (2) and [Cu4(HADP)2(bipy)4(H2O)2(NO3)2] · 2 NO3 (3), have been isolated from aqueous solution at respective pH values of 2.8 and 4.0. Their structures have been established by single crystal X-ray diffraction. Tridentate coordination of each of the Cu atoms by ono α-, one β- and one γ-phosphate O atom of one ATP molecule is observed in 2. The binding Oα atoms occupy axial positions in a distorted octahedral geometry at Cu and the Cu- Oα interactions are weak. The other axial position is occupied by a γ-phosphate O atom of the second ATP molecule, leading to a dimeric structure. The basic structure of 3 is similar with, in this case, bidentate coordination of each of the central Cu atoms by one α- and one β-phosphate O atom of ono ADP molecule. In this case, however, the third terminal β-phosphate O atoms each bind a further Cu atom. All four Cu atoms in 3 display square pyramidal coordination. The structures of 2 and 3 are stabilised by intramolecular stacking of adenine and phenanthroline/bipyridyl systems. The significance of these structures as models for enzyme-metal ion-nucleoside polyphosphate complexes is discussed.

(Se,O)-Koordinierte Komplexe niedervalenter Hauptgruppenmetalle: Die Kristallstruktur von Bis(N,N-Diethyl-N′-benzoylselenoureato)blei(II) / (S e,O)-Coordinated Complexes of Subvalent Main Group Metals: The Crystal Structure of Bis(N ,N -diethyl-N′-benzoylselenoureato)lead(II)

1994 ◽  
Vol 49 (12) ◽  
pp. 1615-1619 ◽  
Author(s):  
M. Schuster ◽  
W. Bensch
Keyword(s):  
Crystal Structure ◽  
Lone Pair ◽  
Polar Axis ◽  
Crystal Structure Analysis ◽  
Equatorial Position ◽  
Orthorhombic Space Group ◽  
Cell Parameters ◽  
Main Group Metals ◽  
Single Crystal Structure Analysis ◽  
Neighboring Molecule

Bis(N,N-diethyl-N′-benzoylselenoureato)lead(II) has been prepared and characterized by single-crystal structure analysis. Pb(C12H15N2OSe)2 crystallizes in the non-centrosymmetric orthorhombic space group Iba2. The cell parameters are a = 13.206(3), b = 20.542(4), c = 10.089(2) A and Z = 4. R = 0.025. The direction of the polar axis was determined unambig­ uously. Pb(II) is bidentally coordinated to two N,N-diethyl-N′-benzoylselenourea molecules. The coordination polyhedron is a distorted pseudo-trigonal bi-pyramid with one equatorial position occupied by an electron lone-pair. The Pb-Se and Pb-O bond lengths are 2.876(1) and 2.444(4) Å, respectively. In the crystal lattice, each Pb atom also shows interactions with two Se atoms of a neighboring molecule. The Pb-Se distance of that interaction is 3.643 Å.

Twofac-tricarbonylrhenium(I) azadipyrromethene (ADPM) complexes: ligand-substitution effect on crystal structure

2015 ◽  
Vol 71 (2) ◽  
pp. 122-127 ◽  
Author(s):  
Mihaela Cibian ◽  
André Bessette ◽  
Andrew O'Connor ◽  
Janaina G. Ferreira ◽  
Garry S. Hanan
Keyword(s):  
Crystal Packing ◽  
Solvent Molecule ◽  
Substitution Effect ◽  
Octahedral Geometry ◽  
Axial Position ◽  
Distorted Octahedral Geometry ◽  
Equatorial Position ◽  
Distorted Octahedral ◽  
Steric Factors ◽  
High Flexibility

The crystal structures offac-(acetonitrile-κN)(2-{[3,5-bis(4-methoxyphenyl)-2H-pyrrol-2-ylidene-κN1]amino}-3,5-bis(4-<!?tlsb=0.2pt>methoxyphenyl)-1H-pyrrol-1-ido-κN1)tricarbonylrhenium(I)–hexane–acetonitrile (2/1/2), [Re(C36H30N3O4)(CH3CN)(CO)3]·0.5C6H14·CH3CN, (2), andfac-(2-{[3,5-bis(4-methoxyphenyl)-2H-pyrrol-2-ylidene-κN1]amino}-3,5-bis(4-methoxyphenyl)-1H-pyrrol-1-ido-κN1)tricarbonyl(dimethyl sulfoxide-κO)rhenium(I), [Re(C36H30N3O4)(C2H6OS)(CO)3], (3), at 150 K are reported. Both complexes display a distorted octahedral geometry, with afac-Re(CO)3arrangement and one azadipyrromethene (ADPM) chelating ligand in the equatorial position. One solvent molecule completes the coordination sphere of the ReIcentre in the remaining axial position. The ADPM ligand shows high flexibility upon coordination, while retaining its π-delocalized nature. Bond length and angle analyses indicate that the differences in the geometry around the ReIcentre in (2) and (3), and those found in three reportedfac-Re(CO)3–ADPM complexes, are dictated mainly by steric factors and crystal packing. Both structures display intramolecular C—H...N hydrogen bonding. Intermolecular interactions of the Csp2—H...π and Csp2—H...O(carbonyl) types link the discrete monomers into extended chains.

Structure and Stability of a Linear Trinuclear Cobalt(II) Complex: Co3(PhCH=CHCO2)6(bpy)2

2008 ◽  
Vol 63 (2) ◽  
pp. 129-133 ◽  
Author(s):  
Xian-Wen Wang ◽  
Ying Chen ◽  
Jing-Zhong Chen ◽  
Jian-Hong Liu ◽  
Lei Han
Keyword(s):  
X Ray Diffraction ◽  
Linear Arrangement ◽  
Triclinic Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Hydrogen Bonding Interactions ◽  
Octahedral Environment ◽  
Carboxylate Groups ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral

A trinuclear cobalt(II) complex, [Co3(PhCH=CHCO2)6(bpy)2] (1) (bpy = 2,2-bipyridine), was synthesized and structurally characterized by single crystal X-ray diffraction. Complex 1 crystallizes in the triclinic space group P1 with cell parameters: a = 11.347(6), b = 11.471(6), c = 14.247(8) Å , α = 69.503(9), β = 74.211(9), γ = 76.812(11)°, V = 1653.2(15) Å3, Z = 1, and R1(F) = 0.026, wR2(F2) = 0.138. Complex 1 has a linear arrangement of three Co(II) centers bridged by six cinnamate carboxylate groups, four of which function in a bidentate syn-syn fashion linking the peripheral Co2 atoms, and two as both bidentate bridging and bidentate chelating units. The Co1 atom is located on a crystallographic inversion center and exhibits a slightly distorted octahedral coordination geometry, while the terminal Co atoms (Co2 and Co2#1) have a significantly distorted octahedral environment. Hydrogen bonding interactions and π-π stacking interactions stabilize the structure

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