127 VO(S2)2(bpy) IC

127 VO(S2)2(bpy) IC - 2978 A New Vanadium(V Persulfide...

Info iconThis preview shows pages 1–3. Sign up to view the full content.

View Full Document Right Arrow Icon
Background image of page 1

Info iconThis preview has intentionally blurred sections. Sign up to view the full version.

View Full DocumentRight Arrow Icon
Background image of page 2
Background image of page 3
This is the end of the preview. Sign up to access the rest of the document.

Unformatted text preview: 2978 A New Vanadium(V) Persulfide Complex: (NEt4)[V0(Sz)2(bpy)] Stephanie L. Castro, James D. Martin, and George Christou‘ Department of Chemistry and the Molecular Structure Center, Indiana University, Bloomington, Indiana 47405 Received January 28, 1993 Introduction Over the last several years, we have been investigating nonorganometallic vanadium/ sulfide chemistry, concentrating on the higher metal oxidation states (III—V). We have found this area to be rich in structural types and reactivity character- istics.1 Together with related efforts by others,” an impressive pool of complexes has now been made available spanning a variety of nuclearities and oxidation levels, including mixed valency. Our interest in this area stems from the conversion of crude oil vanadyl impurities to polymeric vanadium sulfides under the sulfur-rich conditions present during catalytic hydrodesulfurization and hydrodemetalation processes.7 A variety of discrete V / S species are probably forming as intermediates, and the characterization of V/ S species thus becomes of relevance to the understanding of these transformations. The area of impact of the present work is vanadium persulfide chemistry. A number of V complexes of various metal nuclearities are now known that contain 822- groups, in either terminal or bridging modes. laid-6,840 With very few exceptions, these involve VIII or V”. Persulfido complexes containing VV are extremely rare, presumably due to the redox instability of this highest V oxidation state in the presence of moderate reducing agents; in fact, to our knowledge, the only characterized example is (Me3NCH2Ph)2[VSZ(SZ)(SPh)].1i However, we herein report a convenient, high-yield procedure to a second VV persulfide complex (1) (a) Money, J. K.; Huffman, J. C.; Christou, G. Inorg. Chem. 1985, 24, 3297. (b) Money, J. K.; Folting, K.; Huffman, J. C.; Collison, D.; Temperly, J.; Mabbs, F. E.; Christou, G. Inorg. Chem. 1986, 25, 4583. (c) Money, J. K.; Nicholson, J. R.; Huffman, J. C.; Christou, G. Inorg. Chem. 1986,25, 4072. ((1) Money, J. K.; Huffman, J. C.; Christou, G. J. Am. Chem. Soc. 1987, 109, 2210. (e) Money, J. K.; Folting, K.; Huffman, J. C.; Christou, G. Inorg. Chem. 1987, 26, 944. (1') Money, J. K.; Huffman, J. C.; Christou, G. Inorg. Chem. 1988, 27, 507. (g) Christou, G.; Heinrich, D. D.; Money, J. K.; Rambo, J. R.; Huffman, J. C.; Folting, K. Polyhedron 1989, 8, 1723. (h) Heinrich, D. D.; Folting, K.; Huffman, J. C.; Reynolds, J. G.; Christou, G. Inorg. Chem. 1991, 30, 300. (i) Sendlinger, S. C.; Nicholson, J. R.; Lobkovsky, E. 13.; Huffman, J. C.; Rehder, D.; Christou, G. Inorg. Chem. 1993, 32, 204. (2) (a) Do, Y.; Simhon, E. D.; Holm, R. H. J. Am. Chem. Soc. 1983, 105, 6371. (b) Do, Y.; Simhon, E. D.; Holm, R. H. Inorg. Chem. 1985, 24, 4635. (3) Halbert, T. R.; Hutchings, L. L.; Rhodes, R.; Stiefel, E. I. J. Am. Chem. Soc. 1986, 108, 6437. (4) Al-Ani, F. T.; Hughes, D. L.; Pickett, C. J. J. Chem. Soc. Dalton Trans. 1988, 1705. (5) Duraj,S. A.; Andras, M. T.; Kibala, P. A. Inorg. Chem. 1990, 29, 1232. (6) (a) Yang, Y.; Huang, L.; Liu, Q.; Kang, B. Acta Crystallogr. 