Table 1. Crystal data and structure refinement for 98SRC114. Identification code 98SRC114 Empirical formula C35.60 H32 Cl2 Fe O1.40 P2 Pd Formula weight 777.30 Temperature 293(2) K Wavelength 1.54178 A Crystal system Triclinic Space group P-1 Unit cell dimensions a = 11.082(2) A alpha = 88.85(3) deg. b = 13.340(3) A beta = 76.48(3) deg. c = 13.783(3) A gamma = 72.31(3) deg. Volume 1884.6(7) A^3 Z 2 Density (calculated) 1.370 Mg/m^3 Absorption coefficient 9.242 mm^-1 F(000) 786 Crystal size 0.24 x 0.2 x 0.3 mm Theta range for data collection 3.30 to 66.93 deg. Index ranges 0<=h<=13, -15<=k<=15, -15<=l<=16 Reflections collected 6865 Independent reflections 6503 [R(int) = 0.0218] Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 6495 / 0 / 417 Goodness-of-fit on F^2 1.052 Final R indices [I>2sigma(I)] R1 = 0.0514, wR2 = 0.1443 R indices (all data) R1 = 0.0635, wR2 = 0.1599 Largest diff. peak and hole 0.887 and -1.333 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for 98SRC114. ________________________________________________________________ x y z U(eq) ________________________________________________________________ Pd(1) 9582(1) 9918(1) 6300(1) 45(1) Fe(1) 11257(1) 6897(1) 6891(1) 49(1) Cl(1) 9997(1) 10737(1) 7557(1) 64(1) Cl(2) 9106(2) 9278(1) 4926(1) 68(1) P(1) 8489(1) 9017(1) 7337(1) 45(1) P(2) 13853(1) 4834(1) 7405(1) 58(1) C(1) 9794(4) 7046(4) 6188(4) 58(1) C(2) 10345(5) 5972(4) 6370(5) 69(2) C(3) 10220(5) 5864(4) 7397(5) 70(2) C(4) 9565(5) 6885(4) 7906(4) 62(1) C(5) 9293(4) 7634(3) 7144(3) 49(1) C(6) 12578(4) 7136(4) 7609(4) 58(1) C(7) 12215(5) 7973(4) 7012(5) 63(1) C(8) 12518(5) 7582(4) 6014(5) 67(2) C(9) 13102(5) 6475(4) 5977(4) 62(1) C(10) 13150(4) 6166(4) 6994(4) 54(1) C(11) 8188(5) 9295(4) 8663(3) 58(1) C(12) 6937(7) 9786(8) 9224(5) 111(3) C(13) 6727(9) 10006(11) 10257(6) 157(5) C(14) 7727(9) 9715(10) 10709(5) 136(4) C(15) 8949(7) 9225(6) 10166(4) 85(2) C(16) 9184(5) 9042(5) 9150(4) 66(1) C(17) 6907(4) 9248(4) 7061(3) 48(1) C(18) 6319(5) 8472(5) 7131(5) 70(2) C(19) 5102(6) 8691(6) 6902(6) 94(2) C(20) 4494(6) 9651(6) 6651(6) 90(2) C(21) 5071(6) 10422(7) 6579(7) 109(3) C(22) 6272(6) 10227(5) 6786(6) 85(2) C(23) 13258(5) 3834(4) 6920(4) 62(1) C(24) 13477(8) 3620(5) 5906(6) 89(2) C(25) 12903(11) 2935(7) 5575(9) 133(4) C(26) 12137(9) 2456(6) 6314(11) 126(4) C(27) 11983(9) 2632(6) 7241(10) 119(3) C(28) 12512(6) 