Table 1. Crystal data and structure refinement for 96SRC233. Identification code 96SRC233 Empirical formula C31 H22 Cl2 I3 Mo N O3 P Formula weight 1035.01 Temperature 293(2) K Wavelength 0.71069 A Crystal system Triclinic Space group P-1 Unit cell dimensions a = 10.54(2) A alpha = 74.90(5) deg. b = 11.21(2) A beta = 77.50(7) deg. c = 16.580(4) A gamma = 72.15(5) deg. Volume 1780(5) A^3 Z 2 Density (calculated) 1.931 Mg/m^3 Absorption coefficient 3.196 mm^-1 F(000) 978 Crystal size 0.24 x 0.14 x 0.14 mm Theta range for data collection 1.95 to 24.72 deg. Index ranges -10<=h<=10, -12<=k<=11, -19<=l<=19 Reflections collected 5101 Independent reflections 3518 [R(int) = 0.0532] Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 3515 / 0 / 379 Goodness-of-fit on F^2 0.930 Final R indices [I>2sigma(I)] R1 = 0.0562, wR2 = 0.1324 R indices (all data) R1 = 0.0804, wR2 = 0.1445 Largest diff. peak and hole 1.875 and -0.813 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for 96SRC233.U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________ x y z U(eq) ________________________________________________________________ Mo(1) -1626(1) 10563(1) 2285(1) 33(1) Cl(1) -6680(7) 9151(6) 3594(4) 110(3) Cl(2) -5351(6) 7013(6) 4810(4) 119(3) I(1) 1099(1) 9057(1) 1862(1) 48(1) I(2) -2367(1) 8174(1) 2914(1) 58(1) I(3) -973(1) 10492(1) 3916(1) 60(1) P(1) -2974(4) 12481(3) 1390(2) 34(1) N(1) 939(17) 6726(14) 3866(10) 70(6) O(1) -1760(13) 9701(9) 644(7) 67(4) O(2) 129(14) 12516(11) 1899(8) 70(4) O(3) -4412(13) 11320(10) 3442(7) 69(4) C(1) -1733(16) 9996(13) 1227(9) 38(4) C(2) -531(20) 11858(14) 2022(11) 52(6) C(3) -3350(17) 11086(12) 2994(9) 41(5) C(4) -4228(15) 12142(12) 931(8) 39(5) C(5) -5163(23) 11537(16) 1432(13) 68(6) C(6) -6038(23) 11207(19) 1115(16) 84(8) C(7) -6074(21) 11446(18) 257(17) 83(7) C(8) -5109(30) 12062(18) -271(14) 96(10) C(9) -4169(21) 12391(15) 70(10) 55(5) C(10) -1984(15) 13311(11) 475(8) 30(4) C(11) -2400(15) 14608(13) 170(9) 40(5) C(12) -1673(20) 15230(15) -506(11) 74(7) C(13) -476(19) 14531(14) -902(10) 64(7) C(14) -30(17) 13257(12) -622(10) 48(5) C(15) -814(18) 12633(13) 87(8) 56(6) C(16) -3981(16) 13789(13) 1908(9) 39(5) C(17) -3436(20) 14136(14) 2478(11) 63(6) C(18) -4120(25) 15199(17) 2855(11) 85(8) C(19) -5339(26) 15878(19) 2629(13) 90(10) C(20) -5912(21) 15575(15) 2063(12) 73(8) C(21) -5209(17) 14499(14) 1723(9) 50(5) C(22) 1119(21) 7033(18) 4548(14) 72(7) C(23) 1574(22) 6162(16) 5167(13) 75(7) C(24) 1947(20) 4914(17) 5182(12) 66(6) C(25) 1799(22) 4499(14) 4510(11) 68(7) C(26) 2084(23) 3144(17) 4422(16) 78(8) C(27) 1889(28) 2890(23) 3746(17) 109(11) C(28) 1406(27) 3868(27) 3085(20) 117(10) C(29) 1076(24) 5122(22) 3107(13) 83(8) C(30) 1226(18) 5404(20) 3826(11) 60(6) C(31) -5737(22) 8698(19) 4536(14) 97(9) ________________________________________________________________ Table 4. Bond lengths [A] and angles [deg] for 96SRC233. _____________________________________________________________ Mo(1)-C(3) 1.95(2) Mo(1)-C(2) 2.03(2) Mo(1)-C(1) 2.05(2) Mo(1)-P(1) 2.494(5) Mo(1)-I(2) 2.889(6) Mo(1)-I(1) 2.892(5) Mo(1)-I(3) 2.908(2) Cl(1)-C(31) 1.91(3) Cl(2)-C(31) 1.76(2) P(1)-C(16) 1.822(14) P(1)-C(4) 1.83(2) P(1)-C(10) 1.852(14) N(1)-C(22) 1.33(3) N(1)-C(30) 1.43(3) O(1)-C(1) 1.11(2) O(2)-C(2) 1.11(2) O(3)-C(3) 1.20(2) C(4)-C(9) 1.37(2) C(4)-C(5) 1.37(2) C(5)-C(6) 1.34(3) C(6)-C(7) 1.38(3) C(7)-C(8) 1.42(3) C(8)-C(9) 1.42(3) C(10)-C(15) 1.36(2) C(10)-C(11) 1.37(2) C(11)-C(12) 1.37(2) C(12)-C(13) 1.39(2) C(13)-C(14) 1.35(2) C(14)-C(15) 1.43(2) C(16)-C(21) 1.35(2) C(16)-C(17) 1.39(3) C(17)-C(18) 1.41(2) C(18)-C(19) 1.35(3) C(19)-C(20) 1.38(3) C(20)-C(21) 1.40(2) C(22)-C(23) 1.28(2) C(23)-C(24) 1.33(2) C(24)-C(25) 1.37(3) C(25)-C(30) 1.41(2) C(25)-C(26) 1.49(3) C(26)-C(27) 1.30(3) C(27)-C(28) 1.39(3) C(28)-C(29) 1.35(3) C(29)-C(30) 1.36(3) C(3)-Mo(1)-C(2) 112.6(6) C(3)-Mo(1)-C(1) 115.1(7) C(2)-Mo(1)-C(1) 112.4(7) C(3)-Mo(1)-P(1) 74.5(4) C(2)-Mo(1)-P(1) 76.1(5) C(1)-Mo(1)-P(1) 73.7(4) C(3)-Mo(1)-I(2) 78.2(4) C(2)-Mo(1)-I(2) 160.1(5) C(1)-Mo(1)-I(2) 75.0(4) P(1)-Mo(1)-I(2) 123.7(2) C(3)-Mo(1)-I(1) 157.0(4) C(2)-Mo(1)-I(1) 76.9(5) C(1)-Mo(1)-I(1) 77.4(4) P(1)-Mo(1)-I(1) 128.46(11) I(2)-Mo(1)-I(1) 87.32(14)C(3)-Mo(1)-I(3) 74.2(5) C(2)-Mo(1)-I(3) 76.1(5) C(1)-Mo(1)-I(3) 161.1(3) P(1)-Mo(1)-I(3) 125.23(13)I(2)-Mo(1)-I(3) 91.77(8) I(1)-Mo(1)-I(3) 88.72(11)C(16)-P(1)-C(4) 102.5(8) C(16)-P(1)-C(10) 102.1(6) C(4)-P(1)-C(10) 104.5(7) C(16)-P(1)-Mo(1) 116.6(5) C(4)-P(1)-Mo(1) 114.1(4) C(10)-P(1)-Mo(1) 115.3(5) C(22)-N(1)-C(30) 120(2) O(1)-C(1)-Mo(1) 178(2) O(2)-C(2)-Mo(1) 176(2) O(3)-C(3)-Mo(1) 175.4(12) C(9)-C(4)-C(5) 119(2) C(9)-C(4)-P(1) 120.1(14) C(5)-C(4)-P(1) 120.9(14) C(6)-C(5)-C(4) 123(2) C(5)-C(6)-C(7) 123(2) C(6)-C(7)-C(8) 116(3) C(7)-C(8)-C(9) 121(2) C(4)-C(9)-C(8) 119(2) C(15)-C(10)-C(11) 118.3(12) C(15)-C(10)-P(1) 120.0(9) C(11)-C(10)-P(1) 121.7(10) C(12)-C(11)-C(10) 122.1(13) C(11)-C(12)-C(13) 119.4(13) C(14)-C(13)-C(12) 120.4(13) C(13)-C(14)-C(15) 118.9(13) C(10)-C(15)-C(14) 120.9(12) C(21)-C(16)-C(17) 118(2) C(21)-C(16)-P(1) 123(2) C(17)-C(16)-P(1) 119.3(12) C(16)-C(17)-C(18) 122(2) C(19)-C(18)-C(17) 117(2) C(18)-C(19)-C(20) 123(2) C(19)-C(20)-C(21) 118(2) C(16)-C(21)-C(20) 122(2) C(23)-C(22)-N(1) 121(2) C(22)-C(23)-C(24) 125(2) C(23)-C(24)-C(25) 119(2) C(24)-C(25)-C(30) 119(2) C(24)-C(25)-C(26) 127(2) C(30)-C(25)-C(26) 113(2) C(27)-C(26)-C(25) 121(2) C(26)-C(27)-C(28) 121(3) C(29)-C(28)-C(27) 123(3) C(28)-C(29)-C(30) 116(2) C(29)-C(30)-C(25) 125(2) C(29)-C(30)-N(1) 119(2) C(25)-C(30)-N(1) 116(2) Cl(2)-C(31)-Cl(1) 104.5(14) _____________________________________________________________ Table 5. Anisotropic displacement parameters (A^2 x 10^3) for 96SRC233. 