1991, C47, 2085. (b) Yang, Y.; Liu, Q.; Huang, L.; Kang, 3.; Lu, J. J. Chem. Soc, Chem. Commun. 1992, 1512. (7) (a) Silbernagel, B. G. J. Catal. 1979, 56, 315. (b) Rosa-Brussin, M.; Moranta, D. Appl. Catal. 1984, II, 85. (c) Silbernagel, E. G.; Mohan, R. R.; Singhal, G. H. ACS Symp. Ser. 1984, 248, 91. ((1) Mitchell, P. C. H.; Scott, C. E.; Bonnelle, J.-P.; Grimblot, J. G. J. Chem. Soc. Faraday Trans. 1 1985,81, 1047. (e) Asaoka, S.; Nakata, S.; Takeuchi, C. ACS Symp. Ser. 1987, 344, 275. (8) (a) Bolinger, C. M.; Rauchfuss, T. B.; Rheingold, A. L. Organometallies 1982, I, 1551. (b) Bolinger, C. M.; Rauchfuss, T. 3.; Rheingold, A. L. J. Am. Chem. Soc. 1983, 105, 6321. (c) Bolinger, C. M.; Weatherill, T. D.; Rauchfuss, T. B.; Rheingold, A. L.; Day, C. S.; Wilson, S. R. Inorg. Chem. 1986, 25, 634. (9) Halbert, T. R.; Hutchings, L. L.; Rhodes, R.; Stiefel, E. I. J. Am. Chem. Soc. 1986, 108, 6437. (10) Floriani, C.; Gambarotta, S.; Chiesi-Villa, A.; Guastini, C. J. Chem. Soc, Dalton Trans. 1987, 2099. 0020-1669/93/1332-297880400/0 Inorg. Chem. 1993, 32, 2978—2980 Table 1. Crystallographic Data for (NEtl)[VO(S;)1(bpy)]oMeCN (l-MeCN) C20H3xN4084V W? = 522.67 monoclinic P2, (No. 4) a =6.948(1)A T=~154°C b=13.547(1)A x=o.71o 69A c = 12.930(1) A paw = 1.428 g cm—3 13 = 92.45(1)° u = 7.436 cm" V= 1216.01 A3 R“ = 0.0209 Z = 2 R..” = 0.0242 “ R = ZIIFoI — IFcII/ZIFOI. R. = [Mal—|r.|)2/mr,1211/2, where w = 1/02(|F°|). together with its characterization by single-crystal X-ray dif- fractometry and spectroscopy. Experimental Section All manipulations were carried out using standard Schlenk-line techniques or an inert-atmosphere glovebox. Solvents were distilled before use from CaHz (MeCN) or Na / benzophenone (EtzO), except anhydrous EtOH which was used as received in Sure-Seal bottles (Aldrich). Anhydrous Lizs and elemental S and bpy were used as received. (NEts)2[VOC1¢] was prepared as described elsewhere.11 Preparation of (NEMIV0(Sz)2(bpy)]-MeCN (1). In an inert-atmo- sphere glovebox, (NEt4)2[VOCl4] (0.48 g, 1.0 mmol), sulfur (0.080 g, 2.5 mmol), Lizs (0.115 g, 2.50 mmol), and bpy (0.803 g, 5.15 mmol) were placed in a flask. The flask was brought into the laboratory and attached to a Schlenk line, and a 1:1 mixture of MeCN/EtOH (80 mL) was added by syringe; the reaction mixture was then stirred overnight at ambient temperature. The resulting deep red solution was filtered, EtZO (40 mL) added to the filtrate, and the flask stored in a freezer for 1 week. Red/black needles of complex 1-MeCN were collected by filtration, washed with Etzo, and dried briefly in vacuo. The yield was 0.287 g (55%). The same reaction with a V:bpy ratio of 1:1 gave yields of ca. 25%. The presence of one interstitial MeCN molecule was demonstrated by the crystallographic studies, but analytical data for a sample vacuum-dried for a more extended period (ca. 2 h) indicated loss of the MeCN groups. Anal. Calcd (found) for C13H23N3084V: C, 44.89 (44.90); H, 5.86 (5.73); N, 8.72 (8.69). Electronic spectrum in MeCN (~5 mM), Amx/nm (eM/L mol‘l cm’l): 336 (7600), 384 (4270), 520 (874). X-ray Crystallography. Data were collected on a Picker four-circle diffractometer; details of the diffractometry, low-temperature facilities, and computational procedures employed by the Molecular Structure Center are available elsewhere.12 The crystal employed was a fragment cleaved from a larger crystal and affixed to a glass fiber using silicone grease. It was then transferred to the