Synthesis and characterization of dimethyl- and dimethoxyphenylbis(N,N-dialkyldithiocarbamato)tellurium(IV) and chlorodimethyl- and chlorodimethoxyphenyl-(N,N-dialkyldithiocarbamato)tellurium(IV). Crystal structures of Me2Te[S2CNMe2]2 and (p-MeOC6H4)2Te[S2CNMe2]2

1993 ◽  
Vol 71 (1) ◽  
pp. 42-50 ◽  
Author(s):  
Jane H. E. Bailey ◽  
John E. Drake
Keyword(s):  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Variable Temperature ◽  
Reductive Elimination ◽  
Synthesis And Characterization ◽  
Space Group ◽  
Cell Parameters

The compounds Me2Te[S2CNR2]2, Me2TeCl[S2CNR2], (p-MeOC6H4)2Te[S2CNR2]2, and (p-MeOC6H4)2TeCl[S2CNR2], where R = Me, Et, have been prepared and characterised primarily by vibrational and NMR spectroscopy. Variable temperature NMR spectroscopy and qualitative time studies indicate that in solution the dimethoxyphenyltellurium derivatives undergo the reductive-elimination noted for analogous phenyl derivatives but the reductive-elimination does not occur with the dimethyl tellurium derivatives. The crystal structures of Me2Te[S2CNMe2]2, 1, and (p-MeOC6H4)2-Te[S2CNMe2]2, 5, were completed. The cell parameters for 1, which crystallizes as monoclinic in space group P21/n, are a = 13.550(2), b = 13.034(2), c = 17.854(2) Å, β = 106.61(1)°, V = 3021.6(7) Å3, Z = 8, R = 0.0368, and Rw = 0.0402 and for 5, which crystallizes as monoclinic in space group C2/c, are a = 35.36(1), b = 11.063(3), c = 12.778(3) Å, β = 96.16(3)°, V = 4963(3) Å3, Z = 8, R = 0.0627, and Rw = 0.0646.

Synthesis, spectroscopic characterization, and structural studies of organogermanium tri- and monothiocarbonates. Crystal structures of Me2Ge[S2CSEt]2, Ph3Ge[SCO2Me], Ph3Ge[SCO2(i-Pr)], and Ph2Ge[SCO2Me]2

1998 ◽  
Vol 76 (3) ◽  
pp. 319-334 ◽  
Author(s):  
John E Drake ◽  
Jincai Yang
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Sodium Salt ◽  
Variable Temperature ◽  
Spectroscopic Characterization ◽  
Structural Studies ◽  
Cell Parameters ◽  
Derivatives Of ◽  
C Nmr

Two series of S-alkyl trithiocarbonate derivatives of imethylgermane, Me2Ge[S2CSR]2, and halodiphenylgermane, Ph2GeX[S2CSR], where R = Me, i-Pr, n-Pr, n-Bu and X = Cl, Br, and three series of O-alkyl monothiocarbonate derivatives of triphenylgermane, Ph3Ge[SCO2R], diphenylgermane, Ph2Ge[SCO2R], and trimethylgermane, me3Ge[SCO2R], where R = Me, i-Pr, and n-Pr, have been prepared in 73-92% yields by the reaction of the potassium or sodium salt of the appropriate tri- or monothiocarbonic acid with dichlorodimethyl-, chlorotriphenyl-, dichlorodiphenyl-, and chlorotrimethylgermane. The compounds were principally characterized by infrared, Raman, and 1H and 13C NMR spectroscopy, including some variable temperature studies, as well as by mass spectrometry. Me2Ge[S2CSEt]2, 1: P21/m (No. 11) with cell parameters a = 6.647(4) Å, b = 7.423(2) Å, c = 16.290(4) Å, β = 91.07(3)°, V = 803.6(4) Å3, Z = 2, R = 0.0484,Rw = 0.0485. Ph3Ge[SCO2Me],13: P1bar (No. 2) with cell parameters a = 9.970(4) Å, b = 10.660(3) Å, c = 9.853(2) Å, α = 101.78(2)°, β = 109.98(2)°, γ = 89.76(3)°, V = 961.0(5) Å3, Z = 2, R = 0.0534, Rw = 0.0451. Ph3Ge[SCO2(i-Pr)], 14: P 1bar (No. 2) with cell parameters a = 14.386(7) Å, b = 18.598(6) Å, c = 9.223(3) Å, α = 102.85(3)°, β = 94.58(3)°, γ = 108.13(3)°, V = 2256(1) Å3, Z = 2, R = 0.0545, Rw = 0.0552. Ph2Ge[SCO2Me]2, 16: Cc, (No. 9) with cell parameters a = 11.790(4) Å, b = 13.696(5) Å, c = 23.232(6) Å, β = 92.26(3)°, V = 3748(2) Å3, Z = 8, R = 0.0563, Rw = 0.0512. The immediate environment about Ge is that of tetrahedral but the orientations of the thiocarbonate groups display interesting features.Key words: structure, germanium, phenyl, methyl, thiocarbonates.