3323(5) 7579(6) 90(2) C(29) 15663(5) 4480(4) 6954(4) 58(1) C(30) 16456(6) 3445(5) 6843(5) 78(2) C(31) 17835(7) 3205(6) 6564(6) 93(2) C(32) 18382(6) 3987(7) 6427(6) 95(2) C(33) 17622(6) 5008(6) 6516(6) 103(2) C(34) 16280(5) 5263(5) 6772(5) 79(2) O(1) 13428(4) 4836(3) 8615(3) 80(1) O(2) 13029(12) 6407(7) 9983(6) 70(3) C(35) 10996(23) 6098(18) 10503(16) 133(10) C(36) 11854(24) 6485(16) 10743(11) 108(8) C(37) 16146(35) 3285(19) 9784(15) 145(13) C(38) 15101(30) 3252(19) 10469(24) 148(12) ________________________________________________________________ Table 3. Bond lengths [A] and angles [deg] for 98SRC114. _____________________________________________________________ Pd(1)-P(1) 2.2267(13)Pd(1)-Cl(1) 2.2716(13) Pd(1)-Cl(2) 2.3239(13)Pd(1)-Cl(2)#1 2.4187(14) Fe(1)-C(1) 2.034(5) Fe(1)-C(5) 2.046(4) Fe(1)-C(2) 2.048(5) Fe(1)-C(8) 2.048(5) Fe(1)-C(6) 2.049(5) Fe(1)-C(9) 2.052(5) Fe(1)-C(7) 2.058(5) Fe(1)-C(3) 2.062(5) Fe(1)-C(4) 2.065(5) Fe(1)-C(10) 2.065(4) Cl(2)-Pd(1)#1 2.4187(14)P(1)-C(5) 1.782(5) P(1)-C(11) 1.804(5) P(1)-C(17) 1.814(4) P(2)-O(1) 1.623(4) P(2)-C(10) 1.847(5) P(2)-C(23) 1.854(5) P(2)-C(29) 1.867(5) C(1)-C(2) 1.420(7) C(1)-C(5) 1.447(7) C(2)-C(3) 1.398(9) C(3)-C(4) 1.440(8) C(4)-C(5) 1.455(7) C(6)-C(7) 1.389(7) C(6)-C(10) 1.445(7) C(7)-C(8) 1.409(8) C(8)-C(9) 1.417(7) C(9)-C(10) 1.462(7) C(11)-C(16) 1.376(7) C(11)-C(12) 1.384(8) C(12)-C(13) 1.409(10) C(13)-C(14) 1.348(13) C(14)-C(15) 1.352(11) C(15)-C(16) 1.376(7) C(17)-C(18) 1.372(7) C(17)-C(22) 1.375(7) C(18)-C(19) 1.399(8) C(19)-C(20) 1.335(10) C(20)-C(21) 1.357(11) C(21)-C(22) 1.373(9) C(23)-C(24) 1.381(9) C(23)-C(28) 1.393(9) C(24)-C(25) 1.397(11) C(25)-C(26) 1.437(14) C(26)-C(27) 1.27(2) C(27)-C(28) 1.372(10) C(29)-C(30) 1.382(7) C(29)-C(34) 1.401(8) C(30)-C(31) 1.421(9) C(31)-C(32) 1.347(10) C(32)-C(33) 1.356(10) C(33)-C(34) 1.379(8) O(2)-C(37)#2 1.22(4) O(2)-C(36) 1.44(2) C(35)-C(36) 1.32(3) C(37)-O(2)#2 1.22(4) C(37)-C(38) 1.32(4) P(1)-Pd(1)-Cl(1) 93.57(5) P(1)-Pd(1)-Cl(2) 91.69(5) Cl(1)-Pd(1)-Cl(2) 172.99(5) P(1)-Pd(1)-Cl(2)#1 173.94(5) Cl(1)-Pd(1)-Cl(2)#1 90.45(5) Cl(2)-Pd(1)-Cl(2)#1 84.69(5) C(1)-Fe(1)-C(5) 41.5(2) C(1)-Fe(1)-C(2) 40.7(2) C(5)-Fe(1)-C(2) 68.9(2) C(1)-Fe(1)-C(8) 106.2(2) C(5)-Fe(1)-C(8) 119.1(2) C(2)-Fe(1)-C(8) 125.1(3) C(1)-Fe(1)-C(6) 166.1(2) C(5)-Fe(1)-C(6) 129.5(2) C(2)-Fe(1)-C(6) 153.0(2) C(8)-Fe(1)-C(6) 67.5(2) C(1)-Fe(1)-C(9) 