goniostat where it was cooled to —154 °C for characterization and data collection (Table I). A systematic search of a limited hemisphere of reciprocal space yielded a set of reflections exhibiting monoclinic symmetry. The systematic extinction of 0k0, k = 2n + 1, and subsequent refinement confirmed the space group P2]. Following the usual data reduction and averaging of equivalent reflections, a unique set of 1682 reflections was obtained. Plots of the four standard reflections measured every 300 reflections showed no significant variation. The structure was solved using a combination of direct methods (SHELXS- 86)” and standard Fourier techniques. After unsuccessful refinement in the centric space group sz/m, the acentric space group P2, was considered. The vanadium, sulfur, and oxygen atoms as well as two- thirds of the bpy atoms were located in the initial E map from SHELXS. All the remaining atoms, including the hydrogen atoms, were located in successive difference Fourier maps. The full-matrix, least-squares refinement was completed using anisotropic thermal parameters on the non-hydrogen atoms and isotropic thermal parameters on the hydrogens. All unique reflections were used for the refinement. An absorption correction was deemed unnecessary and was not performed. Since P21 is an acentric space group, the absolute structure for the crystal employed was determined by refinement of both possibilities. The final difference (11) Rambo, J. R.; Christou, G. Manuscript in preparation. (12) Chisholm, M. H.; Folting, K.; Huffman, J. C.; Kirkpatrick, C. C. Inorg. Chem. 1984, 23, 1021. (13) Sheldrick, G. M. In Crystallographic Computing 3; Sheldrick, G. M., Kruger, C., Goddard, R., Eds.; Oxford University Press: New York, 1985; pp 175—189. © 1993 American Chemical Society Notes map was essentially featureless with the largest peaks being 50.33 e/A3 in the immediate vicinity of the vanadium atom. Final values of conventional discrepancy indices R and Rw are listed in Table 1. Other Measurements. Infrared (Nujol mull) and electronic absorption solution spectra were recorded on Nicolet Model SIOP and Hewlett- Packard Model 8452A spectrophotometers, respectively. 51V NMR spectra (94.95 MHz) were obtained on a Nicolet NT360 instrument using a sample concentration of ca. 50 mM in CD3CN and 5-mm tubes. Chemical shifts are quoted versus VOCla in CDClg as an external reference. Results Synthesis of Complex 1. The procedure described in the Experimental Section employs an equimolar mixture of 1.128 and elemental S as a potential source of 822-. In fact, since the VIv is oxidized to V", the sulfur reagents must also be involved in additional redox chemistry. The half-reactions describing the various redox changes are shown in eqs 1-3. The overall formation v4+_e—_’V$+ 2.58 + 2.5sl-—> 2.5822' (2) 0.5s22— + e” —» sz- (3) of complex 1 can now be summarized in eq 4; this equation predicts voc142‘ + 2.5s + 2.5s2- + bpy —» [V0(Sz)2(bpy)l‘ + 82‘ + 4Cl' (4) that a S:Li;S ratio of 25:15 should suffice for the formation of l, and we have indeed found that comparable yields are obtained from the 2.5: 1 .5 reaction system. Note also that the bpy:V ratio employed is larger than the 1:1 suggested by eq 4. In this case, we have found that the presence of excess bpy results in higher yields (approximately double) than for Vszy = 1:1 reactions. The reason for this is unclear, but we note that the yield of MoO(S2)2(bpy) is also improved in the presence of a 100% excess of bpy.” Description of Structure. Fractional coordinates