The hetero-metal clusters [■5-C5H4C（O）CH2CH2C（O）OCH3]FeCoM（■3-S）（CO）8 （M = Mo 1, M = W 2） were prepared by thermal reactions of FeCo2（CO）9(（3-S） with metal exchange reagent [■5-C5H4C（O）CH2CH2C（O）O...The hetero-metal clusters [■5-C5H4C（O）CH2CH2C（O）OCH3]FeCoM（■3-S）（CO）8 （M = Mo 1, M = W 2） were prepared by thermal reactions of FeCo2（CO）9(（3-S） with metal exchange reagent [■5-C5H4C（O）CH2CH2C（O）OCH3]M（CO）3Na （M = Mo or W） in THF. Cluster 1 reacted with 2,4-dinitrophenylhydrazine at room temperature to yield the cluster hydrazone derivative (（3-S）CoFeMo（CO）8[(5-C5H4C（NR）Me] [R = NHC6H3-2,4-（NO2）2] 3. All the compounds were characterized by elemental analyses, IR and NMR spectra. Cluster 1 was determined by single crystal X-ray diffraction. Crystal data: C18H11O11SCoFeMo, Mr = 646.05, triclinic, space group P, a = 8.148（2）, b = 10.685（3）, c = 13.410（4） ?, ( = 100.077（5）, ( = 102.452（5）, ( = 91.108（6）(, V = 1120.4（5） ?3, Z = 2, Dc = 1.915 g/cm3, F（000） = 636, ( = 2.071 mm(1, the final R = 0.0378 and wR = 0.0968 for 5074 observations with (I > 2（（I））.展开更多
S A new cyclomercurated ferrocenylketimine containing pyridyl ring ([HgCl(5- C5H3C(CH3)=N-3-C5H4N)Fe(5-C5H5)]紺H2Cl2, Mr = 581.66) was synthesized and its molecular structure has been confirmed by IR, elemental analys...S A new cyclomercurated ferrocenylketimine containing pyridyl ring ([HgCl(5- C5H3C(CH3)=N-3-C5H4N)Fe(5-C5H5)]紺H2Cl2, Mr = 581.66) was synthesized and its molecular structure has been confirmed by IR, elemental analysis, 1H-NMR and X-ray crystal structure analysis. It is of monoclinic system, space group P21/c with a = 9.213(2), b = 17.479(4), c = 11.510(2) ? b = 100.32(3)o, V = 1823.7(6) 3, Z = 4, C17.5H16Cl2FeHgN2, Dc = 2.119 g/cm3, m = 9.497 mm-1, F(000) = 1100, R = 0.0436 and wR = 0.0987. The independent reflections are 3527, of which 3153 with I ≥ 2s(I) were observed. The compound contains a five-membered metallocycle. The mercury atom is bonded with the 2-position of substituted cyclopentadienyl ring (Cp), and coordinated weakly to the N atom of imino group. The pyridyl ring is almost perpendicular to the substituted Cp which is nearly coplanar with the metallocycle. The Hg(1)C(1) and Hg(1)Cl(1) bond lengths are 2.050(8) and 2.321(2) ? respectively.展开更多
基金the National Natural Science Foundation of China.
文摘The hetero-metal clusters [■5-C5H4C（O）CH2CH2C（O）OCH3]FeCoM（■3-S）（CO）8 （M = Mo 1, M = W 2） were prepared by thermal reactions of FeCo2（CO）9(（3-S） with metal exchange reagent [■5-C5H4C（O）CH2CH2C（O）OCH3]M（CO）3Na （M = Mo or W） in THF. Cluster 1 reacted with 2,4-dinitrophenylhydrazine at room temperature to yield the cluster hydrazone derivative (（3-S）CoFeMo（CO）8[(5-C5H4C（NR）Me] [R = NHC6H3-2,4-（NO2）2] 3. All the compounds were characterized by elemental analyses, IR and NMR spectra. Cluster 1 was determined by single crystal X-ray diffraction. Crystal data: C18H11O11SCoFeMo, Mr = 646.05, triclinic, space group P, a = 8.148（2）, b = 10.685（3）, c = 13.410（4） ?, ( = 100.077（5）, ( = 102.452（5）, ( = 91.108（6）(, V = 1120.4（5） ?3, Z = 2, Dc = 1.915 g/cm3, F（000） = 636, ( = 2.071 mm(1, the final R = 0.0378 and wR = 0.0968 for 5074 observations with (I > 2（（I））.
基金This work was supported by NNSFC (No. 20072034) and NSF of Henan province
文摘S A new cyclomercurated ferrocenylketimine containing pyridyl ring ([HgCl(5- C5H3C(CH3)=N-3-C5H4N)Fe(5-C5H5)]紺H2Cl2, Mr = 581.66) was synthesized and its molecular structure has been confirmed by IR, elemental analysis, 1H-NMR and X-ray crystal structure analysis. It is of monoclinic system, space group P21/c with a = 9.213(2), b = 17.479(4), c = 11.510(2) ? b = 100.32(3)o, V = 1823.7(6) 3, Z = 4, C17.5H16Cl2FeHgN2, Dc = 2.119 g/cm3, m = 9.497 mm-1, F(000) = 1100, R = 0.0436 and wR = 0.0987. The independent reflections are 3527, of which 3153 with I ≥ 2s(I) were observed. The compound contains a five-membered metallocycle. The mercury atom is bonded with the 2-position of substituted cyclopentadienyl ring (Cp), and coordinated weakly to the N atom of imino group. The pyridyl ring is almost perpendicular to the substituted Cp which is nearly coplanar with the metallocycle. The Hg(1)C(1) and Hg(1)Cl(1) bond lengths are 2.050(8) and 2.321(2) ? respectively.