115.4(2) C(5)-Fe(1)-C(9) 151.3(2) C(2)-Fe(1)-C(9) 104.7(2) C(8)-Fe(1)-C(9) 40.5(2) C(6)-Fe(1)-C(9) 68.5(2) C(1)-Fe(1)-C(7) 127.9(2) C(5)-Fe(1)-C(7) 110.3(2) C(2)-Fe(1)-C(7) 163.8(3) C(8)-Fe(1)-C(7) 40.1(2) C(6)-Fe(1)-C(7) 39.5(2) C(9)-Fe(1)-C(7) 67.8(2) C(1)-Fe(1)-C(3) 68.4(2) C(5)-Fe(1)-C(3) 69.0(2) C(2)-Fe(1)-C(3) 39.8(2) C(8)-Fe(1)-C(3) 161.9(3) C(6)-Fe(1)-C(3) 121.5(2) C(9)-Fe(1)-C(3) 124.8(2) C(7)-Fe(1)-C(3) 156.2(3) C(1)-Fe(1)-C(4) 69.4(2) C(5)-Fe(1)-C(4) 41.5(2) C(2)-Fe(1)-C(4) 68.2(2) C(8)-Fe(1)-C(4) 155.3(2) C(6)-Fe(1)-C(4) 110.8(2) C(9)-Fe(1)-C(4) 163.9(2) C(7)-Fe(1)-C(4) 122.6(2) C(3)-Fe(1)-C(4) 40.8(2) C(1)-Fe(1)-C(10) 150.0(2) C(5)-Fe(1)-C(10) 166.6(2) C(2)-Fe(1)-C(10) 116.4(2) C(8)-Fe(1)-C(10) 69.0(2) C(6)-Fe(1)-C(10) 41.1(2) C(9)-Fe(1)-C(10) 41.6(2) C(7)-Fe(1)-C(10) 68.3(2) C(3)-Fe(1)-C(10) 106.6(2) C(4)-Fe(1)-C(10) 127.2(2) Pd(1)-Cl(2)-Pd(1)#1 95.31(5) C(5)-P(1)-C(11) 105.3(2) C(5)-P(1)-C(17) 106.5(2) C(11)-P(1)-C(17) 106.6(2) C(5)-P(1)-Pd(1) 111.3(2) C(11)-P(1)-Pd(1) 118.1(2) C(17)-P(1)-Pd(1) 108.4(2) O(1)-P(2)-C(10) 109.7(2) O(1)-P(2)-C(23) 106.3(3) C(10)-P(2)-C(23) 112.6(2) O(1)-P(2)-C(29) 110.9(2) C(10)-P(2)-C(29) 107.2(2) C(23)-P(2)-C(29) 110.2(2) C(2)-C(1)-C(5) 107.7(5) C(2)-C(1)-Fe(1) 70.2(3) C(5)-C(1)-Fe(1) 69.7(3) C(3)-C(2)-C(1) 109.5(5) C(3)-C(2)-Fe(1) 70.7(3) C(1)-C(2)-Fe(1) 69.1(3) C(2)-C(3)-C(4) 108.7(5) C(2)-C(3)-Fe(1) 69.5(3) C(4)-C(3)-Fe(1) 69.7(3) C(3)-C(4)-C(5) 107.0(5) C(3)-C(4)-Fe(1) 69.5(3) C(5)-C(4)-Fe(1) 68.6(3) C(1)-C(5)-C(4) 107.1(4) C(1)-C(5)-P(1) 125.9(4) C(4)-C(5)-P(1) 127.0(4) C(1)-C(5)-Fe(1) 68.8(3) C(4)-C(5)-Fe(1) 70.0(3) P(1)-C(5)-Fe(1) 126.5(2) C(7)-C(6)-C(10) 109.5(5) C(7)-C(6)-Fe(1) 70.6(3) C(10)-C(6)-Fe(1) 70.0(3) C(6)-C(7)-C(8) 109.0(5) C(6)-C(7)-Fe(1) 69.9(3) C(8)-C(7)-Fe(1) 69.5(3) C(7)-C(8)-C(9) 108.4(5) C(7)-C(8)-Fe(1) 70.3(3) C(9)-C(8)-Fe(1) 69.9(3) C(8)-C(9)-C(10) 108.0(5) C(8)-C(9)-Fe(1) 69.6(3) C(10)-C(9)-Fe(1) 69.7(3) C(6)-C(10)-C(9) 105.1(4) C(6)-C(10)-P(2) 127.1(4) C(9)-C(10)-P(2) 127.7(4) C(6)-C(10)-Fe(1) 68.9(2) C(9)-C(10)-Fe(1) 68.7(3) P(2)-C(10)-Fe(1) 128.5(3) C(16)-C(11)-C(12) 117.6(5) C(16)-C(11)-P(1) 121.7(4) C(12)-C(11)-P(1) 120.7(5) C(11)-C(12)-C(13) 119.7(7) C(14)-C(13)-C(12) 120.6(8) C(13)-C(14)-C(15) 120.0(7) C(14)-C(15)-C(16) 120.4(7) C(11)-C(16)-C(15) 121.6(5) C(18)-C(17)-C(22) 119.0(5) C(18)-C(17)-P(1) 121.6(4) C(22)-C(17)-P(1) 119.4(4) C(17)-C(18)-C(19) 