Table 1. Crystal data and structure refinement for 94SRC094. Identification code 94SRC094 Empirical formula C45.50 H46 Cl2 Fe2 O3 P2 Pd Formula weight 991.76 Temperature 120(2) K Wavelength 0.71069 A Crystal system Triclinic Space group P1 Unit cell dimensions a = 9.697(3) A b = 10.0628(13) A c = 13.213(2) A alpha = 105.157(14) deg. beta = 97.17(2) deg. gamma = 112.543(9) deg. Volume 1112.1(4) A^3 Z 1 Density (calculated) 1.481 Mg/m^3 Absorption coefficient 1.274 mm^-1 F(000) 505 Crystal size 0.1 x 0.1 x 0.25 mm Theta range for data collection 2.36 to 24.97 deg. Index ranges -10<=h<=10, -11<=k<=11, -14<=l<=12 Reflections collected 3700 Independent reflections 2621 [R(int) = 0.0379] Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 2619 / 34 / 298 Goodness-of-fit on F^2 1.124 Final R indices [I>2sigma(I)] R1 = 0.0511, wR2 = 0.1541 R indices (all data) R1 = 0.0528, wR2 = 0.1587 Largest diff. peak and hole 1.520 and -0.523 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for 94src094. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________ x y z U(eq) ________________________________________________________________ Pd(1) 0 0 0 20(1) Fe(1) 1705(1) -1525(1) 2584(1) 23(1) Cl(1) -1250(2) -2475(1) -1207(1) 27(1) P(1) -1169(1) -903(1) 1274(1) 21(1) O(1) 2310(6) 990(6) 5511(3) 54(1) C(1) 2327(7) 1160(8) 4643(5) 40(2) C(2) 2987(6) 504(7) 3841(4) 31(2) C(3) 3535(6) -634(6) 3892(4) 33(1) C(4) 4011(6) -1046(7) 2929(5) 37(2) C(5) 3736(6) -226(7) 2281(4) 34(1) C(6) 3086(6) 720(6) 2817(4) 31(1) C(7) 226(6) -2995(6) 1114(4) 26(1) C(8) 597(6) -3849(6) 1714(5) 31(1) C(9) 128(6) -3489(6) 2715(4) 34(1) C(10) -526(6) -2468(6) 2711(4) 30(1) C(11) -478(6) -2137(5) 1710(4) 23(1) C(12) -3260(6) -2002(6) 743(4) 27(1) C(13) -4134(6) -3093(6) 1153(5) 33(1) C(14) -5721(7) -3873(7) 734(6) 46(2) C(15) -6435(7) -3540(8) -62(6) 49(2) C(16) -5597(8) -2460(9) -459(5) 53(2) C(17) -3998(7) -1691(8) -67(5) 42(2) C(18) -967(6) 535(6) 2530(4) 29(1) C(19) -1861(7) 1465(7) 2399(6) 44(2) C(20) -1378(20) 2974(22) 3205(14) 28(4) C(21) -1716(29) 2710(22) 4272(14) 54(6) C(20') -1444(23) 2665(21) 3683(22) 72(7) C(21') -2445(22) 3540(20) 3756(23) 128(13) O(30) -6252(20) 4876(24) 6699(16) 167(8) C(33) -5000 5000 5000 12(3) C(31) -4781(17) 4923(21) 6636(16) 88(6) C(30) -5898(24) 5334(25) 5811(15) 