Table 1. Crystal data and structure refinement for 97src027. Identification code 97src027 Empirical formula C17 H11 Br Fe Mo O6 Formula weight 542.96 Temperature 293(2) K Wavelength 0.71069 A Crystal system Monoclinic Space group P2(1)/c Unit cell dimensions a = 10.655(4) A b = 12.3456(6) A c = 14.319(2) A beta = 103.142(11) deg. Volume 1834.1(7) A^3 Z 4 Density (calculated) 1.966 Mg/m^3 Absorption coefficient 3.683 mm^-1 F(000) 1056 Crystal size 0.31 x 0.18 x 0.11 mm Theta range for data collection 1.96 to 24.94 deg. Index ranges -11<=h<=12, -12<=k<=13, -16<=l<=14 Reflections collected 7104 Independent reflections 2654 [R(int) = 0.0586] Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 2646 / 0 / 236 Goodness-of-fit on F^2 0.912 Final R indices [I>2sigma(I)] R1 = 0.0448, wR2 = 0.1230 R indices (all data) R1 = 0.0586, wR2 = 0.1471 Largest diff. peak and hole 0.703 and -1.265 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for 97src027.U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________ x y z U(eq) ________________________________________________________________ Mo(1) 523(1) 6915(1) 1646(1) 29(1) Br(1) 6586(1) 6084(1) 5444(1) 77(1) Fe(1) 4675(1) 7446(1) 3483(1) 34(1) O(1) 2534(4) 8837(4) 1538(3) 39(1) O(2) 1376(5) 5854(5) 3702(4) 58(2) O(3) -902(7) 8706(5) 2631(5) 77(2) O(4) -1997(6) 5518(5) 1496(4) 74(2) O(5) -748(6) 7737(5) -478(4) 72(2) O(6) 1738(6) 4990(5) 667(4) 73(2) C(1) 5437(8) 7192(7) 4902(5) 47(2) C(2) 5771(9) 8242(7) 4630(6) 60(2) C(3) 4633(11) 8799(7) 4291(6) 68(3) C(4) 3585(9) 8150(7) 4330(6) 59(2) C(5) 4081(8) 7144(7) 4724(5) 52(2) C(6) 3988(7) 6288(5) 2477(5) 36(2) C(7) 5338(7) 6219(6) 2767(5) 43(2) C(8) 5858(7) 7185(7) 2559(6) 54(2) C(9) 4852(7) 7920(6) 2174(5) 45(2) C(10) 3647(6) 7343(6) 2100(4) 34(2) C(11) 2362(6) 7819(5) 1784(4) 31(2) C(12) 1459(7) 9550(6) 1183(6) 45(2) C(13) 1125(6) 6255(6) 2978(5) 38(2) C(14) -364(8) 8107(6) 2266(6) 46(2) C(15) -1105(8) 6033(6) 1527(5) 44(2) C(16) -267(8) 7488(6) 281(6) 49(2) C(17) 1327(7) 5689(6) 1025(5) 43(2) ________________________________________________________________ Table 4. Bond lengths [A] and angles [deg] for 97src027. _____________________________________________________________ Mo(1)-C(15) 2.022(8) Mo(1)-C(17) 2.040(8) Mo(1)-C(13) 2.039(8) Mo(1)-C(16) 2.069(9) Mo(1)-C(14) 2.057(9) Mo(1)-C(11) 2.224(7) Br(1)-C(1) 1.882(8) Fe(1)-C(9) 2.012(7) Fe(1)-C(1) 2.033(7) Fe(1)-C(2) 2.038(8) Fe(1)-C(10) 2.037(6) Fe(1)-C(3) 2.038(8) Fe(1)-C(6) 2.043(7) Fe(1)-C(7) 2.043(7) Fe(1)-C(5) 2.052(8) Fe(1)-C(8) 2.049(8) Fe(1)-C(4) 2.054(8) O(1)-C(11) 1.329(8) O(1)-C(12) 