Table 1. Crystal data and structure refinement for 94src190. Identification code 94src190 Empirical formula C50 H45 Cl3 N P Pd Formula weight 458.80 Temperature 150(2) K Wavelength 0.71069 A Crystal system Monoclinic Space group P21 Unit cell dimensions a = 10.227(3) A b = 18.698(3) A c = 11.133(4) A beta = 93.41(4) deg. Volume 2125.1(10) A^3 Z 2 Density (calculated) 1.434 Mg/m^3 Absorption coefficient 0.701 mm^-1 F(000) 942 Crystal size 0.18 x 0.14 x 0.14 mm Theta range for data collection 1.83 to 25.05 deg. Index ranges -10<=h<=11, -15<=k<=16, -7<=l<=12 Reflections collected 5717 Independent reflections 5336 [R(int) = 0.0547] Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 5333 / 1 / 517 Goodness-of-fit on F^2 1.068 Final R indices [I>2sigma(I)] R1 = 0.0413, wR2 = 0.1075 R indices (all data) R1 = 0.0434, wR2 = 0.1097 Absolute structure parameter -0.02(3) Largest diff. peak and hole 1.045 and -0.428 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for 94src190.U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________ x y z U(eq) ________________________________________________________________ Pd(1) 918(1) -3(1) 8237(1) 19(1) P(1) 121(2) -689(1) 9703(1) 19(1) N(1) 1523(5) 806(3) 7013(5) 22(1) N(2) -181(6) -2141(3) 7723(5) 27(1) Cl(1) 3000(1) -49(1) 9353(1) 27(1) Cl(2) 3407(2) 30(2) 2804(2) 68(1) Cl(3) 5707(2) -894(2) 2824(2) 78(1) C(1) -1530(6) -1085(4) 9678(6) 26(2) C(2) -1734(7) -1812(4) 9911(6) 29(2) C(3) -2988(8) -2076(5) 9935(8) 47(2) C(4) -4057(9) -1619(6) 9718(9) 60(3) C(5) -3844(7) -911(5) 9471(7) 49(3) C(6) -2589(6) -633(4) 9456(6) 34(2) C(7) 25(6) -110(5) 11067(5) 26(2) C(8) -668(7) -357(4) 12042(7) 37(2) C(9) -815(8) 85(6) 13008(6) 42(2) C(10) -276(8) 754(5) 13021(7) 47(2) C(11) 418(8) 994(4) 12062(7) 39(2) C(12) 553(7) 548(4) 11098(6) 34(2) C(13) 1219(6) -1448(3) 10127(6) 18(1) C(14) 1788(6) -1498(4) 11303(6) 27(2) C(15) 2631(6) -2028(4) 11653(6) 27(2) C(16) 2913(6) -2574(4) 10820(7) 30(2) C(17) 3748(7) -3157(4) 11153(8) 42(2) C(18) 4015(10) -3672(6) 10351(10) 60(3) C(19) 3459(9) -3635(5) 9185(9) 61(3) C(20) 2667(8) -3088(4) 8813(7) 42(2) C(21) 2348(7) -2537(4) 9640(7) 28(2) C(22) 1499(6) -1951(4) 9270(6) 22(2) C(23) 997(7) -1911(4) 7990(6) 22(2) C(24) 1860(7) -1649(3) 7105(6) 28(2) C(25) 3145(8) -1442(4) 7398(8) 34(2) C(26) 3973(8) -1234(4) 6563(7) 43(2) C(27) 3498(9) -1195(4) 5350(8) 49(2) C(28) 2230(8) -1367(4) 5029(7) 41(2) C(29) 