Table 1. Crystal data and structure refinement for 1. Identification code s92 Empirical formula C23 H29 Br2 Fe2 P Formula weight 607.95 Temperature 293(2) K Wavelength 0.71069 A Crystal system ? Space group ? Unit cell dimensions a = 7.6828(10) A alpha = 99.180(9) deg. b = 9.4950(14) A beta = 93.392(5) deg. c = 14.6420(13) A gamma = 90.311(9) deg. Volume 1052.5(2) A^3 Z 2 Density (calculated) 1.918 Mg/m^3 Absorption coefficient 5.259 mm^-1 F(000) 608 Crystal size ? x ? x ? mm Theta range for data collection 2.17 to 25.06 deg. Index ranges -8<=h<=9, -8<=k<=10, -15<=l<=16 Reflections collected 4038 Independent reflections 2900 [R(int) = 0.0807] Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 2896 / 0 / 249 Goodness-of-fit on F^2 1.043 Final R indices [I>2sigma(I)] R1 = 0.0687, wR2 = 0.1805 R indices (all data) R1 = 0.0799, wR2 = 0.1962 Largest diff. peak and hole 2.242 and -1.038 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for 1. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________ x y z U(eq) ________________________________________________________________ Fe(1) 6786(2) -2182(1) -2653(1) 17(1) Fe(2) 2706(1) 2983(1) -3047(1) 16(1) Br(1) 1720(1) 3416(1) 592(1) 33(1) Br(2) -1164(1) 2447(1) -4467(1) 39(1) P(1) 6150(3) 1542(2) -1860(1) 15(1) C(1) 7924(11) -4120(9) -2614(6) 22(2) C(2) 8390(12) -3548(10) -3403(7) 31(2) C(3) 9247(11) -2227(10) -3101(7) 31(2) C(4) 9324(11) -1960(9) -2131(6) 24(2) C(5) 8490(11) -3096(9) -1848(6) 21(2) C(6) 4710(10) -1364(9) -1932(6) 18(2) C(7) 4161(11) -2518(9) -2633(6) 22(2) C(8) 4580(11) -2158(9) -3495(6) 21(1) C(9) 5407(11) -794(9) -3319(6) 21(1) C(10) 5468(10) -275(8) -2358(6) 16(2) C(11) 6329(11) 1516(9) -591(6) 18(2) C(12) 6573(12) 3048(9) -79(6) 25(2) C(13) 7842(11) 607(9) -320(6) 23(2) C(14) 4023(10) 2368(8) -1918(5) 16(2) C(15) 3726(11) 3876(9) -1774(6) 20(2) C(16) 1938(12) 4131(9) -1838(6) 23(2) C(17) 1037(11) 2801(10) -2032(6) 23(2) C(18) 2308(10) 1708(10) -2079(5) 19(2) C(19) 2076(11) 4146(9) -4077(5) 18(2) C(20) 3910(11) 3903(10) -4014(6) 25(2) C(21) 4154(11) 2411(9) -4169(6) 20(2) C(22) 2534(12) 1732(10) -4321(6) 24(2) C(23) 1267(11) 2777(10) -4255(6) 22(2) ________________________________________________________________ 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 1. _____________________________________________________________ Fe(1)-C(5) 2.003(8) Fe(1)-C(9) 2.028(8) Fe(1)-C(2) 2.032(9) Fe(1)-C(8) 2.038(8) Fe(1)-C(3) 2.036(9) Fe(1)-C(7) 2.043(8) Fe(1)-C(4) 2.050(9) Fe(1)-C(1) 2.049(8) Fe(1)-C(6) 2.053(8) Fe(1)-C(10) 2.076(8) Fe(2)-C(23) 