1.442(8) O(2)-C(13) 1.126(8) O(3)-C(14) 1.133(9) O(4)-C(15) 1.137(8) O(5)-C(16) 1.133(9) O(6)-C(17) 1.140(9) C(1)-C(5) 1.409(11) C(1)-C(2) 1.422(11) C(2)-C(3) 1.383(12) C(3)-C(4) 1.386(13) C(4)-C(5) 1.416(11) C(6)-C(7) 1.405(10) C(6)-C(10) 1.426(9) C(7)-C(8) 1.375(11) C(8)-C(9) 1.417(10) C(9)-C(10) 1.451(10) C(10)-C(11) 1.463(9) C(15)-Mo(1)-C(17) 90.0(3) C(15)-Mo(1)-C(13) 86.9(3) C(17)-Mo(1)-C(13) 92.1(3) C(15)-Mo(1)-C(16) 87.0(3) C(17)-Mo(1)-C(16) 87.9(3) C(13)-Mo(1)-C(16) 173.8(3) C(15)-Mo(1)-C(14) 87.2(3) C(17)-Mo(1)-C(14) 177.3(3) C(13)-Mo(1)-C(14) 87.7(3) C(16)-Mo(1)-C(14) 92.0(3) C(15)-Mo(1)-C(11) 177.5(3) C(17)-Mo(1)-C(11) 87.9(3) C(13)-Mo(1)-C(11) 91.9(3) C(16)-Mo(1)-C(11) 94.2(3) C(14)-Mo(1)-C(11) 94.9(3) C(9)-Fe(1)-C(1) 151.0(3) C(9)-Fe(1)-C(2) 116.9(4) C(1)-Fe(1)-C(2) 40.9(3) C(9)-Fe(1)-C(10) 42.0(3) C(1)-Fe(1)-C(10) 164.9(3) C(2)-Fe(1)-C(10) 153.6(3) C(9)-Fe(1)-C(3) 108.0(4) C(1)-Fe(1)-C(3) 67.3(3) C(2)-Fe(1)-C(3) 39.7(3) C(10)-Fe(1)-C(3) 121.7(3) C(9)-Fe(1)-C(6) 69.0(3) C(1)-Fe(1)-C(6) 126.4(3) C(2)-Fe(1)-C(6) 162.4(3) C(10)-Fe(1)-C(6) 40.9(3) C(3)-Fe(1)-C(6) 157.3(4) C(9)-Fe(1)-C(7) 68.4(3) C(1)-Fe(1)-C(7) 106.4(3) C(2)-Fe(1)-C(7) 124.2(3) C(10)-Fe(1)-C(7) 68.7(3) C(3)-Fe(1)-C(7) 161.3(4) C(6)-Fe(1)-C(7) 40.2(3) C(9)-Fe(1)-C(5) 166.4(3) C(1)-Fe(1)-C(5) 40.4(3) C(2)-Fe(1)-C(5) 67.8(4) C(10)-Fe(1)-C(5) 128.8(3) C(3)-Fe(1)-C(5) 66.8(4) C(6)-Fe(1)-C(5) 110.6(3) C(7)-Fe(1)-C(5) 120.7(3) C(9)-Fe(1)-C(8) 40.8(3) C(1)-Fe(1)-C(8) 117.2(3) C(2)-Fe(1)-C(8) 105.8(4) C(10)-Fe(1)-C(8) 68.7(3) C(3)-Fe(1)-C(8) 126.3(4) C(6)-Fe(1)-C(8) 67.0(3) C(7)-Fe(1)-C(8) 39.3(3) C(5)-Fe(1)-C(8) 152.4(3) C(9)-Fe(1)-C(4) 127.8(3) C(1)-Fe(1)-C(4) 68.0(3) C(2)-Fe(1)-C(4) 67.5(4) C(10)-Fe(1)-C(4) 110.4(3) C(3)-Fe(1)-C(4) 39.6(4) C(6)-Fe(1)-C(4) 123.5(3) C(7)-Fe(1)-C(4) 156.4(4) C(5)-Fe(1)-C(4) 40.3(3) C(8)-Fe(1)-C(4) 164.0(4) C(11)-O(1)-C(12) 121.6(5) C(5)-C(1)-C(2) 107.4(7) C(5)-C(1)-Br(1) 126.0(6) C(2)-C(1)-Br(1) 126.6(6) C(5)-C(1)-Fe(1) 70.6(4) C(2)-C(1)-Fe(1) 69.7(4) Br(1)-C(1)-Fe(1) 126.8(4) C(3)-C(2)-C(1) 107.2(8) C(3)-C(2)-Fe(1) 70.2(5) C(1)-C(2)-Fe(1) 69.4(4) C(2)-C(3)-C(4) 110.4(8) C(2)-C(3)-Fe(1) 70.2(5) C(4)-C(3)-Fe(1) 70.8(5) C(3)-C(4)-C(5) 107.0(8) C(3)-C(4)-Fe(1) 69.6(5) C(5)-C(4)-Fe(1) 69.8(4) C(1)-C(5)-C(4) 108.0(8) C(1)-C(5)-Fe(1) 69.1(4) C(4)-C(5)-Fe(1) 69.9(5) C(7)-C(6)-C(10) 108.8(6) C(7)-C(6)-Fe(1) 69.9(4) C(10)-C(6)-Fe(1) 69.3(4) C(8)-C(7)-C(6) 108.6(7) C(8)-C(7)-Fe(1) 70.6(4) C(6)-C(7)-Fe(1) 69.9(4) C(7)-C(8)-C(9) 109.5(7) C(7)-C(8)-Fe(1) 70.1(5) C(9)-C(8)-Fe(1) 68.2(4) C(8)-C(9)-C(10) 107.0(7) C(8)-C(9)-Fe(1) 