and selected bond distances and angles are collected in Tables 11 and 111, respectively. An ORTEP representation of the anion of 1 is presented in Figure l. The V atom is seven-coordinate and possesses distorted pentagonal bipyramidal geometry. The multiply-bonded oxygen atom 008) and bpy nitrogen atom N(l7) occupy the axial sites (O(18)-V(1)—N(17) = 165.26(l3)°). The anion has idealized C, symmetry. The five equatorial ligating atoms are approximately in a plane; the maximum deviation from the 8(2), 8(3), 8(4), 5(5), N(6) least-squares plane is 0.033 A for 8(4), and V(l) lies 0.324 A out of this plane toward 0(18). The sum of the equatorial angles at V is 355.86°. As expected, there is a significant trans influence of 0(18) on the V(1)-N(17) distance (2.302(3) A), which is noticeably longer than equatorial V(1)—N(6) (2.1 39(3) A). An alternative description of the metal coordination geometry as trigonal bipyramidal can be presented if the 522- ligands are considered to be occupying a single site. If S(2 / 3) and S(4/ 5) are used to represent the midpoints of the S(2)-S( 3) and S(4)—S(5) bonds, respectively, then the equatorial angles become N(6)—V(1)—S(2/3) = lll.4°,S(2/3)-V(l)—S(4/ 5) = 135.1°, and S(4/5)—V(l)—N(6) = 109.3°. It is instructive to compare the structure of the anion of l with those of the anions of (NH4)[VO(02)2(bpy)] (2),15 MoO(S;)2(bpy) (3),14 and MoO(02)2(bpy) (4);16 complexes 2 and 4 contain peroxide (022‘) groups in place of the persulfides (14) Chakrabarty, P. K.; Bhattacharya, 5,; Pierpont, C. G.; Bhattacharyya, R. Inorg. Chem. 1992, 31, 3573. (15) Szentivanyi, H.;Stomberg, R.Acta Chem. Scand., Ser. A 1983, 37, 553. (16) Schlemper, E. 0.; Schrauzer, G. N.; Hughes, C. A. Polyhedron 1984, 3, 377. Inorganic Chemistry, Vol. 32, No. 13, 1993 2979 Table 11. Selected Atomic Coordinates (X10‘)" and Isotropic Thermal Parameters (x10) for l-MeCN atom at y 2 Ba,” A2 V(l) 4094(1) 964* 7552.1(4) 9 8(2) 6852(1) 862(1) 6576(1) 14 5(3) 5904(1) —485(l) 7074(1) 13 8(4) 2595(1) 2280(1) 8524(1) 13 5(5) 4726(1) 2682(1) 7553(1) 12 N(6) 2713(5) 15(3) 8614(3) 11 C(7) 962(5) —366(3) 8351(3) 12 C(8) 52(6) -1009(3) 8989(3) 16 C(9) 918(6) —1278(3) 9928(4) 16 C(10) 2698(6) —882(3) 10199(3) 15 C(11) 3569(5) —237(3) 9527(3) 11 C(12) 5464(5) 224(3) 9771(3) 12 C(13) 6568(6) 48(3) 10674(3) 14 C(14) 8311(6) 537(3) 10827(3) 14 C(15) 8922(6) 1162(3) 10074(3) 15 C(16) 7776(5) 1302(3) 9180(3) 12 N(l7) 6063(4) 844(3) 9025(2) 10 0(18) 2389(4) 852(2) 6684(2) 13 mm 9617(5) 3513(3) 5168(3) 13 C(20) 10804(6) 4461(4) 5333(3) 20 C(21) 11296(8) 4708(4) 6453(4) 25 C(22) 10806(6) 2614(4) 5493(3) 17 C(23) 12505(7) 2415(4) 4833(4) 18 C(24) 7853(6) 3532(4) 5813(4) 19 C(25) 6574(7) 4438(4) 5652(4) 19 C(26) 9069(7) 3490(4) 4024(4) 21 C(27) 8006(9) 2565(5) 3669(5) 31 " Parameter marked with an asterisk was not varied. " Equivalent isotropic values for atoms refined anisotropically were calculated using the published procedure.22 Table In. Selected Bond Distances (A) and Angles (deg) for l-MeCN (a) Bonds V(1)—O(18) 1.6039(26) V(1)—N(6) 2.139(3) V(l )—S(3) 2.4251(12) V(l )—N(l 7) 2.302(3) V(l)—S(2) 2.3437(11) S(2)—S(3) 2.0531(15) V(l)—-S(5) 2.3686(13) S(4)—S(5) 2.0549(13) V(l)—S(4) 2.4403(13) (b) Angles 0(18)—V(1)—S(3) 96.9200) S(3)—V(l)—S(2) 5037(4) 0(18)—V(1)—S(2) 102.35(10) S(3)—V(1)—S(5) 134.19(4) 0(18)—V(1)—S(5) 103.00(11) S(3)—V(1)—S(4) 163.72(4) 0(18)—V(1)—S(4) 96.3800) S(3)-V(l)—N(l 7) 81.80(9) 0(18)-V(1)—N(17) l65.26(l3) S(2)-V(1)—S(5) 8438(4) O(18)—V(1)—N(6) 93.1 1(13) S(2)—V(1)-S(4) 134.19(5) N(6)—V(1)—S(3) 