1384(8) -1602(4) 5881(6) 31(2) C(30) 32(7) -1810(4) 5605(6) 31(2) C(31) -594(9) -1770(4) 4442(7) 42(2) C(32) -1856(9) -1985(4) 4225(8) 47(2) C(33) -2584(8) -2244(4) 5168(8) 46(2) C(34) -1990(7) -2306(4) 6294(7) 35(2) C(35) -690(7) -2089(4) 6539(6) 30(2) C(36) 2706(7) 1227(4) 7443(7) 39(2) C(37) 1811(7) 488(4) 5855(6) 29(2) C(38) 339(6) 1273(3) 6856(6) 23(2) C(39) 181(8) 1778(4) 7933(7) 30(2) C(40) -831(6) 784(4) 6661(5) 20(2) C(41) -738(6) 121(4) 7202(5) 16(2) C(42) -1693(7) -380(4) 6915(6) 24(2) C(43) -2755(7) -242(4) 6152(6) 28(2) C(44) -2958(6) 453(4) 5671(6) 28(2) C(45) -4077(7) 637(4) 4939(7) 36(2) C(46) -4245(7) 1309(5) 4460(7) 42(2) C(47) -3275(7) 1825(4) 4688(7) 37(2) C(48) -2161(7) 1669(4) 5386(6) 25(2) C(49) -1955(6) 981(4) 5914(6) 22(2) C(50) 4635(10) -370(5) 1948(9) 70(3) ________________________________________________________________ Table 3. Selected bond lengths [A] and angles [deg] for 1. _____________________________________________________________ _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: Table 4. Bond lengths [A] and angles [deg] for 94src190. _____________________________________________________________ Pd(1)-C(41) 2.004(6) Pd(1)-N(1) 2.150(5) Pd(1)-P(1) 2.266(2) Pd(1)-Cl(1) 2.403(2) P(1)-C(1) 1.842(7) P(1)-C(13) 1.854(6) P(1)-C(7) 1.872(7) N(1)-C(37) 1.465(8) N(1)-C(38) 1.495(8) N(1)-C(36) 1.498(9) N(2)-C(23) 1.298(9) N(2)-C(35) 1.391(9) Cl(2)-C(50) 1.785(11) Cl(3)-C(50) 1.727(9) C(1)-C(6) 1.384(9) C(1)-C(2) 1.401(10) C(2)-C(3) 1.376(10) C(3)-C(4) 1.397(13) C(4)-C(5) 1.372(13) C(5)-C(6) 1.386(10) C(7)-C(12) 1.343(11) C(7)-C(8) 1.409(9) C(8)-C(9) 1.372(11) C(9)-C(10) 1.367(13) C(10)-C(11) 1.390(12) C(11)-C(12) 1.372(10) C(13)-C(22) 1.381(9) C(13)-C(14) 1.404(9) C(14)-C(15) 1.356(9) C(15)-C(16) 1.420(10) C(16)-C(21) 1.405(10) C(16)-C(17) 1.421(10) C(17)-C(18) 1.352(12) C(18)-C(19) 1.388(13) C(19)-C(20) 1.355(11) C(20)-C(21) 1.432(10) C(21)-C(22) 1.443(10) C(22)-C(23) 1.488(9) C(23)-C(24) 1.446(9) C(24)-C(25) 1.390(11) C(24)-C(29) 1.421(10) C(25)-C(26) 1.351(10) C(26)-C(27) 1.410(12) C(27)-C(28) 1.363(12) C(28)-C(29) 1.392(10) C(29)-C(30) 1.452(10) C(30)-C(31) 1.412(10) C(30)-C(35) 1.410(10) C(31)-C(32) 1.359(12) C(32)-C(33) 1.409(12) C(33)-C(34) 1.364(11) C(34)-C(35) 1.402(10) C(38)-C(40) 1.511(9) C(38)-C(39) 1.542(9) C(40)-C(41) 1.379(10) C(40)-C(49) 1.427(9) C(41)-C(42) 1.377(9) C(42)-C(43) 1.363(10) C(43)-C(44) 1.417(10) C(44)-C(45) 