Table 1. Crystal data and structure refinement for 4. Empirical formula C20 H12 O6 Re2 S4 Formula weight 848.94 Temperature 150(2) K Wavelength 0.71073 A Crystal system, space group Triclinic, P-1 Unit cell dimensions a = 9.894(3) A alpha = 112.34(3) deg. b = 11.157(3) A beta = 102.53(2) deg. c = 12.166(4) A gamma = 97.69(2) deg. Volume 1177.3(6) A^3 Z, Calculated density 2, 2.395 Mg/m^3 Absorption coefficient 10.662 mm^-1 F(000) 788 Crystal size 0.25 x 0.22 x 0.20 mm Theta range for data collection 1.89 to 25.17 deg. Limiting indices -11<=h<=11, -13<=k<=12, 0<=l<=14 Reflections collected / unique 4236 / 4236 [R(int) = 0.0000] Completeness to theta = 25.17 100.0 % Max. and min. transmission 0.2243 and 0.1758 Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 4236 / 0 / 291 Goodness-of-fit on F^2 1.057 Final R indices [I>2sigma(I)] R1 = 0.0310, wR2 = 0.0834 R indices (all data) R1 = 0.0363, wR2 = 0.0853 Largest diff. peak and hole 1.681 and -1.329 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for 4. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________ x y z U(eq) ________________________________________________________________ Re(1) 5210(1) 3407(1) 1996(1) 29(1) Re(2) 1833(1) 3001(1) 2732(1) 29(1) S(1) 3021(2) 4247(2) 1692(2) 31(1) S(2) 3555(2) 1345(2) 417(2) 32(1) S(3) 4371(2) 3200(2) 3760(1) 29(1) S(4) 2089(2) 830(2) 1419(2) 33(1) O(1) 6124(7) 3848(6) -100(6) 63(2) O(2) 7190(8) 6167(6) 3708(6) 72(2) O(3) 7554(6) 1983(6) 2511(7) 62(2) O(4) 421(6) 1687(6) 4154(5) 53(1) O(5) 1682(7) 5656(6) 4704(5) 62(2) O(6) -1000(6) 2763(7) 938(6) 63(2) C(1) 5765(8) 3685(7) 690(7) 39(2) C(2) 6458(8) 5129(8) 3095(7) 41(2) C(3) 6713(7) 2534(7) 2312(7) 40(2) C(4) 978(8) 2161(7) 3610(6) 39(2) C(5) 1733(8) 4690(7) 3951(7) 39(2) C(6) 23(7) 2845(8) 1648(7) 38(2) C(7) 2150(7) 3207(7) 90(6) 32(1) C(8) 2352(7) 1925(7) -457(6) 36(2) C(9) 1618(8) 1078(7) -1686(6) 41(2) C(10) 691(9) 1541(8) -2364(7) 49(2) C(11) 499(8) 2827(8) -1844(7) 45(2) C(12) 1219(7) 3644(7) -616(6) 38(2) C(13) -450(11) 3321(10) -2614(8) 68(3) C(14) 4423(7) 1511(7) 3410(6) 35(2) C(15) 3412(7) 462(7) 2394(6) 36(1) C(16) 3537(9) -847(7) 2073(7) 45(2) C(17) 4671(10) -1109(8) 2775(8) 52(2) C(18) 5686(8) -92(8) 3768(7) 