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Chapter 5 Published Results Table 5.7. Selected Cu–O and Co–O bond lengths [Å] for 29 and 30, respectively a Code 1 2 Cu(1)-O(6C) eq 1.91(1) Co(1)-O 1.97(3), 2.00(2), Cu(1)-O(13C) eq 1.94(1) 2.02(2), 2.03(3), Cu(1)-O(7C) eq 1.95(1) 2.04(2), 2.21(2) Cu(1)-O(12C) eq 1.99(1) Co(2)-O 2.02(2), 2.06(2), Avg. Cu(1)-O eq 1.95(3) 2.06(2), 2.12(2), 2.15(2), 2.25(2) Cu(2)-O(15C) eq 1.93(1) Cu(2)-O(4G2) eq 1.96(1) Cu(2)-O(4G1) eq 1.97(1) Cu(2)-O(9C) eq 1.98(1) Avg. Cu(2)-O eq 1.96(2) Cu(3)-O(4G2) eq 1.97(1) Cu(3)-O(4C) eq 1.98(1) Cu(3)-O(10C) eq 1.98(1) Cu(3)-O(4G1) eq 2.00(1) Avg. Cu(3)-O eq 1.98(1) Co(3)-O 2.06(2), 2.08(2), 2.08(3), 2.09(2), 2.09(2), 2.12(2) Co(4)-O 2.04(3), 2.07(2), 2.08(2), 2.09(2), 2.12(3), 2.18(2) Co(5)-O 2.03(2), 2.03(2), 2.04(3), 2.05(2), 2.08(2), 2.19(2) Co(6)-O 2.04(2), 2.05(2), 2.06(2), 2.07(2), 2.11(2), 2.17(2) Cu(1)-O(4G1) ax1 2.35(1) Cu(2)-O(2C2) ax1 2.30(1) Cu(3)-O(2C) ax1 2.31(1) Avg. Cu-O ax1 2.32(3) Cu(1)-O(1CU) ax2 2.55(2) Cu(2)-O(13C) ax2 2.54(1) Cu(3)-O(12C) ax2 2.52(1) Avg. Cu-O ax2 2.54(2) a Mean values are indicated in bold. 209
Chapter 5 Published Results The manganese(II) containing polyanion 31 is composed of two fragments of [Mn 3 (H 2 O)(B-β-GeW 9 O 33 (OH))(B-β-GeW 8 O 30 (OH))] 12– linked through an octahedrally coordinated Mn 2+ ion. In close analogy to 30, this extra metal ion links the two sandwich fragments by coordinating to the pair of rotated tungsten centers in each (B-β-GeW 8 O 31 ) unit and it also has two trans-related terminal water ligands (Figure 5.20). Polyanion 31 exhibits a small degree (~15%) of crystallographic alpha/beta disorder of two W 3 O 13 triads in the (B-β-GeW 9 O 34 ) unit. We were able to resolve this issue by assigning partial occupancies to the involved W atoms. Figure 5.20. Combined polyhedral/ball-and-stick representation of 31. The pink spheres represent Mn 2+ (31). Otherwise, the color code is the same as in Figures 5.15 – 5.19. 210
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