1.408(10) C(44)-C(49) 1.438(9) C(45)-C(46) 1.371(11) C(46)-C(47) 1.397(11) C(47)-C(48) 1.373(10) C(48)-C(49) 1.425(9) C(41)-Pd(1)-N(1) 79.7(2) C(41)-Pd(1)-P(1) 98.7(2) N(1)-Pd(1)-P(1) 169.7(2) C(41)-Pd(1)-Cl(1) 173.8(2) N(1)-Pd(1)-Cl(1) 94.2(2) P(1)-Pd(1)-Cl(1) 87.28(7) C(1)-P(1)-C(13) 103.7(3) C(1)-P(1)-C(7) 98.8(3) C(13)-P(1)-C(7) 107.2(3) C(1)-P(1)-Pd(1) 125.8(2) C(13)-P(1)-Pd(1) 112.2(2) C(7)-P(1)-Pd(1) 107.2(3) C(37)-N(1)-C(38) 109.7(5) C(37)-N(1)-C(36) 107.1(5) C(38)-N(1)-C(36) 111.4(5) C(37)-N(1)-Pd(1) 110.6(4) C(38)-N(1)-Pd(1) 102.9(4) C(36)-N(1)-Pd(1) 115.1(4) C(23)-N(2)-C(35) 118.9(6) C(6)-C(1)-C(2) 120.1(6) C(6)-C(1)-P(1) 117.7(6) C(2)-C(1)-P(1) 122.2(5) C(3)-C(2)-C(1) 120.1(7) C(2)-C(3)-C(4) 119.9(8) C(5)-C(4)-C(3) 119.5(8) C(4)-C(5)-C(6) 121.5(8) C(1)-C(6)-C(5) 119.0(8) C(12)-C(7)-C(8) 120.0(7) C(12)-C(7)-P(1) 120.7(5) C(8)-C(7)-P(1) 119.2(6) C(9)-C(8)-C(7) 119.3(8) C(10)-C(9)-C(8) 119.7(7) C(9)-C(10)-C(11) 120.8(7) C(12)-C(11)-C(10) 118.9(8) C(7)-C(12)-C(11) 121.2(7) C(22)-C(13)-C(14) 120.5(6) C(22)-C(13)-P(1) 119.5(5) C(14)-C(13)-P(1) 119.9(5) C(15)-C(14)-C(13) 122.5(6) C(14)-C(15)-C(16) 119.2(6) C(21)-C(16)-C(15) 119.2(6) C(21)-C(16)-C(17) 119.2(7) C(15)-C(16)-C(17) 121.6(7) C(18)-C(17)-C(16) 121.1(8) C(17)-C(18)-C(19) 119.6(9) C(20)-C(19)-C(18) 121.9(8) C(19)-C(20)-C(21) 120.1(8) C(16)-C(21)-C(20) 118.0(6) C(16)-C(21)-C(22) 120.7(6) C(20)-C(21)-C(22) 121.3(6) C(13)-C(22)-C(21) 117.8(6) C(13)-C(22)-C(23) 123.6(6) C(21)-C(22)-C(23) 118.6(6) N(2)-C(23)-C(24) 123.5(6) N(2)-C(23)-C(22) 117.7(6) C(24)-C(23)-C(22) 118.7(6) C(25)-C(24)-C(29) 118.2(7) C(25)-C(24)-C(23) 122.7(7) C(29)-C(24)-C(23) 119.1(6) C(26)-C(25)-C(24) 122.8(8) C(25)-C(26)-C(27) 118.6(8) C(28)-C(27)-C(26) 120.5(7) C(27)-C(28)-C(29) 121.0(8) C(28)-C(29)-C(24) 118.8(7) C(28)-C(29)-C(30) 124.2(7) C(24)-C(29)-C(30) 117.0(6) C(31)-C(30)-C(35) 117.9(7) C(31)-C(30)-C(29) 123.6(7) C(35)-C(30)-C(29) 118.4(6) C(32)-C(31)-C(30) 121.4(8) C(31)-C(32)-C(33) 120.5(8) C(34)-C(33)-C(32) 119.2(8) C(33)-C(34)-C(35) 121.3(8) N(2)-C(35)-C(34) 117.5(7) N(2)-C(35)-C(30) 122.8(7) C(34)-C(35)-C(30) 119.7(7) N(1)-C(38)-C(40) 107.0(5) N(1)-C(38)-C(39) 112.9(5) C(40)-C(38)-C(39) 111.4(5) C(41)-C(40)-C(49) 121.3(6) C(41)-C(40)-C(38) 116.6(6) C(49)-C(40)-C(38) 122.1(6) C(42)-C(41)-C(40) 118.7(6) C(42)-C(41)-Pd(1) 128.2(5) C(40)-C(41)-Pd(1) 112.9(5) C(43)-C(42)-C(41) 122.9(6) C(42)-C(43)-C(44) 120.2(6) C(45)-C(44)-C(43) 