Table 1. Crystal data and structure refinement for 95SRC149. Identification code 95SRC149 Empirical formula C24 H16 Fe Mo N2 O4 Formula weight 548.18 Temperature 150(2) K Wavelength 0.71069 A Crystal system Monoclinic Space group P2(1)/n Unit cell dimensions a = 12.839(4) A b = 12.9785(10) A c = 12.980(2) A beta = 95.693(10) deg. Volume 2152.2(7) A^3 Z 4 Density (calculated) 1.692 Mg/m^3 Absorption coefficient 1.291 mm^-1 F(000) 1096 Crystal size 0.2 x 0.14 x 0.06 mm Theta range for data collection 2.13 to 25.04 deg. Index ranges -14<=h<=13, -9<=k<=14, -14<=l<=14 Reflections collected 8753 Independent reflections 3221 [R(int) = 0.0766] Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 3215 / 0 / 289 Goodness-of-fit on F^2 0.760 Final R indices [I>2sigma(I)] R1 = 0.0409, wR2 = 0.0772 R indices (all data) R1 = 0.0751, wR2 = 0.0872 Largest diff. peak and hole 0.778 and -0.412 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for 95SRC149. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________ x y z U(eq) ________________________________________________________________ Mo(1) -121(1) 3290(1) 7135(1) 21(1) Fe(1) 412(1) 9176(1) 7848(1) 23(1) N(1) -852(3) 4147(3) 8382(3) 20(1) N(2) -1027(3) 2113(3) 8020(4) 18(1) O(1) -2092(4) 3413(3) 5464(4) 50(1) O(2) 805(4) 5209(3) 6109(4) 58(2) O(3) 740(3) 1965(3) 5414(3) 38(1) O(4) 2094(4) 2977(3) 8370(4) 39(1) C(1) 856(4) 10682(4) 7770(5) 24(2) C(2) 1464(5) 10065(4) 7159(5) 25(2) C(3) 752(5) 9571(4) 6391(5) 26(2) C(4) -270(4) 9857(4) 6538(5) 23(2) C(5) -224(4) 10568(4) 7376(4) 21(2) C(6) -427(6) 7926(5) 8220(6) 48(2) C(7) 549(6) 7596(4) 7948(5) 44(2) C(8) 1315(6) 8101(5) 8667(5) 44(2) C(9) 777(5) 8704(4) 9345(5) 33(2) C(10) -310(5) 8602(4) 9063(5) 34(2) C(11) -643(4) 5140(4) 8650(4) 21(2) C(12) -1126(4) 5638(4) 9398(4) 24(2) C(13) -1861(5) 5111(4) 9917(5) 29(2) C(14) -2074(4) 4096(4) 9665(4) 23(2) C(15) -1573(4) 3646(4) 8885(5) 20(1) C(16) -1768(4) 2552(4) 8567(4) 19(1) C(17) -2657(4) 2031(4) 8812(4) 21(1) C(18) -2787(4) 1001(4) 8483(4) 24(2) C(19) -1998(4) 527(4) 8016(4) 22(1) C(20) -1117(4) 1085(4) 7813(4) 20(1) C(21) -1430(5) 3393(4) 6091(5) 24(1) C(22) 460(5) 4485(5) 6460(5) 29(2) C(23) 