122(7) C(32) -3705(14) 4354(17) 6128(12) 61(4) ________________________________________________________________ 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 94src094. _____________________________________________________________ Pd(1)-Cl(1)#1 2.3109(13) Pd(1)-Cl(1) 2.3109(13) Pd(1)-P(1) 2.3310(13) Pd(1)-P(1)#1 2.3310(13) Fe(1)-C(3) 2.036(5) Fe(1)-C(7) 2.047(5) Fe(1)-C(10) 2.052(5) Fe(1)-C(9) 2.050(5) Fe(1)-C(6) 2.050(5) Fe(1)-C(2) 2.058(5) Fe(1)-C(11) 2.052(5) Fe(1)-C(4) 2.060(6) Fe(1)-C(5) 2.061(5) Fe(1)-C(8) 2.075(5) P(1)-C(11) 1.800(6) P(1)-C(18) 1.825(5) P(1)-C(12) 1.829(5) O(1)-C(1) 1.205(8) C(1)-C(2) 1.447(8) C(1)-H(1) 0.89(7) C(2)-C(6) 1.434(8) C(2)-C(3) 1.449(9) C(3)-C(4) 1.421(8) C(3)-H(3) 0.93 C(4)-C(5) 1.402(9) C(4)-H(4) 0.93 C(5)-C(6) 1.423(9) C(5)-H(5) 0.93 C(6)-H(6) 0.93 C(7)-C(8) 1.420(9) C(7)-C(11) 1.437(8) C(7)-H(7) 0.93 C(8)-C(9) 1.454(8) C(8)-H(8) 0.93 C(9)-C(10) 1.400(8) C(9)-H(9) 0.93 C(10)-C(11) 1.447(7) C(10)-H(10) 0.93 C(12)-C(17) 1.382(9) C(12)-C(13) 1.390(8) C(13)-C(14) 1.388(9) C(13)-H(13) 0.93 C(14)-C(15) 1.371(11) C(14)-H(14) 0.93 C(15)-C(16) 1.358(11) C(15)-H(15) 0.93 C(16)-C(17) 1.393(9) C(16)-H(16) 0.93 C(17)-H(17) 0.93 C(18)-C(19) 1.526(8) C(18)-H(18A) 0.97 C(18)-H(18B) 0.97 C(19)-C(20) 1.46(2) C(19)-C(20') 1.70(2) C(19)-H(19A) 0.97 C(19)-H(19B) 0.97 C(20)-C(21) 1.55(2) C(20)-H(20A) 0.97 C(20)-H(20B) 0.97 C(21)-H(21A) 0.9600(10) C(21)-H(21B) 0.96 C(21)-H(21C) 0.96 C(21)-H(21D) 1.53(2) C(20')-C(21') 1.54(3) C(20')-H(20C) 0.97 C(20')-H(20D) 0.97 C(21')-H(21D) 1.04(3) C(21')-H(21E) 0.92(2) C(21')-H(21F) 0.88(3) O(30)-C(30) 1.403(10) O(30)-C(31) 1.423(10) C(33)-C(30)#2 1.512(5) C(33)-C(30) 1.512(5) C(31)-C(32) 1.516(5) Cl(1)#1-Pd(1)-Cl(1) 180.0 Cl(1)#1-Pd(1)-P(1) 92.08(4) Cl(1)-Pd(1)-P(1) 87.92(4) Cl(1)#1-Pd(1)-P(1)#1 87.92(4) Cl(1)-Pd(1)-P(1)#1 92.08(4) P(1)-Pd(1)-P(1)#1 180.0 C(3)-Fe(1)-C(7) 158.0(2) C(3)-Fe(1)-C(10) 121.7(2) C(7)-Fe(1)-C(10) 68.8(2) C(3)-Fe(1)-C(9) 106.3(2) C(7)-Fe(1)-C(9) 68.3(2) C(10)-Fe(1)-C(9) 39.9(2) C(3)-Fe(1)-C(6) 69.1(2) C(7)-Fe(1)-C(6) 121.8(2) C(10)-Fe(1)-C(6) 128.1(2) C(9)-Fe(1)-C(6) 163.7(2) C(3)-Fe(1)-C(2) 41.4(2) C(7)-Fe(1)-C(2) 158.6(3) C(10)-Fe(1)-C(2) 110.2(2) C(9)-Fe(1)-C(2) 125.6(2) C(6)-Fe(1)-C(2) 40.9(2) C(3)-Fe(1)-C(11) 158.9(2) C(7)-Fe(1)-C(11) 41.0(2) C(10)-Fe(1)-C(11) 