122.6(7) C(45)-C(44)-C(49) 119.2(7) C(43)-C(44)-C(49) 118.2(6) C(46)-C(45)-C(44) 121.8(7) C(45)-C(46)-C(47) 119.5(7) C(48)-C(47)-C(46) 120.8(7) C(47)-C(48)-C(49) 121.5(7) C(48)-C(49)-C(40) 124.6(6) C(48)-C(49)-C(44) 117.2(6) C(40)-C(49)-C(44) 118.2(6) Cl(3)-C(50)-Cl(2) 112.3(6) ______________________________________________________________ Symmetry transformations used to generate equivalent atoms: Table 5.Anisotropic displacement parameters (A^2 x 10^3) for 94src190. 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 _______________________________________________________________________ Pd(1) 18(1) 18(1) 20(1) 2(1) 1(1) 1(1) P(1) 18(1) 19(1) 20(1) 2(1) 1(1) 2(1) N(1) 19(3) 21(3) 26(3) 5(2) -2(2) -1(2) N(2) 29(4) 23(4) 27(3) 2(3) -5(3) 3(3) Cl(1) 20(1) 30(1) 29(1) 3(1) -4(1) 0(1) Cl(2) 63(1) 65(2) 71(1) -9(2) -34(1) 10(2) Cl(3) 61(2) 126(3) 47(1) 16(1) 7(1) 30(2) C(1) 13(3) 40(5) 27(4) 3(3) 5(3) -1(3) C(2) 23(4) 33(6) 32(4) 12(3) -2(3) -3(3) C(3) 36(5) 49(6) 57(6) 18(5) 3(4) -14(4) C(4) 19(5) 93(9) 67(7) 31(6) 0(4) -13(5) C(5) 18(4) 80(8) 47(5) 24(5) -1(3) 14(4) C(6) 25(4) 52(6) 25(4) 8(3) 6(3) 6(3) C(7) 25(3) 32(6) 20(3) -1(4) 3(2) 13(4) C(8) 39(5) 41(5) 31(4) 6(3) 7(3) 7(3) C(9) 55(4) 53(6) 19(3) 0(4) 6(3) 13(6) C(10) 55(6) 55(7) 30(5) -15(4) -5(4) 27(5) C(11) 52(5) 26(5) 38(5) -8(3) -6(4) 4(4) C(12) 38(4) 42(6) 22(4) -2(3) -1(3) 16(4) C(13) 16(3) 13(4) 26(4) 7(3) 2(3) 4(3) C(14) 20(4) 35(5) 24(4) 1(3) 1(3) -2(3) C(15) 25(4) 29(5) 25(4) 8(3) -5(3) 0(3) C(16) 20(4) 24(5) 44(5) 1(3) -6(3) -3(3) C(17) 32(4) 44(6) 50(6) 9(4) -14(4) 8(4) C(18) 49(6) 39(7) 90(9) -11(6) -18(6) 20(5) C(19) 65(6) 36(6) 79(7) -22(5) -20(5) 31(5) C(20) 52(5) 32(6) 41(5) -8(4) -8(4) 10(4) C(21) 22(4) 17(5) 44(5) 0(3) -3(3) 2(3) C(22) 15(3) 23(5) 28(4) -2(3) 0(3) -3(3) C(23) 25(4) 9(5) 33(4) -6(3) 1(3) 5(3) C(24) 39(4) 8(4) 37(4) -9(3) 8(3) -2(3) C(25) 35(5) 25(5) 43(5) -9(4) 11(4) -6(4) C(26) 48(5) 32(6) 51(6) -11(4) 12(4) -15(4) C(27) 66(6) 30(6) 54(6) -8(4) 32(5) -16(4) C(28) 62(6) 28(5) 32(4) -5(3) 10(4) 1(4) C(29) 48(5) 20(5) 25(4) -3(3) -1(3) 0(3) C(30) 50(5) 11(4) 32(4) -6(3) 0(4) 11(3) C(31) 64(6) 23(5) 38(5) -7(3) -8(4) 16(4) C(32) 63(6) 28(6) 48(5) -15(4) -21(5) 19(4) C(33) 41(5) 31(6) 61(6) -11(4) -26(5) 12(4) C(34) 40(5) 22(5) 41(5) -7(3) -12(4) 3(3) C(35) 33(4) 26(5) 31(4) -10(3) -7(3) 8(3) C(36) 32(5) 38(6) 45(5) 14(4) -10(4) -10(4) C(37) 36(4) 24(5) 28(4) 2(3) 8(3) 1(3) C(38) 22(4) 