Home Crystal and molecular structures of P,P-dicyclohexyl-N-methyl-phosphinylthioformamide, P,P-dicyclohexyl-N-phenyl-phosphinylthioformamide, P,P-dicyclohexyl-N-methyl-thiophosphinylthioformamide, and P,P-dicyclohexyl-N-phenyl-thiophosphinylthioformamide
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Crystal and molecular structures of P,P-dicyclohexyl-N-methyl-phosphinylthioformamide, P,P-dicyclohexyl-N-phenyl-phosphinylthioformamide, P,P-dicyclohexyl-N-methyl-thiophosphinylthioformamide, and P,P-dicyclohexyl-N-phenyl-thiophosphinylthioformamide

Published/Copyright: July 28, 2010
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Zeitschrift für Kristallographie - Crystalline Materials
From the journal Zeitschrift für Kristallographie - Crystalline Materials Volume 209 Issue 11

Abstract

The crystal structures of the title compounds P,P-dicyclohexyl-N-methyl-phosphinylthioformamide, [cHex2P(O)C(S)N(H)Me], C14H26ONPS, P,P-dicyclohexyl-N-phenylphosphinylthioformamide, [cHex2P(O)C(S)N(H)Ph], C19H28ONPS, P,P-dicyclohexyl-N-methylthiophosphinylthioformamide, [cHex2P(S)C(S)N(H)Me], C14H26NPS2, and P,P-dicyclohexyl-N-phenyl-thiophosphinylthioformamide, [cHex2P(S)C(S)N(H)Ph], C19H28NPS2, have been determined at room temperature. The green crystals of [cHex2P(O)C(S)N(H)Me] are monoclinic, space group C2/c, with unit cell dimensions a = 10.247(2) Å, b = 16.025(4) Å, c = 19.358(4) Å, β = 97.75(2)°, Z = 8 and Dx = 1.212 Mg m−3. Crystals of [cHex2P(O)C(S)N(H)Ph] are also monoclinic, space group C2/c, with unit cell dimensions a = 14.856(4) Å, b = 11.666(4) Å, c = 22.039(3) Å, β = 95.59(1)°, Z = 8 and Dx = 1.221 Mg m−3. The colorless crystals of [cHex2P(S)C(S)N(H)Me] are orthorhombic, crystallizing in the Pnma space group with dimensions a = 10.2600(9) Å, b = 15.447(2) Å, c = 10.141(3) Å, Z = 4 and Dx = 1.254 Mg m−3. Yellow crystals of [cHex2P(S)C(S)N(H)Ph] are triclinic, space group P[unk], with dimensions a = 9.766(2) Å, b = 11.111(2) Å, c = 9.388(2) Å α = 100.54(2)°, β = 104.66(1)° and γ = 83.86(1)°, Z = 2 and Dx = 1.249 Mg m−3. The structures were solved by directmethods and each refined by a full-matrix least-squares procedure to final R = 0.036 (0.046; 0.040; and 0.038) using 1383 (1257; 1362; and 2758) reflections for each of the above [cHex2P(Y)C(S)N(H)R] (where Y = O or S and R = Me or Ph) compounds, respectively. The conformation about the C–N bond in each of [cHex2P(Y)C(S)N(H)R] is Z. Important parameters for Y = O, R = Me: P = O 1.480(2), P–C 1.814(4), C = S 1.630(3) and C–N 1.306(4) Å; Y = O, R = Ph: P = O 1.479(4), P–C 1.817(5), C = S 1.618(5) and C–N 1.327(6) Å; Y = S, R = Me: P = S 1.942(1), P–C 1.823(4), C = S 1.644(4) and C–N 1.290(5) Å; and Y = S, R = Ph: P = S 1.9495(9), P–C 1.846(3), C = S 1.624(2) and C–N 1.317(3) Å. Symmetry related molecules of [cHex2P(O)C(S)N(H)R] associate in the lattice via hydrogen bonding contacts. The P–C(1) bond distances in the [cHex2P(Y)C(S)N(H)R] compounds are shown to be significantly shorter than those found in the related [Ph2P(Y)C(S)N(H)R] compounds.