41.3(2) C(9)-Fe(1)-C(11) 68.4(2) C(6)-Fe(1)-C(11) 109.8(2) C(2)-Fe(1)-C(11) 123.9(2) C(3)-Fe(1)-C(4) 40.6(2) C(7)-Fe(1)-C(4) 121.8(2) C(10)-Fe(1)-C(4) 155.2(3) C(9)-Fe(1)-C(4) 119.3(3) C(6)-Fe(1)-C(4) 68.2(3) C(2)-Fe(1)-C(4) 68.5(2) C(11)-Fe(1)-C(4) 160.1(2) C(3)-Fe(1)-C(5) 67.9(2) C(7)-Fe(1)-C(5) 106.9(2) C(10)-Fe(1)-C(5) 164.6(3) C(9)-Fe(1)-C(5) 153.8(3) C(6)-Fe(1)-C(5) 40.5(2) C(2)-Fe(1)-C(5) 68.0(2) C(11)-Fe(1)-C(5) 125.9(2) C(4)-Fe(1)-C(5) 39.8(3) C(3)-Fe(1)-C(8) 121.7(2) C(7)-Fe(1)-C(8) 40.3(2) C(10)-Fe(1)-C(8) 68.7(2) C(9)-Fe(1)-C(8) 41.3(2) C(6)-Fe(1)-C(8) 154.6(2) C(2)-Fe(1)-C(8) 160.8(3) C(11)-Fe(1)-C(8) 68.8(2) C(4)-Fe(1)-C(8) 104.1(2) C(5)-Fe(1)-C(8) 118.3(2) C(11)-P(1)-C(18) 104.5(2) C(11)-P(1)-C(12) 106.4(2) C(18)-P(1)-C(12) 103.4(2) C(11)-P(1)-Pd(1) 113.3(2) C(18)-P(1)-Pd(1) 116.6(2) C(12)-P(1)-Pd(1) 111.8(2) O(1)-C(1)-C(2) 125.7(8) O(1)-C(1)-H(1) 112(4) C(2)-C(1)-H(1) 122(4) C(6)-C(2)-C(3) 107.1(5) C(6)-C(2)-C(1) 127.7(7) C(3)-C(2)-C(1) 124.9(6) C(6)-C(2)-Fe(1) 69.3(3) C(3)-C(2)-Fe(1) 68.4(3) C(1)-C(2)-Fe(1) 122.8(4) C(4)-C(3)-C(2) 107.8(5) C(4)-C(3)-Fe(1) 70.6(3) C(2)-C(3)-Fe(1) 70.1(3) C(4)-C(3)-H(3) 126.1(4) C(2)-C(3)-H(3) 126.1(3) Fe(1)-C(3)-H(3) 124.7(2) C(5)-C(4)-C(3) 108.3(5) C(5)-C(4)-Fe(1) 70.1(3) C(3)-C(4)-Fe(1) 68.8(3) C(5)-C(4)-H(4) 125.9(3) C(3)-C(4)-H(4) 125.8(4) Fe(1)-C(4)-H(4) 126.8(2) C(4)-C(5)-C(6) 109.3(5) C(4)-C(5)-Fe(1) 70.1(3) C(6)-C(5)-Fe(1) 69.4(3) C(4)-C(5)-H(5) 125.3(3) C(6)-C(5)-H(5) 125.3(4) Fe(1)-C(5)-H(5) 126.80(14) C(2)-C(6)-C(5) 107.5(6) C(2)-C(6)-Fe(1) 69.9(3) C(5)-C(6)-Fe(1) 70.1(3) C(2)-C(6)-H(6) 126.2(4) C(5)-C(6)-H(6) 126.3(4) Fe(1)-C(6)-H(6) 125.3(2) C(8)-C(7)-C(11) 109.4(5) C(8)-C(7)-Fe(1) 70.9(3) C(11)-C(7)-Fe(1) 69.7(3) C(8)-C(7)-H(7) 125.3(3) C(11)-C(7)-H(7) 125.3(3) Fe(1)-C(7)-H(7) 125.7(2) C(7)-C(8)-C(9) 106.4(5) C(7)-C(8)-Fe(1) 68.8(3) C(9)-C(8)-Fe(1) 68.4(3) C(7)-C(8)-H(8) 126.8(3) C(9)-C(8)-H(8) 126.8(3) Fe(1)-C(8)-H(8) 127.5(2) C(10)-C(9)-C(8) 109.2(5) C(10)-C(9)-Fe(1) 70.1(3) C(8)-C(9)-Fe(1) 70.3(3) C(10)-C(9)-H(9) 125.4(3) C(8)-C(9)-H(9) 125.4(3) Fe(1)-C(9)-H(9) 125.8(2) C(9)-C(10)-C(11) 108.2(5) C(9)-C(10)-Fe(1) 70.0(3) C(11)-C(10)-Fe(1) 69.4(3) C(9)-C(10)-H(10) 125.9(3) C(11)-C(10)-H(10) 125.9(3) Fe(1)-C(10)-H(10) 126.3(2) C(7)-C(11)-C(10) 106.8(5) C(7)-C(11)-P(1) 125.8(4) C(10)-C(11)-P(1) 