Iridium(I) complexes containing bidentate pyrazolylgallate ligands. X-ray crystal structures of [Me2Gapz2]Ir(COD), [Ir(μ-pz)(CO)2]2, and [Ir(μ-3,5-Me2pz)(CO)2]2

1985 ◽  
Vol 63 (3) ◽  
pp. 692-702 ◽  
Author(s):  
Sophia Nussbaum ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Crystal Structures ◽  
Variable Temperature ◽  
Hydrogenation Reaction ◽  
Synthesis And Characterization ◽  
Nmr Studies ◽  
X Ray ◽  
H Nmr ◽  
Measurable Activity

The synthesis and characterization of a number of Ir(I) complexes incorporating bidentate, chelating, pyrazolylgallate ligands are described. Non-rigidity for some of the complexes in solution has been demonstrated by variable temperature 1H nmr studies. Crystal structures of three complexes, [Me2Gapz2]Ir(COD), [Ir(μ-pz)(CO)2]2, and [Ir(μ-3,5-Me2pz)(CO)2]2 are reported and confirm the expected boat conformations for the six-membered M—(N—N)2—Ir rings (where M = Ir or Ga) in the compounds. One of the complexes studied has exhibited measurable activity as a catalyst in the hydrogenation reaction of cyclohexene.

Solvothermal Synthesis and Characterization of Two Iron Complexes

2011 ◽  
Vol 492 ◽  
pp. 324-327
Author(s):  
Ya Wei Hu ◽  
Yang Min Ma
Keyword(s):  
Solvothermal Synthesis ◽  
Layer Structure ◽  
Iron Complexes ◽  
Synthesis And Characterization ◽  
Molecular Architecture ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

Two iron complexes, Fe3(dtdb)2(HCO2)2(DMF)2(H2O)2(1) and Fe(bpy)(Hdtdb)(H2O) (2) were solvothermally synthesized and characterized by single crystal X-ray diffraction. Fe3(dtdb)2(HCO2)2(DMF)2(H2O)2 (1) shows 2D layer structure crystallized in a triclinic with space group P-1 and cell parameters, a = 8.5591(10) nm, b = 11.2502(13) nm, c = 11.4370(14) nm, α = 90.687(2)º, β = 110.275(2)º , γ = 90.712(2)º, and Z = 1. Fe(bpy)(Hdtdb)(H2O) (2) shows surper- molecular architecture crystallized in a triclinic with space group P-1 and cell parameters, a = 8.286(12) nm, b = 11.5937(16) nm, c = 11.8477(17) nm, α = 93.932(3)º, β = 102.442(3)º, γ = 97.117(3)º, and Z = 1.

Preparation and characterization of a series of bromodiphenyl(N,N-dialkyldithiocarbamato)tellurium(IV) compounds where R=Me, Et, i-Pr, Bu, and of chlorodiphenyl(N,N-dibutyldithiocarbamato)tellurium(IV) and diphenylbis(N,N-dibutyldithiocarbamato)tellurium(IV). Crystal structure of Ph2TeBr[S2CNEt2] and Ph2Te[S2CNBu2]2

1991 ◽  
Vol 69 (12) ◽  
pp. 1948-1956 ◽  
Author(s):  
Jane H. E. Bailey ◽  
John E. Drake ◽  
Maria L. Y. Wong
Keyword(s):  
Crystal Structure ◽  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Crystal Structures ◽  
Vibrational Spectroscopy ◽  
Elemental Analysis ◽  
Reductive Elimination ◽  
Cell Parameters ◽  
Nuclear Magnetic Resonance Spectra

The series Ph2TeBr[S2CNR2], where R = Bu, Pr, i-Pr, Et, and Me, as well as Ph2TeCl[S2CNR2] and Ph2Te[S2CNR2]2, where R=Bu, Pr, have been synthesized and characterized by elemental analysis and vibrational spectroscopy. Comparisons of the effect of changing R groups and halogen atoms can be made based on the two crystal structures determined herein along with earlier work. The geometry about tellurium is consistent with that of a distorted sawhorse structure where the dithiocarbamate groups are monodentate (or anisobidentate). The crystal structures of Ph2TeBr[S2CNEt2], 4, and Ph2Te[S2CNBu2]2, 7, were completed. The cell parameters for 4 are a = 11.204(3) Å, b = 14.106(11) Å, c = 13.867(10) Å, α = 99.62(6)°, β = 102.76(5)°, γ = 87.73(4)°, V = 2107 Å3, Z = 4, R = 0.0448, and Rw = 0.0489 and for 7 are a = 19.392(6) Å, b = 9.622(2) Å, c = 19.089(6) Å, β = 104.70(2)°, V = 3445(2) Å3, Z = 4, R = 0.0397, and Rw = 0.0439. Nuclear magnetic resonance spectra are not simple and indicate that several species are present in solution, as rearrangements and reductive elimination take place. Key words: structure, tellurium, bromo, diphenyl, dialkyldithiocarbamato.