18(4) 28(4) 1(3) 0(3) 1(3) C(39) 37(5) 18(5) 36(4) -6(3) 4(4) 0(3) C(40) 23(4) 21(5) 17(3) -4(3) -3(3) 0(3) C(41) 22(3) 14(5) 12(3) -3(3) 5(2) 3(3) C(42) 32(4) 14(4) 25(4) 8(3) 9(3) 9(3) C(43) 28(4) 29(6) 25(4) 5(3) -6(3) -6(3) C(44) 20(4) 39(6) 23(4) 6(3) -4(3) -6(3) C(45) 26(4) 39(6) 43(5) 11(4) -5(3) -3(3) C(46) 30(4) 39(6) 55(5) 12(4) -17(4) 6(4) C(47) 38(5) 30(5) 42(5) 14(4) 0(4) 7(4) C(48) 27(4) 15(5) 33(4) 6(3) -1(3) 3(3) C(49) 20(4) 24(5) 23(4) 5(3) 6(3) 1(3) C(50) 59(6) 80(8) 70(7) 36(5) -1(5) -3(5) _______________________________________________________________________ Table 6. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for 94src190. ________________________________________________________________ x y z U(iso) ________________________________________________________________ H(1) -682(6) -906(4) 9673(6) 32 H(2) -1021(7) -2116(4) 10049(6) 35 H(3) -3124(8) -2557(5) 10096(8) 57 H(4) -4907(9) -1793(6) 9741(9) 72 H(5) -4558(7) -611(5) 9310(7) 59 H(6) -2460(6) -151(4) 9298(6) 40 H(7) 117(6) -402(5) 10402(5) 31 H(8) -1022(7) -816(4) 12030(7) 44 H(9) -1280(8) -70(6) 13652(6) 51 H(10) -374(8) 1052(5) 13678(7) 56 H(11) 784(8) 1449(4) 12074(7) 47 H(12) 1017(7) 704(4) 10455(6) 41 H(13) 650(6) -1073(3) 9923(6) 22 H(14) 1578(6) -1154(4) 11864(6) 32 H(15) 3021(6) -2034(4) 12429(6) 32 H(17) 4117(7) -3185(4) 11935(8) 51 H(18) 4569(10) -4049(6) 10580(10) 72 H(19) 3636(9) -3997(5) 8644(9) 74 H(20) 2330(8) -3070(4) 8019(7) 51 H(25) 3447(8) -1448(4) 8202(8) 41 H(26) 4839(8) -1119(4) 6785(7) 52 H(27) 4054(9) -1051(4) 4764(8) 59 H(28) 1924(8) -1326(4) 4228(7) 49 H(31) -133(9) -1593(4) 3810(7) 50 H(32) -2242(9) -1960(4) 3449(8) 57 H(33) -3458(8) -2372(4) 5025(8) 55 H(34) -2458(7) -2496(4) 6910(7) 42 H(36A) 2595(22) 1397(22) 8244(18) 58 H(36B) 2814(29) 1627(16) 6917(26) 58 H(36C) 3468(10) 927(9) 7444(43) 58 H(37A) 1031(11) 272(19) 5495(17) 44 H(37B) 2479(28) 130(15) 5980(7) 44 H(37C) 2110(38) 853(5) 5332(14) 44 H(38) 414(6) 1563(3) 6131(6) 27 H(39A) 941(21) 2077(17) 8042(26) 45 H(39B) 84(45) 1501(4) 8648(10) 45 H(39C) -582(27) 2071(17) 7780(19) 45 H(42) -1610(7) -833(4) 7258(6) 28 H(43) -3348(7) -605(4) 5947(6) 33 H(45) -4721(7) 293(4) 4775(7) 44 H(46) -4998(7) 1420(5) 3988(7) 51 H(47) -3386(7) 2281(4) 4361(7) 44 H(48) -1525(7) 2021(4) 5519(6) 30 H(50A) 4215(10) -662(5) 1317(9) 84 H(50B) 5124(10) 3(5) 1568(9) 84 ________________________________________________________________