127.3(4) C(7)-C(11)-Fe(1) 69.3(3) C(10)-C(11)-Fe(1) 69.3(3) P(1)-C(11)-Fe(1) 126.6(2) C(17)-C(12)-C(13) 119.0(5) C(17)-C(12)-P(1) 118.6(4) C(13)-C(12)-P(1) 122.3(5) C(12)-C(13)-C(14) 119.9(6) C(12)-C(13)-H(13) 120.0(3) C(14)-C(13)-H(13) 120.1(4) C(15)-C(14)-C(13) 120.2(6) C(15)-C(14)-H(14) 119.9(4) C(13)-C(14)-H(14) 119.9(4) C(16)-C(15)-C(14) 120.5(6) C(16)-C(15)-H(15) 119.8(4) C(14)-C(15)-H(15) 119.8(4) C(15)-C(16)-C(17) 120.1(7) C(15)-C(16)-H(16) 119.9(4) C(17)-C(16)-H(16) 119.9(4) C(12)-C(17)-C(16) 120.2(6) C(12)-C(17)-H(17) 119.9(3) C(16)-C(17)-H(17) 119.9(4) C(19)-C(18)-P(1) 114.4(4) C(19)-C(18)-H(18A) 108.6(3) P(1)-C(18)-H(18A) 108.6(2) C(19)-C(18)-H(18B) 108.7(3) P(1)-C(18)-H(18B) 108.7(2) H(18A)-C(18)-H(18B) 107.6 C(20)-C(19)-C(18) 119.5(9) C(18)-C(19)-C(20') 102.8(9) C(20)-C(19)-H(19A) 107.3(8) C(18)-C(19)-H(19A) 107.4(3) C(20)-C(19)-H(19B) 107.5(8) C(18)-C(19)-H(19B) 107.5(3) H(19A)-C(19)-H(19B) 107.0 C(19)-C(20)-C(21) 106.9(14) C(19)-C(20)-H(20A) 110.3(8) C(21)-C(20)-H(20A) 110.2(11) C(19)-C(20)-H(20B) 110.4(8) C(21)-C(20)-H(20B) 110.5(12) H(20A)-C(20)-H(20B) 108.6 C(20)-C(21)-H(21A) 109.4(10) C(20)-C(21)-H(21B) 109.4(11) H(21A)-C(21)-H(21B) 109.47(10) C(20)-C(21)-H(21C) 109.6(12) H(21A)-C(21)-H(21C) 109.47(6) H(21B)-C(21)-H(21C) 109.47(6) C(21')-C(20')-C(19) 111(2) C(21')-C(20')-H(20C) 110(2) C(19)-C(20')-H(20C) 109.5(9) C(21')-C(20')-H(20D) 109.5(9) C(19)-C(20')-H(20D) 109.5(7) H(20C)-C(20')-H(20D) 108.1 C(20')-C(21')-H(21D) 101(3) C(20')-C(21')-H(21E) 107(2) H(21D)-C(21')-H(21E) 106(2) C(20')-C(21')-H(21F) 111(2) H(21D)-C(21')-H(21F) 109(2) H(21E)-C(21')-H(21F) 121(4) C(30)-O(30)-C(31) 73(2) C(30)#2-C(33)-C(30) 180.000(8) O(30)-C(31)-C(32) 154(2) O(30)-C(30)-C(33) 135(2) _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: #1 -x,-y,-z #2 -x-1,-y+1,-z+1 Table 5. Anisotropic displacement parameters (A^2 x 10^3) for 94src094. 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) 16(1) 18(1) 22(1) 6(1) 3(1) 5(1) Fe(1) 19(1) 22(1) 24(1) 5(1) 1(1) 7(1) Cl(1) 27(1) 20(1) 26(1) 5(1) 4(1) 4(1) P(1) 17(1) 20(1) 25(1) 7(1) 5(1) 7(1) O(1) 63(3) 60(3) 34(2) 10(2) 17(2) 23(2) C(1) 37(4) 40(3) 30(3) -5(3) 0(2) 17(3) C(2) 19(3) 34(3) 22(3) -2(2) -3(2) 1(2) C(3) 28(3) 35(3) 31(3) 9(2) -2(2) 12(2) C(4) 25(3) 34(3) 42(3) 1(3) -3(2) 13(2) C(5) 22(3) 39(3) 