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Convenient Syntheses and Structural Characterizations of Mono-substituted Alkylimido Hexamolybdates: [Mo6O18(NR)]2- (R = Me, Et, n-Pr, i-Pr, n-Bu, t-Bu, Cy, Hex, Ode)
†
Qiang Lia, Longsheng Wanga, Panchao Yina, Yongge Wei* , a , Jian Haoa, Yulin Zhua, Li Zhua, Gu Yuanb Received (in XXX, XXX) Xth XXXXXXXXX 200X, Accepted Xth XXXXXXXXX 200X First published on the web Xth XXXXXXXXX 200X DOI: 10.1039/b000000x a
Department of Chemistry, Tsinghua University, Beijing 100084, China E-mail:
[email protected] College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, PR China † Electronic Supplementary Information (ESI) available: [Listing of X-ray crystallographic data in CIF format]. See DOI: 10.1039/b000000x/ b
Electronic Supplementary Information for Dalton Transactions This journal is © The Royal Society of Chemistry 2009
Table S1 Summary of crystallographic data for compounds 5 and 7I. 5 7I Formula C36H81Mo6N3O18 C38H83Mo6N3O18 F.W.. 1419.68 1445.71 Crys. Sys. Orthorhombic Triclinic Space group Pbca P-1 a (Å) 16.8504(8) 12.5288(4) b (Å) 20.0036(10) 19.4569(6) c (Å) 31.6503(15) 23.1302(7) α (°) 90 93.7700(10) β (°) 90 103.1410(10) γ (°) 90 91.4990(10) 3 V (Å ) 10668.3(9) 5474.0(3) Z 8 4 3 ρcalc. Mg/m 1.768 1.754 -1 μ (mm ) 1.433 1.398 Refl. collected 48987 44067 Unique refl. (Rint.) 9378(0.0327) 18581(0.0302) R1 0.0509 0.0559 wR2 0.1351 0.1483 GOF 1.127 1.136 R = Σ||Fo| – |Fc||/Σ|Fo| and Rw = [Σ[w(Fo2 – Fc2)2]/Σw(Fo2)2]1/2 with w = 1/[σ2(Fo2) + (aP)2 + bP], where P = (Fo2 + 2Fc2)/3 0.0449, b = 46.6940; 7I : a = 0.0434, b = 21.3101.
5:a=
Electronic Supplementary Information for Dalton Transactions This journal is © The Royal Society of Chemistry 2009
Figure S1. ORTEP drawing of the [Mo6O18(=NR)]2- anion of 5
Electronic Supplementary Information for Dalton Transactions This journal is © The Royal Society of Chemistry 2009
Figure S2. ORTEP drawing of the [Mo6O18(=NR)]2- anion of 7I
Electronic Supplementary Information for Dalton Transactions This journal is © The Royal Society of Chemistry 2009
N
1.705 1.925 Mo 1.896 Et
O
O
1.864
1.946 Mo
Mo
1.931
1.891
O
O
1.925 Mo 1.910
N
O
1.910
O
Pr
1.871
Mo
Mo
1.892
O
1.948
O
O
1.907 1.909
1.894 Mo 1.930
1.920 Mo 1.903
Mo
Mo
1.923
1.894
O
O
1.935
1.917 Mo 1.904
1.879 Mo
Mo O
O
1.928
1.905
O
O
Mo
Mo
1.917
1.869
O
O
1.940
1.940 Mo 1.912
1.937 Mo 1.887
N
N
1.956 Mo 1.939
1.949 Mo 1.961
1.885
O
O
1.928
O
1.891 Mo
Mo O
1.916 Mo
Mo
1.948
O
1.929
O
Mo 1.925
1.923
1.911 Mo 1.906
1.893
O
O
1.937
O
1.878 Mo
Mo O
O
O
1.923
1.956 Mo
Mo
1.942
O
O
1.906
1.912 Mo 1.956
1.934 Mo 1.963
O
O
1.928 Mo 1.916
1.952 Mo 1.955
1.907
i-Pr-b
1.901
O
O
N
O
O
1.920
1.913
N
1.900 i-Pr-a
1.936
O
1.704 1.936 Mo 1.948
Mo
Mo
1.911
N
1.704 1.964 Mo 1.944 O
1.912 Mo 1.909
1.925 Mo 1.901
N
O
1.705
1.913
1.912 Mo 1.934
1.929 Mo 1.945 O
1.927
O
Mo
Mo
1.921
1.915
O
O
1.930
1.935 Mo 1.928
1.903 Mo 1.965 O
1.959
O
Mo
Mo
1.896
O
1.905
O
1.963
1.978 Mo 1.904
Figure S3. Bond length in the Mo4(Ob)4 belts in compounds 2, 3, 4a and 4b
Electronic Supplementary Information for Dalton Transactions This journal is © The Royal Society of Chemistry 2009
N
N
1.694
1.952 Mo 1.949 t-Bu
O
O
1.879
1.890 Mo
Mo
1.908
O
O
1.943
1.928 Mo 1.894
1.967 Mo 1.953 1.879
O
O
1.931
hex-a
O
N
O
O
1.917
1.930
hex-b
1.883
O
O
1.910 Mo
Mo
1.939
O
N
O
1.915
1.903 Mo 1.930
1.919
O
O
O
1.876 Mo
Mo
1.903
1.986
O
1.960
O
1.904 Mo
Mo
1.912
O
O
1.957
1.951 Mo 1.914
1.711
1.935 Mo 1.969 1.907
O
1.894 Mo 1.959
1.904 Mo 1.926
N
O
1.896 Mo
O
1.890 Mo
O
1.709 O
O
O
1.981 Mo 1.877
Mo
1.897 Mo 1.936
1.711 1.952 Mo 1.947
1.887
1.955 Mo 1.944 1.883
O
1.981
Mo
1.910
O 1.903 Mo 1.937
Mo
Mo
1.951
1.909
1.899
O
1.709 1.973 Mo 1.936 O
1.892 Mo 1.989
Mo
Mo
N
1.874
1.694
O
1.954
1.944 Mo 1.889
1.894 Mo 1.975 1.975
O
O
Mo
1.893
O
1.902 Mo
O
1.966
1.976 Mo 1.903
Figure S4. Bond length in the Mo4(Ob)4 belts in compounds 6, 8a and 8b.