427(4) 2441(4) 6069(5) 24(2) C(24) 1271(5) 3108(4) 7994(5) 25(2) ________________________________________________________________ Table 4. Bond lengths [A] and angles [deg] for 95SRC149. _____________________________________________________________ Mo(1)-C(23) 1.954(6) Mo(1)-C(22) 1.964(6) Mo(1)-C(24) 2.025(6) Mo(1)-C(21) 2.056(7) Mo(1)-N(1) 2.244(4) Mo(1)-N(2) 2.295(4) Fe(1)-C(6) 2.031(6) Fe(1)-C(4) 2.036(6) Fe(1)-C(8) 2.043(6) Fe(1)-C(1) 2.042(5) Fe(1)-C(9) 2.047(6) Fe(1)-C(10) 2.047(6) Fe(1)-C(3) 2.049(6) Fe(1)-C(2) 2.049(5) Fe(1)-C(5) 2.052(5) Fe(1)-C(7) 2.060(6) N(1)-C(15) 1.352(6) N(1)-C(11) 1.354(6) N(2)-C(20) 1.364(6) N(2)-C(16) 1.367(6) O(1)-C(21) 1.116(7) O(2)-C(22) 1.153(6) O(3)-C(23) 1.155(6) O(4)-C(24) 1.131(6) C(1)-C(2) 1.416(7) C(1)-C(5) 1.437(8) C(2)-C(3) 1.435(8) C(3)-C(4) 1.395(7) C(4)-C(5) 1.423(7) C(5)-C(20)#1 1.488(7) C(6)-C(10) 1.399(9) C(6)-C(7) 1.402(9) C(7)-C(8) 1.444(9) C(8)-C(9) 1.409(8) C(9)-C(10) 1.413(8) C(11)-C(12) 1.366(7) C(12)-C(13) 1.391(7) C(13)-C(14) 1.378(7) C(14)-C(15) 1.382(7) C(15)-C(16) 1.492(7) C(16)-C(17) 1.391(7) C(17)-C(18) 1.407(7) C(18)-C(19) 1.376(7) C(19)-C(20) 1.391(7) C(20)-C(5)#2 1.488(7) C(23)-Mo(1)-C(22) 87.1(2) C(23)-Mo(1)-C(24) 87.9(2) C(22)-Mo(1)-C(24) 89.1(2) C(23)-Mo(1)-C(21) 84.1(2) C(22)-Mo(1)-C(21) 88.7(2) C(24)-Mo(1)-C(21) 171.8(2) C(23)-Mo(1)-N(1) 174.8(2) C(22)-Mo(1)-N(1) 97.7(2) C(24)-Mo(1)-N(1) 94.0(2) C(21)-Mo(1)-N(1) 94.0(2) C(23)-Mo(1)-N(2) 102.4(2) C(22)-Mo(1)-N(2) 169.1(2) C(24)-Mo(1)-N(2) 96.3(2) C(21)-Mo(1)-N(2) 87.2(2) N(1)-Mo(1)-N(2) 72.6(2) C(6)-Fe(1)-C(4) 110.6(3) C(6)-Fe(1)-C(8) 67.6(3) C(4)-Fe(1)-C(8) 154.9(2) C(6)-Fe(1)-C(1) 159.0(3) C(4)-Fe(1)-C(1) 69.0(2) C(8)-Fe(1)-C(1) 122.2(3) C(6)-Fe(1)-C(9) 67.2(3) C(4)-Fe(1)-C(9) 164.2(2) C(8)-Fe(1)-C(9) 40.3(2) C(1)-Fe(1)-C(9) 107.2(2) C(6)-Fe(1)-C(10) 40.1(2) C(4)-Fe(1)-C(10) 127.7(2) C(8)-Fe(1)-C(10) 68.2(3) C(1)-Fe(1)-C(10) 122.5(2) C(9)-Fe(1)-C(10) 40.4(2) C(6)-Fe(1)-C(3) 125.9(3) C(4)-Fe(1)-C(3) 39.9(2) C(8)-Fe(1)-C(3) 119.3(2) C(1)-Fe(1)-C(3) 68.1(2) C(9)-Fe(1)-C(3) 154.4(3) C(10)-Fe(1)-C(3) 163.1(3) C(6)-Fe(1)-C(2) 160.3(3) C(4)-Fe(1)-C(2) 68.8(2) C(8)-Fe(1)-C(2) 104.3(3) C(1)-Fe(1)-C(2) 