2.011(8) Fe(2)-C(15) 2.030(8) Fe(2)-C(19) 2.044(8) Fe(2)-C(18) 2.040(8) Fe(2)-C(22) 2.042(8) Fe(2)-C(21) 2.043(8) Fe(2)-C(16) 2.045(8) Fe(2)-C(20) 2.041(8) Fe(2)-C(17) 2.047(8) Fe(2)-C(14) 2.053(8) Br(1)-C(5)#1 1.927(9) Br(2)-C(23) 1.891(8) P(1)-C(14) 1.820(8) P(1)-C(10) 1.824(8) P(1)-C(11) 1.859(8) C(1)-C(5) 1.408(12) C(1)-C(2) 1.415(13) C(2)-C(3) 1.408(13) C(3)-C(4) 1.400(13) C(4)-C(5) 1.383(12) C(5)-Br(1)#1 1.927(9) C(6)-C(7) 1.420(12) C(6)-C(10) 1.428(12) C(7)-C(8) 1.414(13) C(8)-C(9) 1.419(12) C(9)-C(10) 1.414(12) C(11)-C(13) 1.523(12) C(11)-C(12) 1.531(12) C(14)-C(15) 1.435(12) C(14)-C(18) 1.446(11) C(15)-C(16) 1.396(12) C(16)-C(17) 1.417(12) C(17)-C(18) 1.425(12) C(19)-C(23) 1.417(12) C(19)-C(20) 1.429(12) C(20)-C(21) 1.414(12) C(21)-C(22) 1.388(12) C(22)-C(23) 1.390(13) C(5)-Fe(1)-C(9) 165.2(3) C(5)-Fe(1)-C(2) 67.6(4) C(9)-Fe(1)-C(2) 117.9(4) C(5)-Fe(1)-C(8) 153.7(3) C(9)-Fe(1)-C(8) 40.9(3) C(2)-Fe(1)-C(8) 104.6(4) C(5)-Fe(1)-C(3) 67.1(4) C(9)-Fe(1)-C(3) 107.4(4) C(2)-Fe(1)-C(3) 40.5(4) C(8)-Fe(1)-C(3) 124.2(4) C(5)-Fe(1)-C(7) 121.4(4) C(9)-Fe(1)-C(7) 68.3(4) C(2)-Fe(1)-C(7) 123.6(4) C(8)-Fe(1)-C(7) 40.5(4) C(3)-Fe(1)-C(7) 160.9(4) C(5)-Fe(1)-C(4) 39.9(4) C(9)-Fe(1)-C(4) 127.2(3) C(2)-Fe(1)-C(4) 67.9(4) C(8)-Fe(1)-C(4) 162.5(4) C(3)-Fe(1)-C(4) 40.1(4) C(7)-Fe(1)-C(4) 156.8(4) C(5)-Fe(1)-C(1) 40.6(3) C(9)-Fe(1)-C(1) 152.0(3) C(2)-Fe(1)-C(1) 40.6(4) C(8)-Fe(1)-C(1) 117.1(3) C(3)-Fe(1)-C(1) 68.2(4) C(7)-Fe(1)-C(1) 106.3(3) C(4)-Fe(1)-C(1) 68.3(3) C(5)-Fe(1)-C(6) 111.4(3) C(9)-Fe(1)-C(6) 67.8(3) C(2)-Fe(1)-C(6) 162.3(4) C(8)-Fe(1)-C(6) 68.1(3) C(3)-Fe(1)-C(6) 156.8(4) C(7)-Fe(1)-C(6) 40.6(3) C(4)-Fe(1)-C(6) 123.6(3) C(1)-Fe(1)-C(6) 127.0(3) C(5)-Fe(1)-C(10) 129.5(3) C(9)-Fe(1)-C(10) 40.3(3) C(2)-Fe(1)-C(10) 153.7(4) C(8)-Fe(1)-C(10) 68.3(3) C(3)-Fe(1)-C(10) 121.2(3) C(7)-Fe(1)-C(10) 68.4(3) C(4)-Fe(1)-C(10) 110.9(3) C(1)-Fe(1)-C(10) 165.5(3) C(6)-Fe(1)-C(10) 40.5(3) C(23)-Fe(2)-C(15) 159.4(4) C(23)-Fe(2)-C(19) 40.9(3) C(15)-Fe(2)-C(19) 123.0(3) C(23)-Fe(2)-C(18) 122.0(3) C(15)-Fe(2)-C(18) 68.5(3) C(19)-Fe(2)-C(18) 157.6(3) C(23)-Fe(2)-C(22) 40.1(4) C(15)-Fe(2)-C(22) 159.2(4) C(19)-Fe(2)-C(22) 68.3(4) C(18)-Fe(2)-C(22) 107.9(4) C(23)-Fe(2)-C(21) 67.3(3) C(15)-Fe(2)-C(21) 124.0(3) C(19)-Fe(2)-C(21) 68.3(3) C(18)-Fe(2)-C(21) 123.9(3) C(22)-Fe(2)-C(21) 39.7(3) C(23)-Fe(2)-C(16) 123.5(4) C(15)-Fe(2)-C(16) 40.1(3) C(19)-Fe(2)-C(16) 107.0(3) C(18)-Fe(2)-C(16) 68.3(3) C(22)-Fe(2)-C(16) 159.5(4) C(21)-Fe(2)-C(16) 159.0(3) C(23)-Fe(2)-C(20) 68.2(3) C(15)-Fe(2)-C(20) 108.1(4) C(19)-Fe(2)-C(20) 41.0(3) C(18)-Fe(2)-C(20) 