Published Online: 2010-7-28
Published in Print: 1994-11-1

© 2015 Oldenbourg Wissenschaftsverlag GmbH, Rosenheimer Str. 145, 81671 München

Articles in the same Issue

  1. Thermal dependence of the Pb5Al3F19 lattice parameters in phases I–IV
  2. Crystal growth and crystal structure of arsenicv ditelluroidide semihydrate, AsTe2I · 0.5 H2O
  3. Submicroscopic twinning and chemical inhomogeneity of ilvaite, a mixed-valence iron sorosilicate HCaFe22 + Fe3 + Si2O9
  4. Substitutional disorder in the system Mg1 − xCu2 + xO3: Cu2+ in a compressed octahedral environment
  5. A crystal structure determination of HgC2O4 from synchrotron X-ray and neutron powder diffraction data
  6. Crystal and molecular structure of 5-(3-methylbut-2-enyloxy)-7-methoxy-8-(3-methylbut-2-enyl)-2 H-[1]-benzopyran-2-one (Sesibiricin)
  7. Structural studies on oxalatotriorganostannates. Crystal structure of trimethylsulfonium catena-O,O′-oxalatotriphenylstannate
  8. Crystal and molecular structures of P,P-dicyclohexyl-N-methyl-phosphinylthioformamide, P,P-dicyclohexyl-N-phenyl-phosphinylthioformamide, P,P-dicyclohexyl-N-methyl-thiophosphinylthioformamide, and P,P-dicyclohexyl-N-phenyl-thiophosphinylthioformamide
  9. Two organically-templated vanadium arsenate phases: V4As6O30H6 · 2 N2C6H14 · 4 H2O and V4As6O30H8 · 2 N(CH3)4 · 5.33 H2O
  10. Crystal structure of manganese ultraphosphate, MnP4O11
  11. Crystal structure of c-6-[N,N-bis(trimethylsilyl)amino]-5,6-dihydro-r-4-[(1′-hydroxy-1′-methyl)ethyl]-t-5-methyl-3-phenyl-4H-1,2-oxazine, ONC(CH)(CH)(CH)(C6H5)C(OH)(CH3)2(CH3)NSi(CH3)3Si(CH3)3
  12. Crystal structure of 2-methyl-6-phenyl-pyridin-3-al, (C6H5)C(CH)2CCNCHO(CH3)
  13. Crystal structure of 3-O-(5,6-dihydro-5-methyl-3-phenyl-4H-1,2-oxazin-6-yl)-1,2:5,6-di-O-isopropyliden-α-D-glucofuranose, O(CH)4OCO(CH3)2CHCH2OCO(CH3)2OCHCHCH2CNO(CH3)(C6H5)
  14. Crystal structure of 1,3-bis(3-trifluoromethylphenyl)-2,2,4,4-tetramethyl-1,3-diaza-2,4-disila-cyclobutane, (F3C(C6H4)NSi(CH3)2)2
  15. Crystal structure of 5-ethyl-2′-deoxyuridine, C11H16N2O5
  16. Crystal structure of 3,6-dimethyl-5-methylthio-thieno[3,2-b]-thiophen-2-carbaldehyde, C10H10OS3
  17. Crystal structure of anti-5,13-di-tert-butyl-8,16-difluoro-[2.2]metacyclophane, C24H30F2
  18. Crystal structure of 1-(3,5-difluoro-2,6-di(trans-stilbenyl)phenyl)-2-phenyl-diazene, (C6H5)NN(C6F2H(C(C6H5)CH(C6H5))2)
  19. Crystal structure of di(bis(1,1-dimethylethyl)phosphinic amide) hydrobromide,((C4H9)2(NH2)PO)2(HBr)
  20. Crystal structure of bis(lignocainium) dioxotrichloronitratouranate(IV), (C14H22ON2)2(UO2(NO3)Cl3)
  21. Crystal structure of bis(lignocainium) tetrathiocyanatocobaltate(II) hydrate, (C14H22ON2)2 Co(NCS)4 (H2O)
  22. Crystal structure of bis(lignocainium) tetrabromocuprate(II), (C14H22ON2)2CuBr4
  23. Crystal structure of terbium chromium aluminium, Tb6Cr4+xAl43−x (x = 1.6), erbium chromium aluminium, Er6Cr4+xAl43−x (x = 1.96), holmium chromium aluminium, Ho6Cr4+xAl43−x (x = 1.6), and lutetium chromium aluminium, Lu6Cr4+xAl43−X (x = 2.76)
https://doi.org/10.1524/zkri.1994.209.11.885