40.5(2) C(9)-Fe(1)-C(2) 119.0(3) C(10)-Fe(1)-C(2) 155.5(3) C(3)-Fe(1)-C(2) 41.0(2) C(6)-Fe(1)-C(5) 124.7(3) C(4)-Fe(1)-C(5) 40.7(2) C(8)-Fe(1)-C(5) 161.0(3) C(1)-Fe(1)-C(5) 41.1(2) C(9)-Fe(1)-C(5) 126.5(2) C(10)-Fe(1)-C(5) 110.7(2) C(3)-Fe(1)-C(5) 67.5(2) C(2)-Fe(1)-C(5) 68.5(2) C(6)-Fe(1)-C(7) 40.1(2) C(4)-Fe(1)-C(7) 120.8(3) C(8)-Fe(1)-C(7) 41.2(2) C(1)-Fe(1)-C(7) 158.9(3) C(9)-Fe(1)-C(7) 68.5(2) C(10)-Fe(1)-C(7) 68.4(2) C(3)-Fe(1)-C(7) 106.4(2) C(2)-Fe(1)-C(7) 122.1(3) C(5)-Fe(1)-C(7) 157.5(3) C(15)-N(1)-C(11) 117.5(5) C(15)-N(1)-Mo(1) 117.7(3) C(11)-N(1)-Mo(1) 124.8(4) C(20)-N(2)-C(16) 117.4(5) C(20)-N(2)-Mo(1) 126.2(4) C(16)-N(2)-Mo(1) 113.3(3) C(2)-C(1)-C(5) 108.0(5) C(2)-C(1)-Fe(1) 70.0(3) C(5)-C(1)-Fe(1) 69.8(3) C(1)-C(2)-C(3) 107.1(5) C(1)-C(2)-Fe(1) 69.5(3) C(3)-C(2)-Fe(1) 69.5(3) C(4)-C(3)-C(2) 109.2(5) C(4)-C(3)-Fe(1) 69.5(3) C(2)-C(3)-Fe(1) 69.5(3) C(3)-C(4)-C(5) 108.0(5) C(3)-C(4)-Fe(1) 70.5(3) C(5)-C(4)-Fe(1) 70.2(3) C(4)-C(5)-C(1) 107.7(5) C(4)-C(5)-C(20)#1 127.5(5) C(1)-C(5)-C(20)#1 124.8(5) C(4)-C(5)-Fe(1) 69.1(3) C(1)-C(5)-Fe(1) 69.1(3) C(20)#1-C(5)-Fe(1) 125.6(4) C(10)-C(6)-C(7) 111.1(7) C(10)-C(6)-Fe(1) 70.5(3) C(7)-C(6)-Fe(1) 71.1(4) C(6)-C(7)-C(8) 105.5(6) C(6)-C(7)-Fe(1) 68.9(3) C(8)-C(7)-Fe(1) 68.8(3) C(9)-C(8)-C(7) 108.1(6) C(9)-C(8)-Fe(1) 70.0(3) C(7)-C(8)-Fe(1) 70.0(4) C(8)-C(9)-C(10) 108.6(6) C(8)-C(9)-Fe(1) 69.7(4) C(10)-C(9)-Fe(1) 69.8(4) C(6)-C(10)-C(9) 106.7(6) C(6)-C(10)-Fe(1) 69.3(4) C(9)-C(10)-Fe(1) 69.8(3) N(1)-C(11)-C(12) 122.7(5) C(11)-C(12)-C(13) 119.3(5) C(14)-C(13)-C(12) 118.9(5) C(13)-C(14)-C(15) 118.8(5) N(1)-C(15)-C(14) 122.8(5) N(1)-C(15)-C(16) 115.4(5) C(14)-C(15)-C(16) 121.8(5) N(2)-C(16)-C(17) 123.1(5) N(2)-C(16)-C(15) 115.7(5) C(17)-C(16)-C(15) 121.3(5) C(16)-C(17)-C(18) 117.9(5) C(19)-C(18)-C(17) 119.2(5) C(18)-C(19)-C(20) 120.0(5) N(2)-C(20)-C(19) 121.8(5) N(2)-C(20)-C(5)#2 117.6(5) C(19)-C(20)-C(5)#2 120.7(5) O(1)-C(21)-Mo(1) 174.1(5) O(2)-C(22)-Mo(1) 176.8(6) O(3)-C(23)-Mo(1) 177.7(5) O(4)-C(24)-Mo(1) 172.1(6) _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: #1 x,y+1,z #2 x,y-1,z Table 5. Anisotropic displacement parameters (A^2 x 10^3) for 95SRC149. 