43(2) C(19) 5546(7) 1214(7) 4086(6) 37(2) C(20) 6958(9) -380(10) 4472(8) 57(2) ________________________________________________________________ Table 3. Bond lengths [A] and angles [deg] for 4. _______________________________________________________ Re(1)-C(1) 1.906(7) Re(1)-C(2) 1.923(8) Re(1)-C(3) 1.932(7) Re(1)-S(2) 2.436(2) Re(1)-S(1) 2.4827(17) Re(1)-S(3) 2.5393(18) Re(2)-C(4) 1.918(8) Re(2)-C(6) 1.921(7) Re(2)-C(5) 1.936(8) Re(2)-S(4) 2.4252(19) Re(2)-S(3) 2.4892(17) Re(2)-S(1) 2.5419(17) S(1)-C(7) 1.780(7) S(2)-C(8) 1.774(6) S(2)-S(4) 2.235(2) S(3)-C(14) 1.777(7) S(4)-C(15) 1.769(7) O(1)-C(1) 1.160(9) O(2)-C(2) 1.143(9) O(3)-C(3) 1.137(9) O(4)-C(4) 1.170(9) O(5)-C(5) 1.135(9) O(6)-C(6) 1.147(9) C(7)-C(12) 1.385(9) C(7)-C(8) 1.392(9) C(8)-C(9) 1.388(10) C(9)-C(10) 1.382(10) C(10)-C(11) 1.389(11) C(11)-C(12) 1.378(10) C(11)-C(13) 1.488(10) C(14)-C(19) 1.389(9) C(14)-C(15) 1.396(10) C(15)-C(16) 1.392(10) C(16)-C(17) 1.391(11) C(17)-C(18) 1.372(12) C(18)-C(19) 1.394(10) C(18)-C(20) 1.506(10) C(1)-Re(1)-C(2) 86.4(3) C(1)-Re(1)-C(3) 94.0(3) C(2)-Re(1)-C(3) 91.0(3) C(1)-Re(1)-S(2) 87.8(2) C(2)-Re(1)-S(2) 172.8(2) C(3)-Re(1)-S(2) 93.7(2) C(1)-Re(1)-S(1) 94.6(2) C(2)-Re(1)-S(1) 95.4(2) C(3)-Re(1)-S(1) 169.6(2) S(2)-Re(1)-S(1) 80.79(6) C(1)-Re(1)-S(3) 175.2(2) C(2)-Re(1)-S(3) 91.6(2) C(3)-Re(1)-S(3) 90.5(2) S(2)-Re(1)-S(3) 93.81(6) S(1)-Re(1)-S(3) 81.16(6) C(4)-Re(2)-C(6) 93.1(3) C(4)-Re(2)-C(5) 87.5(3) C(6)-Re(2)-C(5) 91.1(3) C(4)-Re(2)-S(4) 87.9(2) C(6)-Re(2)-S(4) 94.5(2) C(5)-Re(2)-S(4) 173.0(2) C(4)-Re(2)-S(3) 97.8(2) C(6)-Re(2)-S(3) 167.7(2) C(5)-Re(2)-S(3) 94.8(2) S(4)-Re(2)-S(3) 80.50(6) C(4)-Re(2)-S(1) 176.4(2) C(6)-Re(2)-S(1) 88.4(2) C(5)-Re(2)-S(1) 89.3(2) S(4)-Re(2)-S(1) 95.19(6) S(3)-Re(2)-S(1) 80.99(6) C(7)-S(1)-Re(1) 100.7(2) C(7)-S(1)-Re(2) 101.7(2) Re(1)-S(1)-Re(2) 93.39(6) C(8)-S(2)-S(4) 96.7(2) C(8)-S(2)-Re(1) 102.7(2) S(4)-S(2)-Re(1) 103.37(8) C(14)-S(3)-Re(2) 102.5(2) C(14)-S(3)-Re(1) 98.5(2) Re(2)-S(3)-Re(1) 93.30(6) C(15)-S(4)-S(2) 94.1(2) C(15)-S(4)-Re(2) 104.9(2) S(2)-S(4)-Re(2) 102.46(8) O(1)-C(1)-Re(1) 178.9(7) O(2)-C(2)-Re(1) 177.2(7) O(3)-C(3)-Re(1) 176.8(6) O(4)-C(4)-Re(2) 177.2(6) O(5)-C(5)-Re(2) 177.0(6) O(6)-C(6)-Re(2) 174.6(6) C(12)-C(7)-C(8) 