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) 42(1) 25(1) 31(1) -2(1) -8(1) -9(1) Cl(1) 99(6) 107(5) 122(5) -27(4) -21(4) -18(4) Cl(2) 81(5) 129(5) 135(5) -1(4) -20(4) -32(4) I(1) 44(1) 45(1) 51(1) -11(1) -4(1) -8(1) I(2) 66(1) 39(1) 65(1) 4(1) -3(1) -24(1) I(3) 70(1) 65(1) 43(1) -19(1) -19(1) -2(1) P(1) 43(3) 29(2) 34(2) -6(2) -11(2) -10(2) N(1) 75(13) 52(10) 77(11) 0(8) -18(10) -19(9) O(1) 99(11) 43(7) 49(7) -15(6) -16(7) 3(7) O(2) 89(11) 54(8) 76(9) 4(7) -17(8) -46(7) O(3) 69(9) 68(8) 57(7) -12(6) 12(7) -14(7) C(1) 52(11) 28(8) 37(8) -7(7) -17(7) -6(7) C(2) 66(14) 21(8) 64(11) 0(8) -10(10) -13(8) C(3) 55(12) 34(8) 41(8) -9(7) -19(8) -10(8) C(4) 46(11) 30(8) 38(8) -4(6) -17(7) -1(7) C(5) 84(17) 63(12) 72(13) 13(10) -40(12) -45(12) C(6) 62(17) 77(15) 114(19) -10(14) -19(14) -24(13) C(7) 60(17) 57(12) 135(22) -19(14) -55(14) 4(12) C(8) 145(27) 59(14) 71(14) -22(11) -18(16) -1(14) C(9) 81(16) 60(11) 51(10) -12(8) -37(10) -37(11) C(10) 35(10) 25(7) 42(8) -9(6) -22(7) -14(7) C(11) 35(11) 42(9) 44(8) -3(7) -9(7) -13(7) C(12) 86(15) 38(9) 73(12) 3(9) 7(11) -6(9) C(13) 93(16) 44(10) 50(10) 8(8) 4(11) -36(10) C(14) 58(13) 29(8) 61(10) -14(7) -6(9) -13(8) C(15) 88(14) 26(8) 34(8) -3(6) 12(9) -5(8) C(16) 42(11) 34(8) 43(9) -8(7) -10(8) -10(8) C(17) 69(15) 41(10) 83(13) -16(9) -30(11) -5(10) C(18) 135(23) 56(12) 76(13) -34(10) -49(13) -4(14) C(19) 114(23) 62(14) 78(14) -27(12) 10(15) -5(14) C(20) 70(16) 46(11) 84(14) -21(10) -5(12) 13(10) C(21) 57(13) 52(10) 52(9) -17(8) -18(9) -20(10) C(22) 75(16) 52(12) 93(15) 0(12) -19(13) -29(11) C(23) 103(19) 40(11) 101(15) -12(11) -47(14) -27(11) C(24) 76(16) 63(13) 71(13) 1(10) -40(11) -29(11) C(25) 101(18) 36(10) 57(11) -2(9) -5(11) -15(10) C(26) 84(19) 51(12) 120(19) -26(12) -23(15) -37(11) C(27) 122(25) 70(15) 130(22) -45(16) -36(18) 15(16) C(28) 90(23) 122(23) 188(30) -73(22) -64(20) -35(19) C(29) 89(18) 94(17) 74(14) -9(12) -37(12) -25(14) C(30) 29(12) 98(16) 59(11) -13(11) -19(8) -19(11) C(31) 90(20) 73(14) 120(18) -12(13) -18(15) -14(13) _______________________________________________________________________ Table 6. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for 96SRC233. ________________________________________________________________ x y z U(eq) ________________________________________________________________ H(5) -5188(23) 11350(16) 2015(13) 82 H(6) -6649(23) 10800(19) 1487(16) 101 H(7) -6690(21) 11217(18) 41(17) 99 H(8) -5092(30) 12255(18) -853(14) 115 H(9) -3522(21) 12771(15) -284(10) 66 H(11) -3200(15) 15079(13) 431(9) 48 H(12) -1975(20) 16111(15) -697(11) 89 H(13) 18(19) 14947(14) -1364(10) 77 H(14) 771(17) 12790(12) -884(10) 58 H(15) -517(18) 11753(13) 284(8) 67 H(17) -2592(20) 13650(14) 2615(11) 76 H(18) -3751(25) 15421(17) 3238(11) 101 H(19) -5814(26) 16583(19) 2868(13) 109 H(20) -6743(21) 16074(15) 1912(12) 88 H(21) -5601(17) 14265(14) 1357(9) 59 H(22) 911(21) 7891(18) 4576(14) 86 H(23) 1648(22) 6423(16) 5639(13) 90 H(24) 2303(20) 4330(17) 5642(12) 79 H(26) 2405(23) 2475(17) 4857(16) 93 H(27) 2074(28) 2041(23) 3702(17) 131 H(28) 1306(27) 3646(27) 2604(20) 140 H(29) 764(24) 5760(22) 2655(13) 100 ________________________________________________________________