29(3) 5(3) 1(2) 8(2) C(6) 26(3) 23(3) 30(3) 5(2) 1(2) 2(2) C(7) 21(3) 22(3) 29(3) 2(2) 0(2) 9(2) C(8) 22(3) 16(2) 51(3) 10(3) 1(2) 8(2) C(9) 33(3) 26(3) 39(3) 15(3) 1(2) 10(2) C(10) 19(3) 28(3) 38(3) 14(3) 8(2) 4(2) C(11) 18(3) 21(2) 24(2) 5(2) 1(2) 7(2) C(12) 18(3) 27(3) 32(3) 3(2) 6(2) 11(2) C(13) 22(3) 29(3) 47(3) 12(3) 14(2) 9(2) C(14) 24(3) 31(3) 72(4) 8(3) 20(3) 6(3) C(15) 18(3) 48(4) 56(4) -11(3) 7(3) 8(3) C(16) 31(4) 70(5) 55(4) 15(4) -2(3) 25(3) C(17) 26(3) 51(4) 47(3) 22(3) 4(2) 13(3) C(18) 31(3) 23(3) 31(3) 8(2) 14(2) 8(2) C(19) 25(3) 31(3) 75(4) 8(3) 16(3) 15(3) C(20) 29(8) 12(8) 38(10) 15(7) 1(6) 2(6) C(21) 107(16) 54(11) 33(10) 21(9) 33(9) 60(11) C(20') 81(13) 35(10) 109(24) 16(13) 42(14) 35(8) C(21') 71(13) 57(10) 210(27) -19(13) 50(14) 18(9) O(30) 190(12) 145(11) 170(11) 23(8) 41(9) 99(9) C(33) 13(6) 11(5) 13(5) 1(4) 3(4) 8(4) C(31) 68(9) 65(8) 106(10) 18(7) -20(7) 25(7) C(30) 124(11) 93(10) 134(11) 38(8) 3(8) 42(8) C(32) 27(6) 58(8) 59(8) -21(7) 12(5) 7(6) _______________________________________________________________________ Table 6. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for 94src094. ________________________________________________________________ x y z U(iso) ________________________________________________________________ H(1) 1782(76) 1662(77) 4502(50) 45(20) H(3) 3570(6) -1026(6) 4454(4) 40 H(4) 4432(6) -1740(7) 2758(5) 45 H(5) 3947(6) -291(7) 1606(4) 41 H(6) 2780(6) 1360(6) 2551(4) 37 H(7) 411(6) -2992(6) 441(4) 31 H(8) 1050(6) -4507(6) 1507(5) 37 H(9) 245(6) -3876(6) 3270(4) 41 H(10) -924(6) -2071(6) 3257(4) 36 H(13) -3656(6) -3301(6) 1708(5) 39 H(14) -6303(7) -4625(7) 994(6) 55 H(15) -7502(7) -4056(8) -331(6) 59 H(16) -6091(8) -2234(9) -994(5) 64 H(17) -3426(7) -966(8) -350(5) 50 H(18A) -1315(6) 29(6) 3044(4) 35 H(18B) 118(6) 1230(6) 2835(4) 35 H(19A) -1845(7) 1599(7) 1699(6) 53 H(19B) -2928(7) 850(7) 2369(6) 53 H(20A) -1949(20) 3490(22) 2965(14) 34 H(20B) -286(20) 3598(22) 3315(14) 34 H(21A) -1475(151) 3671(29) 4811(35) 80 H(21B) -1094(115) 2259(143) 4526(60) 80 H(21C) -2787(42) 2038(123) 4141(27) 80 H(20C) -1625(23) 2082(21) 4172(22) 86 H(20D) -362(23) 3387(21) 3905(22) 86 H(21D) -2364 3888 4585 192 H(21E) -3451 2832 3431 192 H(21F) -2028 4354 3567 192 ________________________________________________________________