Articles in the same Issue

  1. Thermal dependence of the Pb5Al3F19 lattice parameters in phases I–IV
  2. Crystal growth and crystal structure of arsenicv ditelluroidide semihydrate, AsTe2I · 0.5 H2O
  3. Submicroscopic twinning and chemical inhomogeneity of ilvaite, a mixed-valence iron sorosilicate HCaFe22 + Fe3 + Si2O9
  4. Substitutional disorder in the system Mg1 − xCu2 + xO3: Cu2+ in a compressed octahedral environment
  5. A crystal structure determination of HgC2O4 from synchrotron X-ray and neutron powder diffraction data
  6. Crystal and molecular structure of 5-(3-methylbut-2-enyloxy)-7-methoxy-8-(3-methylbut-2-enyl)-2 H-[1]-benzopyran-2-one (Sesibiricin)
  7. Structural studies on oxalatotriorganostannates. Crystal structure of trimethylsulfonium catena-O,O′-oxalatotriphenylstannate
  8. Crystal and molecular structures of P,P-dicyclohexyl-N-methyl-phosphinylthioformamide, P,P-dicyclohexyl-N-phenyl-phosphinylthioformamide, P,P-dicyclohexyl-N-methyl-thiophosphinylthioformamide, and P,P-dicyclohexyl-N-phenyl-thiophosphinylthioformamide
  9. Two organically-templated vanadium arsenate phases: V4As6O30H6 · 2 N2C6H14 · 4 H2O and V4As6O30H8 · 2 N(CH3)4 · 5.33 H2O
  10. Crystal structure of manganese ultraphosphate, MnP4O11
  11. Crystal structure of c-6-[N,N-bis(trimethylsilyl)amino]-5,6-dihydro-r-4-[(1′-hydroxy-1′-methyl)ethyl]-t-5-methyl-3-phenyl-4H-1,2-oxazine, ONC(CH)(CH)(CH)(C6H5)C(OH)(CH3)2(CH3)NSi(CH3)3Si(CH3)3
  12. Crystal structure of 2-methyl-6-phenyl-pyridin-3-al, (C6H5)C(CH)2CCNCHO(CH3)
  13. Crystal structure of 3-O-(5,6-dihydro-5-methyl-3-phenyl-4H-1,2-oxazin-6-yl)-1,2:5,6-di-O-isopropyliden-α-D-glucofuranose, O(CH)4OCO(CH3)2CHCH2OCO(CH3)2OCHCHCH2CNO(CH3)(C6H5)
  14. Crystal structure of 1,3-bis(3-trifluoromethylphenyl)-2,2,4,4-tetramethyl-1,3-diaza-2,4-disila-cyclobutane, (F3C(C6H4)NSi(CH3)2)2
  15. Crystal structure of 5-ethyl-2′-deoxyuridine, C11H16N2O5
  16. Crystal structure of 3,6-dimethyl-5-methylthio-thieno[3,2-b]-thiophen-2-carbaldehyde, C10H10OS3
  17. Crystal structure of anti-5,13-di-tert-butyl-8,16-difluoro-[2.2]metacyclophane, C24H30F2
  18. Crystal structure of 1-(3,5-difluoro-2,6-di(trans-stilbenyl)phenyl)-2-phenyl-diazene, (C6H5)NN(C6F2H(C(C6H5)CH(C6H5))2)
  19. Crystal structure of di(bis(1,1-dimethylethyl)phosphinic amide) hydrobromide,((C4H9)2(NH2)PO)2(HBr)
  20. Crystal structure of bis(lignocainium) dioxotrichloronitratouranate(IV), (C14H22ON2)2(UO2(NO3)Cl3)
  21. Crystal structure of bis(lignocainium) tetrathiocyanatocobaltate(II) hydrate, (C14H22ON2)2 Co(NCS)4 (H2O)
  22. Crystal structure of bis(lignocainium) tetrabromocuprate(II), (C14H22ON2)2CuBr4
  23. Crystal structure of terbium chromium aluminium, Tb6Cr4+xAl43−x (x = 1.6), erbium chromium aluminium, Er6Cr4+xAl43−x (x = 1.96), holmium chromium aluminium, Ho6Cr4+xAl43−x (x = 1.6), and lutetium chromium aluminium, Lu6Cr4+xAl43−X (x = 2.76)
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