Chem. J. Chinese Universities ›› 2015, Vol. 36 ›› Issue (1): 34.doi: 10.7503/cjcu20140763
• Articles: Inorganic Chemistry • Previous Articles Next Articles
LIU Yabing1,2,*(), DUAN Weijie2, CUI Xiaobing2, XU Jiqing2
Received:
2014-08-20
Revised:
2014-12-23
Online:
2015-01-10
Published:
2014-12-23
Contact:
LIU Yabing
E-mail:liuyab@163.com
CLC Number:
TrendMD:
LIU Yabing, DUAN Weijie, CUI Xiaobing, XU Jiqing. Synthesis and Characterization of a 2D Tungstovanadated Derivative: [Cu(en)2]2[VⅤO44{Cu(en)2(H2O)}2]·3H2O†[J]. Chem. J. Chinese Universities, 2015, 36(1): 34.
Empirical formula | C16W6.5N16Cu4O49V10.5 | D/(Mg·m-3) | 2.949 |
---|---|---|---|
Formula weight | 3258.86 | μ/mm-1 | 12.633 |
Crystal system | Triclinic | Limiting indices | -14≤h≤17 |
Space group | P | -15≤k≤17 | |
a/nm | 1.2857(2) | -15≤l≤18 | |
b/nm | 1.3064(2) | F(000) | 1513 |
c/nm | 1.3951(3) | Crystal size | 0.24 mm×0.22 mm×0.21 mm |
α/(°) | 81.324(1) | Goodness-of-fit on F2 | 1.041 |
β/(°) | 63.094(1) | Final R indices[I>2σ(I)]* | R1=0.0570 |
γ/(°) | 65.150(1) | wR2 = 0.1615 | |
Volume/nm3 | 1.8354(6) | R indices(all data) | R1 = 0.0972 |
Z | 1 | wR2 = 0.1797 |
Table 1 Crystal data and structure refinement for compound 1
Empirical formula | C16W6.5N16Cu4O49V10.5 | D/(Mg·m-3) | 2.949 |
---|---|---|---|
Formula weight | 3258.86 | μ/mm-1 | 12.633 |
Crystal system | Triclinic | Limiting indices | -14≤h≤17 |
Space group | P | -15≤k≤17 | |
a/nm | 1.2857(2) | -15≤l≤18 | |
b/nm | 1.3064(2) | F(000) | 1513 |
c/nm | 1.3951(3) | Crystal size | 0.24 mm×0.22 mm×0.21 mm |
α/(°) | 81.324(1) | Goodness-of-fit on F2 | 1.041 |
β/(°) | 63.094(1) | Final R indices[I>2σ(I)]* | R1=0.0570 |
γ/(°) | 65.150(1) | wR2 = 0.1615 | |
Volume/nm3 | 1.8354(6) | R indices(all data) | R1 = 0.0972 |
Z | 1 | wR2 = 0.1797 |
W1/V1—O10 | 0.1688(8) | W1/V1—O8 | 0.1845(9) | W2/V2—O5 | 0.1804(9) |
---|---|---|---|---|---|
W2/V2—O12 | 0.2031(9) | W3/V3—O18 | 0.1884(8) | W3/V3—O4 | 0.2443(1) |
W4/V4—O20 | 0.1683(8) | W5/V5—O9 | 0.1876(9) | W6/V6—O18 | 0.1989(9) |
V7—O2 | 0.1689(2) | V7—O3 | 0.1666(1) | V8—O12 | 0.1936(9) |
V9—O22 | 0.1913(9) | V9—O18 | 0.1977(1) | Cu1—N2 | 0.2004(1) |
Cu2—N5 | 0.1978(1) | Cu3—N7 | 0.1999(2) | N6—C6 | 0.146(2) |
O4—V7—O1 | 111.0(7) | O2—V7—O1 | 109.4(7) | V7—O1—W2/V2 | 119.8(6) |
V8—O23—W1/V1 | 101.8(4) | C8—C7—N7 | 104.0(2) | V9—O22—W5/V5 | 101.6(4) |
Table 2 Selected bond lengths(nm) and bond angles(°) for compound 1
W1/V1—O10 | 0.1688(8) | W1/V1—O8 | 0.1845(9) | W2/V2—O5 | 0.1804(9) |
---|---|---|---|---|---|
W2/V2—O12 | 0.2031(9) | W3/V3—O18 | 0.1884(8) | W3/V3—O4 | 0.2443(1) |
W4/V4—O20 | 0.1683(8) | W5/V5—O9 | 0.1876(9) | W6/V6—O18 | 0.1989(9) |
V7—O2 | 0.1689(2) | V7—O3 | 0.1666(1) | V8—O12 | 0.1936(9) |
V9—O22 | 0.1913(9) | V9—O18 | 0.1977(1) | Cu1—N2 | 0.2004(1) |
Cu2—N5 | 0.1978(1) | Cu3—N7 | 0.1999(2) | N6—C6 | 0.146(2) |
O4—V7—O1 | 111.0(7) | O2—V7—O1 | 109.4(7) | V7—O1—W2/V2 | 119.8(6) |
V8—O23—W1/V1 | 101.8(4) | C8—C7—N7 | 104.0(2) | V9—O22—W5/V5 | 101.6(4) |
Fig.1 Ball/strick representation of the tetra-capped Keggin polyoxoanion supporting two transition metal complex of compound 1 M1, M2: 0.8W+0.2V; M3, M4: 0.46W+0.54V; M5, M6: 0.36W+0.64V.
Fig.2 [Cu(en)2]2+ cations join polyoxoanion into 2D layer through Cu—O interactions [Cu1(en)2(H2O)]2+ cations, water and en molecules are omitted for clarity.
Fig.3 View of 3D supramolecular network structure with hydrogen bonding interactions between water molecules and oxygen atoms from two neighboring 2D layers along b axix(A) and schematic drawing of the 3D supramolecular topology in compound 1(B) (A) Several hydrogen atoms are omitted for clarity; (B) covalent bond and weak bond are shown with two-colored lines, and hydrogen bonds are shown with purple lines, respectively.
Fig.10 Changes of UV-Vis absorption spectra of RhB solutions with compound 1 Irradiation time(min) from a to m: 0, 30, 60, 90, 120, 150, 180, 210, 240, 270, 300, 330, 360.
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