71.0(4) C(10)-C(9)-Fe(1) 69.9(4) C(6)-C(10)-C(9) 106.0(6) C(6)-C(10)-C(11) 128.6(6) C(9)-C(10)-C(11) 125.1(6) C(6)-C(10)-Fe(1) 69.7(4) C(9)-C(10)-Fe(1) 68.1(4) C(11)-C(10)-Fe(1) 122.3(5) O(1)-C(11)-C(10) 106.6(6) O(1)-C(11)-Mo(1) 128.5(5) C(10)-C(11)-Mo(1) 124.7(5) O(2)-C(13)-Mo(1) 175.1(6) O(3)-C(14)-Mo(1) 175.0(7) O(4)-C(15)-Mo(1) 177.1(6) O(5)-C(16)-Mo(1) 175.2(7) O(6)-C(17)-Mo(1) 177.8(7) _____________________________________________________________ Table 5. Anisotropic displacement parameters (A^2 x 10^3) for 97src027. The anisotropic displacement factor exponent takes the form: -2 pi^2 [ h^2 a*^2 U11 + ... + 2 h k a* b* U12 ] _______________________________________________________________________ U11 U22 U33 U23 U13 U12 _______________________________________________________________________ Mo(1) 31(1) 27(1) 28(1) -1(1) 5(1) -1(1) Br(1) 68(1) 97(1) 63(1) 16(1) 10(1) 26(1) Fe(1) 33(1) 34(1) 33(1) -2(1) 4(1) 1(1) O(1) 41(3) 26(3) 48(3) 10(2) 8(2) 1(2) O(2) 54(3) 80(4) 40(3) 20(3) 7(3) -2(3) O(3) 103(5) 53(4) 90(5) -12(4) 53(4) 19(4) O(4) 55(4) 93(5) 70(4) 7(4) 6(3) -33(4) O(5) 83(5) 86(5) 38(4) 17(3) -6(3) 9(4) O(6) 89(5) 67(4) 67(4) -23(3) 26(3) 11(4) C(1) 53(5) 57(6) 27(4) 2(3) 3(3) 1(4) C(2) 64(6) 56(6) 51(5) -17(4) -6(4) -17(5) C(3) 109(8) 39(5) 47(5) -13(4) 0(5) 12(6) C(4) 72(6) 60(6) 44(5) -13(4) 9(4) 25(5) C(5) 47(5) 75(6) 36(4) -7(4) 13(4) 2(4) C(6) 46(4) 22(4) 36(4) -3(3) 3(3) 4(3) C(7) 41(4) 39(5) 50(5) -2(4) 14(4) 11(4) C(8) 30(4) 86(7) 48(5) -2(4) 12(3) 14(4) C(9) 37(4) 56(5) 44(4) 10(4) 14(3) -5(4) C(10) 38(4) 38(4) 28(4) -1(3) 11(3) 0(3) C(11) 37(4) 33(4) 24(3) -1(3) 6(3) 0(3) C(12) 48(4) 32(4) 54(5) 8(3) 9(4) 6(3) C(13) 33(4) 38(4) 44(5) 3(3) 7(3) -3(3) C(14) 57(5) 39(5) 43(5) 11(4) 9(4) 1(4) C(15) 54(5) 46(5) 29(4) 1(3) 2(3) -9(4) C(16) 50(5) 41(5) 56(6) 2(4) 16(4) -3(4) C(17) 48(5) 41(5) 39(4) -4(4) 7(3) -2(4) _______________________________________________________________________ Table 6. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for 97src027. ________________________________________________________________ x y z U(eq) ________________________________________________________________ H(2) 6600(9) 8505(7) 4672(6) 72 H(3) 4578(11) 9509(7) 4068(6) 81 H(4) 2720(9) 8339(7) 4135(6) 71 H(5) 3598(8) 6555(7) 4845(5) 63 H(6) 3412(7) 5736(5) 2525(5) 43 H(7) 5802(7) 5620(6) 3051(5) 51 H(8) 6734(7) 7332(7) 2657(6) 65 H(9) 4947(7) 8637(6) 2002(5) 54 H(12A) 1037(29) 9340(25) 543(14) 67 H(12B) 1765(9) 10281(8) 1177(34) 67 H(12C) 861(24) 9504(30) 1591(21) 67 ________________________________________________________________