160.0(4) C(22)-Fe(2)-C(20) 67.9(3) C(21)-Fe(2)-C(20) 40.5(3) C(16)-Fe(2)-C(20) 122.6(3) C(23)-Fe(2)-C(17) 107.2(3) C(15)-Fe(2)-C(17) 68.1(4) C(19)-Fe(2)-C(17) 121.4(4) C(18)-Fe(2)-C(17) 40.8(3) C(22)-Fe(2)-C(17) 123.5(3) C(21)-Fe(2)-C(17) 159.5(3) C(16)-Fe(2)-C(17) 40.5(3) C(20)-Fe(2)-C(17) 157.9(4) C(23)-Fe(2)-C(14) 158.1(3) C(15)-Fe(2)-C(14) 41.1(3) C(19)-Fe(2)-C(14) 159.5(3) C(18)-Fe(2)-C(14) 41.4(3) C(22)-Fe(2)-C(14) 122.5(3) C(21)-Fe(2)-C(14) 107.9(3) C(16)-Fe(2)-C(14) 68.9(3) C(20)-Fe(2)-C(14) 123.1(3) C(17)-Fe(2)-C(14) 69.4(3) C(14)-P(1)-C(10) 97.9(4) C(14)-P(1)-C(11) 97.7(4) C(10)-P(1)-C(11) 103.8(4) C(5)-C(1)-C(2) 105.3(8) C(5)-C(1)-Fe(1) 67.9(5) C(2)-C(1)-Fe(1) 69.1(5) C(3)-C(2)-C(1) 108.4(8) C(3)-C(2)-Fe(1) 69.9(5) C(1)-C(2)-Fe(1) 70.4(5) C(4)-C(3)-C(2) 108.5(8) C(4)-C(3)-Fe(1) 70.5(5) C(2)-C(3)-Fe(1) 69.6(5) C(5)-C(4)-C(3) 106.8(8) C(5)-C(4)-Fe(1) 68.3(5) C(3)-C(4)-Fe(1) 69.5(5) C(4)-C(5)-C(1) 110.9(8) C(4)-C(5)-Br(1)#1 127.0(7) C(1)-C(5)-Br(1)#1 121.8(7) C(4)-C(5)-Fe(1) 71.9(5) C(1)-C(5)-Fe(1) 71.4(5) Br(1)#1-C(5)-Fe(1) 128.5(4) C(7)-C(6)-C(10) 108.8(8) C(7)-C(6)-Fe(1) 69.3(5) C(10)-C(6)-Fe(1) 70.7(4) C(6)-C(7)-C(8) 107.8(8) C(6)-C(7)-Fe(1) 70.1(5) C(8)-C(7)-Fe(1) 69.6(5) C(9)-C(8)-C(7) 107.6(7) C(9)-C(8)-Fe(1) 69.2(5) C(7)-C(8)-Fe(1) 69.9(5) C(8)-C(9)-C(10) 109.3(8) C(8)-C(9)-Fe(1) 70.0(5) C(10)-C(9)-Fe(1) 71.7(5) C(9)-C(10)-C(6) 106.5(7) C(9)-C(10)-P(1) 123.1(6) C(6)-C(10)-P(1) 129.9(6) C(9)-C(10)-Fe(1) 68.0(4) C(6)-C(10)-Fe(1) 68.9(4) P(1)-C(10)-Fe(1) 133.7(4) C(13)-C(11)-C(12) 109.9(7) C(13)-C(11)-P(1) 111.6(6) C(12)-C(11)-P(1) 109.0(6) C(15)-C(14)-C(18) 105.3(7) C(15)-C(14)-P(1) 125.2(6) C(18)-C(14)-P(1) 129.5(6) C(15)-C(14)-Fe(2) 68.6(5) C(18)-C(14)-Fe(2) 68.8(5) P(1)-C(14)-Fe(2) 128.2(4) C(16)-C(15)-C(14) 109.9(7) C(16)-C(15)-Fe(2) 70.5(5) C(14)-C(15)-Fe(2) 70.3(4) C(15)-C(16)-C(17) 108.5(7) C(15)-C(16)-Fe(2) 69.4(5) C(17)-C(16)-Fe(2) 69.8(5) C(18)-C(17)-C(16) 107.6(7) C(18)-C(17)-Fe(2) 69.3(5) C(16)-C(17)-Fe(2) 69.7(5) C(17)-C(18)-C(14) 108.7(8) C(17)-C(18)-Fe(2) 69.8(5) C(14)-C(18)-Fe(2) 69.8(4) C(23)-C(19)-C(20) 105.9(7) C(23)-C(19)-Fe(2) 68.3(5) C(20)-C(19)-Fe(2) 69.4(5) C(21)-C(20)-C(19) 107.6(7) C(21)-C(20)-Fe(2) 69.8(5) C(19)-C(20)-Fe(2) 69.7(5) C(22)-C(21)-C(20) 108.8(8) C(22)-C(21)-Fe(2) 70.1(5) C(20)-C(21)-Fe(2) 69.7(5) C(23)-C(22)-C(21) 107.9(8) C(23)-C(22)-Fe(2) 68.8(5) C(21)-C(22)-Fe(2) 70.1(5) C(22)-C(23)-C(19) 109.7(7) C(22)-C(23)-Br(2) 125.6(7) C(19)-C(23)-Br(2) 124.5(6) C(22)-C(23)-Fe(2) 71.1(5) C(19)-C(23)-Fe(2) 70.8(5) Br(2)-C(23)-Fe(2) 128.3(4) _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: #1 -x+1,-y,-z Table 5. Anisotropic displacement parameters (A^2 x 10^3) for 1. 