119.2(6) C(20)-C(19)-C(18) 120.8(6) C(19)-C(20)-C(21) 120.3(6) C(20)-C(21)-C(22) 120.2(6) C(17)-C(22)-C(21) 120.4(6) C(24)-C(23)-C(28) 118.5(6) C(24)-C(23)-P(2) 121.4(5) C(28)-C(23)-P(2) 120.0(5) C(23)-C(24)-C(25) 119.2(9) C(24)-C(25)-C(26) 118.1(9) C(27)-C(26)-C(25) 121.9(8) C(26)-C(27)-C(28) 120.8(10) C(27)-C(28)-C(23) 121.5(9) C(30)-C(29)-C(34) 117.1(5) C(30)-C(29)-P(2) 121.8(4) C(34)-C(29)-P(2) 121.0(4) C(29)-C(30)-C(31) 120.4(6) C(32)-C(31)-C(30) 120.2(6) C(31)-C(32)-C(33) 120.3(6) C(32)-C(33)-C(34) 120.7(7) C(33)-C(34)-C(29) 121.2(6) C(37)#2-O(2)-C(36) 117(2) C(35)-C(36)-O(2) 117.2(13) O(2)#2-C(37)-C(38) 120(2) _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: #1 -x+2,-y+2,-z+1 #2 -x+3,-y+1,-z+2 Table 4. Anisotropic displacement parameters (A^2 x 10^3) for 98SRC114. _______________________________________________________________________ U11 U22 U33 U23 U13 U12 _______________________________________________________________________ Pd(1) 50(1) 48(1) 42(1) 3(1) -14(1) -21(1) Fe(1) 37(1) 49(1) 62(1) 6(1) -14(1) -14(1) Cl(1) 92(1) 63(1) 51(1) 1(1) -27(1) -37(1) Cl(2) 95(1) 89(1) 45(1) 9(1) -21(1) -62(1) P(1) 40(1) 51(1) 44(1) 4(1) -10(1) -15(1) P(2) 53(1) 57(1) 62(1) 1(1) -14(1) -14(1) C(1) 49(2) 62(3) 65(3) -3(2) -18(2) -16(2) C(2) 51(3) 56(3) 103(4) -6(3) -22(3) -18(2) C(3) 49(3) 53(3) 108(5) 22(3) -18(3) -17(2) C(4) 50(3) 65(3) 75(3) 18(3) -12(2) -23(2) C(5) 40(2) 50(2) 58(2) 11(2) -13(2) -15(2) C(6) 46(2) 60(3) 71(3) -3(2) -20(2) -16(2) C(7) 46(2) 53(3) 94(4) 5(3) -19(3) -18(2) C(8) 44(2) 71(3) 92(4) 29(3) -17(3) -27(2) C(9) 47(2) 67(3) 69(3) 5(2) -9(2) -17(2) C(10) 37(2) 56(3) 66(3) 1(2) -14(2) -11(2) C(11) 54(3) 73(3) 45(2) 5(2) -8(2) -22(2) C(12) 63(4) 188(9) 69(4) -37(5) 1(3) -27(5) C(13) 85(5) 297(15) 75(5) -62(7) 17(4) -61(7) C(14) 116(7) 247(12) 51(4) -24(5) 2(4) -79(8) C(15) 94(5) 118(5) 58(3) 9(3) -24(3) -49(4) C(16) 65(3) 89(4) 47(3) 12(2) -12(2) -29(3) C(17) 35(2) 56(2) 51(2) 1(2) -7(2) -12(2) C(18) 46(3) 70(3) 97(4) 11(3) -21(3) -21(2) C(19) 50(3) 103(5) 135(6) -6(4) -25(4) -31(3) C(20) 40(3) 123(6) 102(5) 2(4) -26(3) -10(3) C(21) 53(3) 108(5) 162(8) 50(5) -43(4) -9(4) C(22) 59(3) 64(3) 132(6) 24(4) -32(4) -13(3) C(23) 49(3) 56(3) 79(3) 2(2) -19(2) -13(2) C(24) 105(5) 77(4) 94(5) -8(3) -44(4) -26(4) C(25) 170(9) 81(5) 158(9) -21(6) -106(8) 0(6) C(26) 100(6) 54(4) 253(14) -1(6) -96(8) -24(4) C(27) 