Supplementary material

Syntheses and characterization of a new class of vanadia precursors of oxime-modified oxovanadium(V) isopropoxide, Crystal and molecular structure of [VO{ONC10H16}3]

Archana Chaudharya, Nikita Sharmab, Meena Nagarb, Shaikh M. Mobina, Pradeep Mathura, Rakesh Bohrab*

a Discipline of Chemistry, School of Basic Sciences, Indian Institute of Technology -Indore , Indore –452017,

Madhya Pradesh, India

b Department of Chemistry, University of Rajasthan, Jaipur-302004, Rajasthan, India.

Fig. S1 51V NMR spectra of (1) and (4)

Table-S1 Fragmented molecular ions vs m/e values for [VO{OPri}2{ONC10H16}] (1), [VO{OPri}{ONC10H16}2] (2), [VO{ONC10H16}3] (3) and [VO{OPri}{ONC(CH)3}2] (5)

Complex / Fragmented ion / m/e value /
[VO{OPri}2{ONC10H16}] (1) / [VO{C10H16NO}{OC3H7}{OC3H6}]+ / 350
[VO{C10H16NO}{OC3H7}{H4}]+ / 296
[VO{C10H16NO}{OC2H9}]+ / 282
[VO{C10H16NO}{OH}]+ / 250
[VO{C10H15NO}]+ / 232
[VO{C7H3N}]+ / 168
[VO{OPri}{ONC10H16}2] (2) / [VO{C10H16NO}2{OC2H}]+ / 440
[VO{C10H16NO}{C8H12NO}]+ / 371
[VO{C10H16NO}{C7H6NO}]+ / 353
[VO{C10H16NO}{C7HO}]+ / 334
[VO{C10H16NO}{C7}]+ / 317
[VO{C10H13NO}{C6}]+ / 302
[VO{C10H12NO}{C6}]+ / 301
[VO{C5H11NO}]+ / 168
[VO{ONC10H16}3] (3) / [VO{ONC10H16NO}3] / 567
[VO{C10H16 NO}2{C10H15NO}] + / 566
[VO{C10H16 NO}{C5H12NO}] + / 335
[VO{C10H16 NO}{C4H6NO}] + / 317
[VO{C10H16 NO}{C4H4N}] + / 299
[VO{C7H16NO}] + / 197
[VO{C6H10NO}] + / 179
[VO{CHN}] + / 78
[VO{OPri}{ONC(CH3)2}2] (5) / [VO{ONC(CH3)2}{ONC3H4}]+ / 209
[VO{ONC3H6}]+ / 139
[VO{C3H6}]+ / 109

Table-S2 Important bond lengths (Å) and angles (°) of [VO{ONC10H16}3] (3)

Bond lengths
V(1)-O(4) / 1.579(4) / V(1)-N(1) / 2.022(4)
V(1)-O(2) / 1.889(3) / V(1)-N(3) / 2.030(4)
V(1)-O(3) / 1.914(3) / V(1)-N(2) / 2.220(4)
V(1)-O(1) / 1.926(4) / N(1)-C(1) / 1.253(6)
O(1)-N(1) / 1.365(5) / N(2)-C(11) / 1.273(6)
O(2)-N(2) / 1.405(5) / N(3)-C(21) / 1.278(6)
O(3)-N(3) / 1.367(5)
Bond angles
O(4)-V(1)-O(1) / 104.85(19) / O(2)-V(1)-O(1) / 127.68(16)
O(4)-V(1)-O(2) / 104.71(17) / O(3)-V(1)-O(1) / 83.91(15)
O(4)-V(1)-O(3) / 107.48(17) / N(1)-V(1)-N(3) / 160.76(16)
O(4)-V(1)-N(1) / 98.00(18) / N(1)-V(1)-N(2) / 85.60(15)
O(4)-V(1)-N(3) / 97.95(17) / N(3)-V(1)-N(2) / 87.92(15)
O(4)-V(1)-N(2) / 143.61(17) / O(2)-V(1)-N(2) / 38.93(14)
O(2)-V(1)-N(1) / 93.43(15) / O(3)-V(1)-N(3) / 40.43(14)
O(3)-V(1)-N(1) / 123.40(16) / O(1)-V(1)-N(1) / 40.36(15)
O(1)-V(1)-N(2) / 101.11(17) / N(1)-O(1)-V(1) / 73.6(2)
O(2)-V(1)-N(3) / 92.86(15) / N(3)-O(3)-V(1) / 74.4(2)
O(1)-V(1)-N(3) / 124.15(16) / N(2)-O(2)-V(1) / 83.4(2)
O(1)-N(1)-V(1) / 66.0(2) / O(2)-N(2)-V(1) / 57.70(18)
O(3)-N(3)-V(1) / 65.2(2) / O(2)-V(1)-O(3) / 125.55(15)
O(3)-V(1)-N(2) / 100.19(15)

Table- S3 XRD data of vanadia samples (a), (b), (c) and (d)

Vanadia / XRD data
2θ / d(Å) / hkl / crystal type
(a) / 26.423
27.870
29.170
30.623
32.905
41.644
45.858
50.661
60.301
67.530 / 3.3704
3.1986
3.0590
2.9170
2.7190
2.1669
1.9771
1.8022
1.5336
1.3859 / -111
-102
002
301
211
-502
-120
-611
-613
-803 / Monoclinic
(b) / 15.348
20.241
21.677
24.894
26.115
29.280
31.020
32.329
41.181 / 5.7684
4.3836
4.0965
3.6324
3.4095
3.0400
2.8806
2.7669
2.1903 / 200
001
101
010
110
210
301
011
002 / Orthorombic
(c) / 20.289
21.713
41.242 / 4.3734
4.0897
2.1872 / 001
101
002 / Orthorombic
(d) / 20.336
21.764
31.029
32.310
41.292 / 4.3633
4.0802
2.8817
2.7672
2.1846 / 001
101
301
011
002 / Orthorombic

Fig. S2 TG curve obtained from [VO{OPri}2{ONC10H16}] (1)