119.1(6) C(12)-C(7)-S(1) 120.3(5) C(8)-C(7)-S(1) 120.5(5) C(9)-C(8)-C(7) 121.1(6) C(9)-C(8)-S(2) 118.8(5) C(7)-C(8)-S(2) 120.1(5) C(10)-C(9)-C(8) 118.4(7) C(9)-C(10)-C(11) 121.4(7) C(12)-C(11)-C(10) 119.2(7) C(12)-C(11)-C(13) 120.6(7) C(10)-C(11)-C(13) 120.2(7) C(11)-C(12)-C(7) 120.8(7) C(19)-C(14)-C(15) 118.4(6) C(19)-C(14)-S(3) 120.2(5) C(15)-C(14)-S(3) 121.2(5) C(16)-C(15)-C(14) 120.4(6) C(16)-C(15)-S(4) 120.2(6) C(14)-C(15)-S(4) 119.1(5) C(17)-C(16)-C(15) 119.7(7) C(18)-C(17)-C(16) 120.9(7) C(17)-C(18)-C(19) 118.9(7) C(17)-C(18)-C(20) 120.5(7) C(19)-C(18)-C(20) 120.6(7) C(14)-C(19)-C(18) 121.7(7) ____________________________________________________________ Table 4. Anisotropic displacement parameters (A^2 x 10^3) for 4. 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 _______________________________________________________________________ Re(1) 25(1) 30(1) 30(1) 14(1) 6(1) 4(1) Re(2) 24(1) 32(1) 29(1) 13(1) 5(1) 4(1) S(1) 31(1) 28(1) 31(1) 13(1) 6(1) 6(1) S(2) 33(1) 30(1) 30(1) 11(1) 5(1) 8(1) S(3) 26(1) 30(1) 29(1) 12(1) 4(1) 2(1) S(4) 32(1) 30(1) 33(1) 13(1) 4(1) 2(1) O(1) 81(4) 60(4) 50(3) 26(3) 30(3) 1(3) O(2) 80(5) 45(3) 58(4) 9(3) 4(3) -20(3) O(3) 45(3) 71(4) 95(5) 51(4) 28(3) 32(3) O(4) 51(3) 53(3) 51(3) 26(3) 14(3) -9(3) O(5) 80(4) 48(3) 48(3) 10(3) 15(3) 28(3) O(6) 37(3) 102(5) 55(4) 41(4) 7(3) 15(3) C(1) 39(4) 32(3) 37(4) 12(3) 8(3) -8(3) C(2) 41(4) 47(4) 37(4) 21(3) 10(3) 7(3) C(3) 30(4) 43(4) 45(4) 18(3) 11(3) 7(3) C(4) 37(4) 37(4) 28(3) 3(3) 1(3) 12(3) C(5) 39(4) 39(4) 38(4) 19(3) 6(3) 8(3) C(6) 28(3) 49(4) 35(4) 20(3) 5(3) 8(3) C(7) 35(3) 33(3) 28(3) 14(3) 8(3) 6(3) C(8) 39(4) 38(4) 34(4) 21(3) 7(3) 11(3) C(9) 47(4) 39(4) 31(4) 12(3) 3(3) 9(3) C(10) 54(5) 50(4) 34(4) 14(3) 1(3) 10(4) C(11) 40(4) 55(5) 42(4) 28(4) 3(3) 12(3) C(12) 40(4) 39(4) 37(4) 20(3) 3(3) 12(3) C(13) 75(6) 64(6) 50(5) 22(4) -13(5) 24(5) C(14) 39(4) 39(4) 35(4) 24(3) 12(3) 8(3) C(15) 36(4) 38(4) 39(4) 23(3) 10(3) 8(3) C(16) 57(5) 36(4) 37(4) 11(3) 11(3) 8(3) C(17) 70(6) 41(4) 59(5) 29(4) 27(4) 22(4) C(18) 47(4) 54(4) 48(4) 35(4) 20(3) 22(4) C(19) 33(4) 48(4) 35(4) 26(3) 6(3) 7(3) C(20) 55(5) 73(6) 62(5) 41(5) 19(4) 30(5) _______________________________________________________________________