8592(9) S(2)—V(1)—N(l7) 8832(8) N(6)—V(1)—S(2) l35.26(9) S(5)—V(1)-S(4) 50.57(4) N(6)—V(1)—S(5) l32.75(9) S(5)—V(l)-N(l7) 8800(9) N(6)—V(l)-S(4) 84.02(9) S(4)—V(1)—-N(l7) 8295(9) N(6)—V(l)—N(17) 72.15(12) (522-) of l and 3. Pertinent structural parameters are listed in Table IV. It is readily apparent that the four species are extremely similar, both in overall structure and in metric parameters. There are the expected differences due to the S vs 0 variation (for example, the M—E bond lengths) and the expected slight variation in analogous parameters due to the size difference between V5+ and Mo“, but otherwise the complexes are almost indistinguish- able within the 36 criterion. Complex] is also related to the VI" complex V(Sz)2(terpy) (terpy = 2,2’:6’,2”-terpyridine),4 which similarly has distorted pentagonal bipyramidal geometry but with the third pyridyl ring occupying the axial position occupied by the 0x0 group in 1. The S—S distances in V(Sz)2(terpy) are 2.043(1) and 2.025(1) A. Spectroscopic Studies. The 1H NMR spectrum in CD3CN displayed NEta+ resonances and eight bpy resonances, as expected from the solid-state structure of l and the C, symmetry of the anion. To probe with better certainty whether more than one V species is formed on dissolution of 1, 5‘V NMR spectroscopy was employed. A single sharp resonance was observed at 6 = -402 2980 Inorganic Chemistry, Vol. 32, No. 13, I 993 Figure l. ORTEP representation of the anion of 1 at the 50% probability level. Carbon atoms are numbered sequentially around the rings. Table IV. Comparative Structural Data“ for Complexes 1—4 [V0(Sz)2' [V0(02)2' MoO(S2)2- M00(02)2- param (bpy)1' (bpy)]‘ (bpy) (bpy) M-E. 2.4403(13) 1.909(3) 2.425(4) 1.948(4) M—Eb 2.3686(13) 1.880(3) 2.378(5) 1.908(4) M-Ec 2.3437(11) 1.883(3) 2.364(4) 1.912(5) M—Ed 2.425102) 1.911(3) 2.437(4) 1.953(4) 13.43., 2.0549(13) 1.471(4) 2.055(6) 1.465(6) Ec-Ed 2.0531(15) 1.465(4) 2.038(6) 1.459(6) M—O 1.6039(26) 1.619(3) 1.690(10) 1.682(4) M-N’ 2.139(3) 2.149(4) 2.207(12) 2.199(5) M—N 2.302(3) 2.288(3) 2.35102) 2.312(5) O—M—E. 96.3800) 99.1(2) 97.9(4) 101.7(2) O—M-Eb 103.0001) 103.3(2) 103.4(4) 105.6(2) O—M—Ec 102.3500) 104.0(2) 103.3(3) 105.4(2) O—M—Ed 96.92(10) 100.2(2) 99.3(4) 101.1(2) O—M—N’ 93.1103) 92.4(2) 91.3(5) 92.4(2) E.—M-E., 5057(4) 45.70) 50.50) 44.6(2) Ec-M—Ed 5097(4) 45.40) 50.4(2) 44.4(2) ‘ Tabulated using the labeling scheme E 1’ E DM—N‘ b EZ—l—‘Ed N ppm vs VOC13. The combined NMR results thus support retention of the solid-state structure on dissolution in MeCN. The 6(5‘V) value lies between the ranges found for V complexes with exclusively O/N ligation (—537 to —672 ppm)17 and exclusively S ligation (+101 to +1457 ppm);“v13 the complex VO(OH)(S;CNEt2)2, which possesses both 0 and S ligation, has 6(5‘V) = —468 ppm.” The 6(51V) value for l is comparable with but upfield (more shielded) vis-a-vis those for the complexes [V2(Il-'Sz)z(css)d" and V2(#'Sz)2(szcx)4 (X = 5M9» NEE NBu“), which have 5 values in the +101 to +173 ppm range and which similarly contain V centers bound to two 822’ groups.1i The relative shielding of 1 compared to these exclusively S-ligated species is as expected given the presence of O and bpy N ligands, (17) (a) Harrison, A. T.; Howarth, O. W. J. Chem. Soc, Dalton Trans. 1985, 1173. (b) Rehder, D.; Wieghardt, K. Z. Naturforsch., B 1981, 36, 1251. (18) (a) Harrison, A. '1'.; Howarth, 0. W. J. Chem. Soc, Dalton Trans. 