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) 24(1) 18(1) 23(1) 1(1) 7(1) -1(1) Fe(1) 32(1) 15(1) 21(1) 0(1) 0(1) 1(1) N(1) 23(3) 16(3) 20(3) 0(2) 0(2) 1(2) N(2) 18(3) 15(3) 20(3) 4(2) -3(2) 1(2) O(1) 35(3) 71(3) 43(4) -1(3) 0(3) 5(3) O(2) 71(4) 43(3) 63(4) 22(3) 19(3) -18(3) O(3) 41(3) 39(3) 35(3) -4(2) 17(2) 2(2) O(4) 37(3) 30(3) 49(3) -1(2) 3(3) -6(2) C(1) 28(4) 16(4) 29(4) 7(3) 2(3) 2(3) C(2) 23(4) 16(3) 38(4) 5(3) 8(3) 1(3) C(3) 42(4) 12(3) 25(4) 4(3) 12(3) 5(3) C(4) 23(4) 20(4) 27(4) 2(3) 1(3) 1(3) C(5) 21(4) 15(3) 27(4) 6(3) 6(3) -2(2) C(6) 69(6) 32(4) 38(5) 18(3) -12(4) -34(4) C(7) 89(7) 12(4) 32(5) 5(3) 16(5) 6(4) C(8) 52(5) 37(4) 45(5) 21(4) 15(4) 23(4) C(9) 46(5) 30(4) 20(4) 3(3) -4(3) 1(3) C(10) 32(5) 37(4) 33(5) 6(3) 6(3) 0(3) C(11) 24(4) 17(4) 22(4) 8(3) 0(3) -1(3) C(12) 33(4) 16(3) 23(4) -4(3) -1(3) -3(3) C(13) 33(4) 30(4) 25(4) -8(3) 4(3) 4(3) C(14) 31(4) 13(3) 26(4) -3(3) 6(3) -4(3) C(15) 16(4) 17(3) 27(4) 3(3) -1(3) -1(2) C(16) 21(4) 20(3) 16(4) 1(2) -3(3) 2(3) C(17) 20(4) 25(4) 18(4) 0(3) -2(3) 1(2) C(18) 17(4) 22(4) 34(4) 8(3) -1(3) -6(3) C(19) 19(4) 27(3) 18(4) 0(3) -4(3) -3(3) C(20) 22(4) 14(4) 24(4) 1(3) 0(3) 2(2) C(21) 28(4) 20(3) 25(4) 1(3) 6(3) 6(3) C(22) 25(4) 36(4) 26(4) 3(3) 4(3) 0(3) C(23) 21(4) 21(4) 31(4) 2(3) 8(3) -3(3) C(24) 17(4) 17(4) 42(5) -1(3) 4(3) -4(3) _______________________________________________________________________ Table 6. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for 95SRC149. ________________________________________________________________ x y z U(eq) ________________________________________________________________ H(1) 1111(4) 11089(4) 8328(5) 29 H(2) 2188(5) 9992(4) 7240(5) 30 H(3) 942(5) 9131(4) 5876(5) 31 H(4) -875(4) 9624(4) 6156(5) 28 H(6) -1068(6) 7722(5) 7885(6) 57 H(7) 676(6) 7147(4) 7416(5) 52 H(8) 2038(6) 8039(5) 8680(5) 52 H(9) 1086(5) 9102(4) 9888(5) 39 H(10) -844(5) 8922(4) 9377(5) 41 H(11) -150(4) 5497(4) 8311(4) 25 H(12) -966(4) 6322(4) 9560(4) 29 H(13) -2202(5) 5438(4) 10425(5) 35 H(14) -2547(4) 3721(4) 10014(4) 28 H(17) -3151(4) 2352(4) 9181(4) 25 H(18) -3399(4) 646(4) 8580(4) 29 H(19) -2055(4) -166(4) 7837(4) 26 ________________________________________________________________