Ultra-low thermal conductivity in Na/Sb chalcobismuthates: synthesis, crystal structures, optical properties and 23Na NMR spectroscopy

2019 ◽  
Vol 43 (27) ◽  
pp. 10814-10820 ◽  
Author(s):  
Fatimah Alahmari ◽  
Somnath Dey ◽  
Abdul-Hamid Emwas ◽  
Bambar Davaasuren ◽  
Alexander Rothenberger
Keyword(s):  
Thermal Conductivity ◽  
Optical Properties ◽  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Unit Cell ◽  
Synthesis And Characterization ◽  
Metal Site ◽  
23Na Nmr ◽  
Metal Phases

The synthesis and characterization of mixed metal phases, Na2BiSbQ4 (Q = S, Se, Te), containing only one metal site in the unit cell, which resulted in extremely low thermal conductivities.

A study of a variety of O,O-alkylene dithiophosphate derivatives of triphenyl-and diphenylgermane. Crystal structures of and

1995 ◽  
Vol 73 (7) ◽  
pp. 915-928 ◽  
Author(s):  
John E. Drake ◽  
Anil G. Mislankar ◽  
Raju Ratnani ◽  
Jincai Yang
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Distorted Tetrahedron ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
Derivatives Of

The O,O-alkylene dithiophosphate derivatives of triphenyl- and diphenylgermane, [Formula: see text] [Formula: see text] [Formula: see text] [Formula: see text] [Formula: see text] and [Formula: see text] have been prepared and characterized by infrared, Raman, and 1H, 13C, and 31P NMR spectroscopy, mass spectrometry, and, in three cases, X-ray crystallography. [Formula: see text] 1, crystallizes as monoclinic in the space group P21/a (No. 14) with the cell parameters a = 12.868(5) Å, b = 11.354(4) Å, c = 17.207(4) Å, β = 95.42(2)°, V = 2502(1) Å3, Z = 4, R = 0.0640, and Rw = 0.0585. [Formula: see text] 2, crystallizes as orthorhombic in the space group Pbca (No. 61) with the cell parameters a = 23.007(4) Å, b = 16.840(4) Å, c = 12.068(3) Å, V = 4657(3) Å3, Z = 8, R = 0.0502, and Rw = 0.0329. [Formula: see text] 3, crystallizes as monoclinic in the space group C2/c (No. 15) with the cell parameters a = 35.48(2) Å, b = 9.275(5) Å, c = 20.78(1) Å, β = 120.93(3)° V = 5866(5) Å3, Z = 8, R = 0.0674, and Rw = 0.0562. As with their methylgermanium analogues, the environment about germanium is essentially that of a distorted tetrahedron, with the terminal sulfur atoms oriented towards germanium rather than away from it, in contrast with analogous noncyclic dithiophosphatogermanes. The substituents on the atoms in both the five- and six-membered rings maintain their nonequivalence in solution, in contrast with tin analogues. Keywords: structure, germanium, diphenyl, triphenyl, cyclic dithiophosphates

Synthesis and characterization of LMo(CO)3M(PPh3)x (where L = tridentate pyrazolyl-gallate or -borate ligand; M = Rh, x = 2; M = Cu, x = 1). X-ray crystal structures of [MeGapz3]Mo(CO)3Rh(PPh3)2 and [MeGapz3]Mo(CO)3Cu(PPh3) (where pz = pyrazolyl, N2C3H3)

1986 ◽  
Vol 64 (2) ◽  
pp. 373-386 ◽  
Author(s):  
Gregory A. Banta ◽  
Brenda M. Louie ◽  
Emmanuel Onyiriuka ◽  
Steven J. Rettig ◽  
Alan Storr
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Heavy Atom ◽  
Synthesis And Characterization ◽  
Octahedral Structure ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