1986, 1405. (b) Preuss, F.; Noichl, A. Z. Naturforsch., B 1987, 42, 121. (19) Rehder, D.; Weidemann, C.; Duch, A.; Priebsch, W. Inorg. Chem. 1988, 27, 584. Notes because d° VV exhibits the so-called inverse polarizability (electronegativity) dependence of metal shielding; i.e., the shielding increases with the more electronegative (or less polarizable) O/ N ligands”:20 The IR spectrum of 1 displays the V0 multiple-bond stretch at 940 cm-1 and the 8—8 stretch at 535 cm-1. These values are consistent with expectation and similar to those for isostructural MO(S2)2(bpy) (M = M0, 930 and 540 cm-1; M = W, 940 and 525 cm").14 The electronic spectrum in MeCN displays three distinct and intense features at 336, 384, and 520 nm assignable to ligand (822-, bpy)-to-metal charge transfer. Discussion Complex 1 represents only the second structurally confirmed example of a vanadium(V) persulfide complex; as mentioned earlier, persulfide complexes of V are primarily found at the VIII and VIV oxidation levels. The other VV example is (MC3NCH2Ph)2[Vsz(Sz)(SPh)], whose structure is shown as follows. Also shown is the anion [V54]3‘, a tetrahedral ion S s\\‘|'é S S\V ’8 S S s/ \S wo<s2)2<bpy)1' [vs2(sz)(sr’h)12' [V3413 possessing four S?“ ligandsfib’” It is interesting to note that these species form a trio related by the fact that they each possess four “inorganic” S atoms either as 482‘ in [VS4]3‘, as 282-, 822' in [VSz(Sz) (SPh)] 2', or as 2S2} in the anion of 1. Additional ligation is required along this series (from right to left) to compensate for decreasing electron donation from 822‘ vs S" ligands. The 8—8 bond length in [VSz(Sz)(SPh)]2-(2.013(3) A) is noticeably shorter than those in [VO(SZ)2(bpy)]' (2.0549(13), 2.0531(15) A), indicating greater electron donation in the former from occupied 822— 1r* orbitals into empty V d orbitals; this would be consistent with the significantly greater coordination number in [V0- (Sz)2(bpy)]‘ (7) Us [V52(Sz)(SPh)]2‘ (5). The convenient and high-yield nature of the preparation of 1 suggests that this complex should be an excellent starting point for synthesis of other V / S species. Preliminary observations are supporting this belief. In this regard, 1 appears to be superior to (MC3NCH2Ph)2[VSz(S2)(SPh)], which is extremely reactive but suffers from being sparingly soluble and metastable in solution, although it has nevertheless been successfully employed for the synthesis of (MC;NCH2Ph)4[V2(S2)2(CS3)4].H Acknowledgment. This work was supported by the Office of Basic Energy Sciences, Division of Chemical Sciences, US. Department of Energy, under Grant DEFG02-87ER13702. Supplementary Material Available: A textual summary of the crystallographic work, tables of crystal data, atomic coordinates, thermal parameters, and bond distances and angles, and additional labeled figures and stereoviews (1 1 pages). Ordering information is given on any current masthead page. (20) (a) Rehder, D. In Transition Metal Nuclear Magnetic Resonance; Pregosin,P. S.,Ed.;Elsevier: Amsterdam, 199l;p 1. (b) Multinuclear NMR; Mason, J ., Ed.; Plenum Press: New York. 1987; pp 488—493 and references therein. (21) Krfiss, G.; Ohnmais, K. Chem. Ber. 1890, 23, 2547; Justus Liebigs Ann. Chem. 1891, 263, 39. (22) Hamilton, W. C. Acta Crystallogr. 1959, 12, 609. ...
View Full Document

This note was uploaded on 01/20/2012 for the course CHM 2210 taught by Professor Reynolds during the Fall '01 term at University of Florida.

Page1 / 3

127 VO(S2)2(bpy) IC - 2978 A New Vanadium(V Persulfide...

This preview shows document pages 1 - 3. Sign up to view the full document.

View Full Document Right Arrow Icon
Ask a homework question - tutors are online