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 _______________________________________________________________________ Fe(1) 17(1) 17(1) 16(1) 0(1) 0(1) 5(1) Fe(2) 13(1) 18(1) 16(1) 0(1) 0(1) 3(1) Br(1) 33(1) 35(1) 31(1) 9(1) -2(1) 3(1) Br(2) 21(1) 51(1) 40(1) -1(1) -8(1) -4(1) P(1) 15(1) 14(1) 16(1) 0(1) 0(1) 1(1) C(1) 23(5) 16(5) 27(5) 1(4) -2(4) 10(4) C(2) 29(5) 31(6) 30(5) -3(4) 5(4) 18(4) C(3) 19(5) 40(7) 34(6) 5(4) 5(4) 3(4) C(4) 18(5) 21(5) 32(5) -2(4) 6(4) 5(4) C(5) 18(4) 28(6) 17(5) 5(4) 1(4) 14(4) C(6) 15(4) 22(5) 15(4) -1(3) 1(3) 6(3) C(7) 15(4) 15(5) 35(5) 1(4) -3(4) 2(3) C(8) 24(3) 16(3) 21(3) 1(2) -6(3) 5(2) C(9) 24(3) 16(3) 21(3) 1(2) -6(3) 5(2) C(10) 10(4) 13(5) 23(5) -4(3) 2(3) 5(3) C(11) 15(4) 20(5) 18(4) 1(3) 2(3) 1(3) C(12) 26(5) 27(5) 21(5) -3(4) -3(4) -2(4) C(13) 28(5) 27(5) 14(4) 2(4) -6(4) 4(4) C(14) 14(4) 21(5) 12(4) 2(3) 1(3) 2(3) C(15) 20(5) 19(5) 18(5) -4(3) -4(3) 4(4) C(16) 33(5) 12(5) 25(5) 2(4) 7(4) 6(4) C(17) 13(4) 38(6) 20(5) 8(4) 8(3) 2(4) C(18) 16(4) 28(5) 12(4) 3(3) 0(3) -4(4) C(19) 22(5) 18(5) 15(4) 2(3) -4(3) 4(3) C(20) 25(5) 36(6) 14(5) 3(4) 0(4) -7(4) C(21) 20(5) 19(6) 22(5) 8(3) 10(4) 8(4) C(22) 34(5) 20(5) 15(5) -4(3) 4(4) 1(4) C(23) 13(4) 34(6) 17(5) 3(4) -1(3) -1(4) _______________________________________________________________________ Table 6. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for 1. ________________________________________________________________ x y z U(eq) ________________________________________________________________ H(1) 7363(11) -4987(9) -2604(6) 27 H(2) 8167(12) -3973(10) -4017(7) 37 H(3) 9688(11) -1632(10) -3482(7) 37 H(4) 9838(11) -1171(9) -1751(6) 29 H(5) 8325(11) -3173(9) -1234(6) 25 H(6) 4594(10) -1324(9) -1299(6) 21 H(7) 3622(11) -3359(9) -2541(6) 27 H(8) 4355(11) -2715(9) -4073(6) 25 H(9) 5841(11) -316(9) -3766(6) 25 H(11) 5244(11) 1119(9) -411(6) 21 H(12A) 5541(31) 3580(19) -182(33) 38 H(12B) 7552(48) 3488(22) -306(29) 38 H(12C) 6779(76) 3036(10) 573(8) 38 H(13A) 7726(39) -332(19) -678(26) 35 H(13B) 7831(41) 543(46) 327(10) 35 H(13C) 8922(12) 1036(31) -440(34) 35 H(15) 4595(11) 4578(9) -1655(6) 24 H(16) 1425(12) 5024(9) -1766(6) 28 H(17) -166(11) 2665(10) -2113(6) 28 H(18) 2073(10) 731(10) -2195(5) 22 H(19) 1526(11) 5023(9) -4014(5) 22 H(20) 4785(11) 4599(10) -3893(6) 30 H(21) 5224(11) 1958(9) -4170(6) 24 H(22) 2331(12) 751(10) -4444(6) 28 ________________________________________________________________