The reactions of the LMo(CO)3− ions (L = MeGapz3, HBpz3, Me2Gapz(OCH2CH2NMe2)) with [Cu(PPh3)Cl]4 and Rh(PPh3)3Cl have yielded complexes with Mo—Cu and Mo—Rh bonds. The X-ray crystal structures of two such complexes have been determined. Crystals of [MeGapz3]Mo(CO)3Cu(PPh3) are monoclinic, a = 17.071(2), b = 16.738(1), c = 23.641(3) Å, β = 104.899(6)°, Z = 8, space group P21/n, and those of [MeGapz3]Mo(CO)3Rh(PPh3)2, are triclinic, a = 12.519(3), b = 17.182(4), c = 12.071(2) Å, α = 105.02(1), β = 109.87(1), γ = 97.10(2)°, Z = 2, space group [Formula: see text]. Both structures were solved by conventional heavy atom methods and were refined by full-matrix least-squares procedures to R = 0.040 and Rw = 0.035 for 6296 reflections with I ≥ 2σ(I) and R = 0.036 and Rw = 0.037 for 5642 reflections with I ≥ 3σ(I), respectively. The former complex provides a rare example of a 3:3:1, or capped octahedral structure, with a short (mean) Mo—Cu distance of 2.513(9) Å. The latter compound displays one terminal and two bridging CO ligands and a Mo—Rh distance of 2.6066(5) Å.

scholarly journals Softening the Donor-Set: From [Cu(P^P)(N^N)][PF6] to [Cu(P^P)(N^S)][PF6]

Inorganics ◽  
2019 ◽  
Vol 7 (1) ◽  
pp. 11 ◽  
Author(s):  
Isaak Nohara ◽  
Alessandro Prescimone ◽  
Catherine Housecroft ◽  
Edwin Constable
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Spectroscopic Data ◽  
1H Nmr Spectroscopy ◽  
Variable Temperature ◽  
Synthesis And Characterization ◽  
Single Crystal Structures ◽  
Roesy Spectrum ◽  
Vt Nmr

We report the synthesis and characterization of [Cu(P^P)(N^S)][PF6] complexes with P^P = bis(2-(diphenylphosphino)phenyl) ether (POP) or 4,5-bis(diphenylphosphino)-9,9- dimethylxanthene (xantphos) and N^S = 2-(iso-propylthio)pyridine (iPrSpy) or 2-(tert-butylthio)pyridine (tBuSpy). The single crystal structures of [Cu(POP)(iPrSPy)][PF6] and [Cu(POP)(tBuSPy)][PF6] have been determined and confirm a distorted tetrahedral copper(I) centre and chelating P^P and N^S ligands in each complex. Variable temperature (VT) 1H and 31P{1H} NMR spectroscopy reveals dynamic behavior with motion of the POP backbone in [Cu(POP)(iPrSPy)][PF6] and [Cu(POP)(tBuSPy)][PF6] frozen out at 238 K. VT NMR spectroscopic data including EXSY peaks in the ROESY spectrum of [Cu(xantphos)(tBuSPy)][PF6] at 198 K reveal that two conformers exist in an approximate ratio of 5:1. Replacing bpy by the N^S ligands shifts the Cu+/Cu2+ oxidation to a higher potential. The copper(I) compounds are weak emitters in the solid state with PLQY values of <2%. These values are similar to those for [Cu(POP)(bpy)][PF6] and [Cu(xantphos)(bpy)][PF6] in the solid state.

Synthesis and Characterization of Bromo- and Bromochloroplumbates(II). Crystal Structures of [Ph4E]2[Pb3Br8] (E = P, As) and [Ph4P][PbBrCl2] • CH3CN

2000 ◽  
Vol 55 (5) ◽  
pp. 377-382 ◽  
Author(s):  
Thomas M. Klapötke ◽  
Burkhard Krumm ◽  
Kurt Polbom ◽  
Claudia M. Rienäcker
Keyword(s):  
Crystal Structures ◽  
Lattice Parameters ◽  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group

[Ph4P]2[Pb3Br8] and [Ph4As]2[Pb3Br8] crystallize both in the monoclinic space group P 21/n. The lattice parameters of [Ph4P]2[Pb3Br8] are a = 14.637(7), b = 8.151(3), c = 23.388(8) Å, β = 106.02(3)°, Z = 2 and of [Ph4As]2[Pb3Br8] are a = 14.697(7), b = 8.219(3), c = 23.527(8) Å, β = 106.27(3)°, Z = 2. The lattice parameters of [Ph4P][PbBrCl2]·CH3CN, which crystallizes in the triclinic space group (P 1̅), are a = 9.435(3), b = 10.2577(14), c = 14.055(2) Å, α = 88.320(11)°, β = 84.82(2)°, γ = 84.19(2)°, Z = 2. 207Pb NMR shifts of halogenoplumbates in solution are reported.

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