91(5) 78(5) 195(11) -16(6) -28(6) -41(4) C(28) 74(4) 65(4) 131(6) 3(4) -10(4) -31(3) C(29) 52(3) 57(3) 62(3) 1(2) -21(2) -9(2) C(30) 66(3) 67(3) 91(4) -1(3) -20(3) -6(3) C(31) 69(4) 83(4) 100(5) -3(4) -20(4) 18(4) C(32) 47(3) 122(6) 98(5) 6(4) -15(3) -4(4) C(33) 57(4) 112(6) 145(7) 12(5) -27(4) -32(4) C(34) 51(3) 74(4) 111(5) -1(3) -18(3) -19(3) O(1) 82(3) 87(3) 61(2) 8(2) -12(2) -18(2) O(2) 122(8) 54(5) 37(4) -15(4) -40(5) -13(5) C(35) 120(18) 122(17) 81(13) 11(12) 74(13) 1(14) C(36) 151(20) 89(12) 36(7) -29(7) 0(10) 18(13) C(37) 237(36) 92(15) 70(12) 18(11) -61(17) 19(19) C(38) 211(30) 119(18) 195(27) 29(19) -162(26) -83(20) _______________________________________________________________________ Table 5. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for 98SRC114. ________________________________________________________________ x y z U(eq) ________________________________________________________________ H(1) 9761(4) 7323(4) 5566(4) 69 H(2) 10729(5) 5424(4) 5881(5) 83 H(3) 10511(5) 5237(4) 7701(5) 84 H(4) 9356(5) 7037(4) 8592(4) 75 H(6) 12470(4) 7191(4) 8297(4) 69 H(7) 11834(5) 8677(4) 7236(5) 76 H(8) 12361(5) 7983(4) 5470(5) 81 H(9) 13402(5) 6025(4) 5406(4) 74 H(12) 6239(7) 9971(8) 8921(5) 133 H(13) 5890(9) 10355(11) 10630(6) 188 H(14) 7576(9) 9850(10) 11393(5) 163 H(15) 9634(7) 9011(6) 10481(4) 102 H(16) 10037(5) 8740(5) 8784(4) 80 H(18) 6724(5) 7809(5) 7328(5) 84 H(19) 4712(6) 8162(6) 6926(6) 112 H(20) 3672(6) 9793(6) 6525(6) 108 H(21) 4651(6) 11085(7) 6389(7) 131 H(22) 6659(6) 10760(5) 6740(6) 103 H(24) 14000(8) 3928(5) 5450(6) 106 H(25) 13014(11) 2793(7) 4896(9) 160 H(26) 11742(9) 2004(6) 6105(11) 152 H(27) 11507(9) 2289(6) 7698(10) 143 H(28) 12369(6) 3452(5) 8263(6) 108 H(30) 16084(6) 2902(5) 6951(5) 93 H(31) 18361(7) 2507(6) 6476(6) 112 H(32) 19285(6) 3827(7) 6272(6) 114 H(33) 18009(6) 5541(6) 6403(6) 123 H(34) 15776(5) 5967(5) 6824(5) 95 H(35A) 10722(143) 6447(107) 9939(92) 200 H(35B) 10254(87) 6210(139) 11059(52) 200 H(35C) 11386(64) 5357(33) 10335(141) 200 H(36A) 12107(24) 6130(16) 11319(11) 130 H(36B) 11425(24) 7223(16) 10949(11) 130 H(37A) 16577(35) 2579(19) 9479(15) 174 H(37B) 15843(35) 3727(19) 9268(15) 174 H(38A) 14624(126) 2891(162) 10187(55) 223 H(38B) 14556(113) 3957(19) 10689(128) 223 H(38C) 15366(32) 2885(159) 11027(78) 223 ________________________________________________________________