TY - JOUR
T1 - Molybdenum(VI) complexes of branched ligands with [N,O,O,O] and [O,O,O] donor sets. The crystal and molecular structures of...
AU - Liu, Shuncheng
AU - Ma, Lidun
AU - McGowty, Deborah
AU - Zubieta, Jon
PY - 1990
Y1 - 1990
N2 - Title full: Molybdenum(VI) complexes of branched ligands with [N,O,O,O] and [O,O,O] donor sets. The crystal and molecular structures of [MoO2{HOC2H4N(C2H 4)O2}], [(n-C4H9)4N]2[Mo2 O4{(O2NCCH2O)3}2] ·202NC(CH2OH)3, [(n-C4H9)4N][Mo2O5 {(HO2CCH2N)(CH2CO2) 2}2]·H2O and [n-C4H9)4N][Mo3O6 (OCH3{(CH3OCH2O)3} 2]. Reactions in methanol of [TBA]2[Mo2O7] with the appropriate branched polyhydroxylic and polycarboxylic ligands yielded the complexes [MoO2{(HOC2H4N(C2H 4O)2}] (3), [TBA]2[Mo2O4{(O2NC(CH 2O)3}2]·2O2NC(CH 2OH)3 (4), [TBA]2[Mo2O5{(HO2CCH 2N(CH2CO2)2}2] ·H2O (5) and [TBA][Mo3O6(OCH3){(CH3CCH 2O)3}2] (6) [where TBA = (n-C4H9)4N]. The deprotonation of 3 yields [Et3NH][MoO2{(N(C2H)4O) 3}] (3a), while 4 was found to aggregate with additional molybdate to give [TBA][Mo3O6(OCH3){(O2NCCH 2O)3}2] (4a) and [MO4O8,(OCH3)2{(O2NCCH2 O)3}2] (4b). The structural interrelationship of this series of polymolybdate coordination compounds is discussed in terms of simple aggregation processes. Crystal data: 3, monoclinic P21/n, a = 10.688(2), b = 7.559(3), c = 11.386(7) β,Å = 99.62(1)°, V = 905.2(5) Å3, Z = 4,Dcalc, = 2.02 g cm-3; 1786 reflections, R = 0.0406. 4, triclinic P1, a = 10.965(2), b = 11.850(3), c = 13.247(3) Å, α= 84.72(1), β = 89.52(2), γ = 66.95(2)°, V = 1576.4(7) Å3, Z = 1, Dcalc = 1.40 g cm-3; 4718 reflections, R = 0.0389. 5, monoclinic P21, a = 10.735(2), b = 13.404(6), c = 19.257(6) Å, β = 90.61(2)°,V = 2770.9(16) Å 3, Z = 2, Dcalc = 1.36 g cm-3; 3212 reflections, R = 0.0380. 6, monoclinic P21/n, a = 10.908(2), b = 25.674(5), c = 13.059(2) Å, β= 96.35(2)°, V = 3635.6(12) Å3, Z = 4, Dcalc = 1.62 g cm-3; 3143 reflections, R = 0.0490.
AB - Title full: Molybdenum(VI) complexes of branched ligands with [N,O,O,O] and [O,O,O] donor sets. The crystal and molecular structures of [MoO2{HOC2H4N(C2H 4)O2}], [(n-C4H9)4N]2[Mo2 O4{(O2NCCH2O)3}2] ·202NC(CH2OH)3, [(n-C4H9)4N][Mo2O5 {(HO2CCH2N)(CH2CO2) 2}2]·H2O and [n-C4H9)4N][Mo3O6 (OCH3{(CH3OCH2O)3} 2]. Reactions in methanol of [TBA]2[Mo2O7] with the appropriate branched polyhydroxylic and polycarboxylic ligands yielded the complexes [MoO2{(HOC2H4N(C2H 4O)2}] (3), [TBA]2[Mo2O4{(O2NC(CH 2O)3}2]·2O2NC(CH 2OH)3 (4), [TBA]2[Mo2O5{(HO2CCH 2N(CH2CO2)2}2] ·H2O (5) and [TBA][Mo3O6(OCH3){(CH3CCH 2O)3}2] (6) [where TBA = (n-C4H9)4N]. The deprotonation of 3 yields [Et3NH][MoO2{(N(C2H)4O) 3}] (3a), while 4 was found to aggregate with additional molybdate to give [TBA][Mo3O6(OCH3){(O2NCCH 2O)3}2] (4a) and [MO4O8,(OCH3)2{(O2NCCH2 O)3}2] (4b). The structural interrelationship of this series of polymolybdate coordination compounds is discussed in terms of simple aggregation processes. Crystal data: 3, monoclinic P21/n, a = 10.688(2), b = 7.559(3), c = 11.386(7) β,Å = 99.62(1)°, V = 905.2(5) Å3, Z = 4,Dcalc, = 2.02 g cm-3; 1786 reflections, R = 0.0406. 4, triclinic P1, a = 10.965(2), b = 11.850(3), c = 13.247(3) Å, α= 84.72(1), β = 89.52(2), γ = 66.95(2)°, V = 1576.4(7) Å3, Z = 1, Dcalc = 1.40 g cm-3; 4718 reflections, R = 0.0389. 5, monoclinic P21, a = 10.735(2), b = 13.404(6), c = 19.257(6) Å, β = 90.61(2)°,V = 2770.9(16) Å 3, Z = 2, Dcalc = 1.36 g cm-3; 3212 reflections, R = 0.0380. 6, monoclinic P21/n, a = 10.908(2), b = 25.674(5), c = 13.059(2) Å, β= 96.35(2)°, V = 3635.6(12) Å3, Z = 4, Dcalc = 1.62 g cm-3; 3143 reflections, R = 0.0490.
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U2 - 10.1016/S0277-5387(00)86572-9
DO - 10.1016/S0277-5387(00)86572-9
M3 - Article
AN - SCOPUS:0000633083
SN - 0277-5387
VL - 9
SP - 1541
EP - 1553
JO - Polyhedron
JF - Polyhedron
IS - 13
ER -