Table 1. Crystal data and structure refinement for 98SRC091. Identification code 98SRC091 Empirical formula C34 H28 Cl3 Fe O P2 Re Formula weight 862.90 Temperature 293(2) K Wavelength 1.54178 A Crystal system Orthorhombic Space group Pbcn Unit cell dimensions a = 9.419(2) A b = 15.687(3) A c = 22.166(5) A Volume 3275.2(12) A^3 Z 4 Density (calculated) 1.750 Mg/m^3 Absorption coefficient 14.052 mm^-1 F(000) 1688 Crystal size 0.5 x 0.2 x 0.2 mm Theta range for data collection 3.99 to 66.93 deg. Index ranges 0<=h<=11, 0<=k<=18, -26<=l<=0 Reflections collected 2923 Independent reflections 2923 [R(int) = 0.0239] Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 2923 / 2 / 195 Goodness-of-fit on F^2 1.060 Final R indices [I>2sigma(I)] R1 = 0.0534, wR2 = 0.1515 R indices (all data) R1 = 0.0673, wR2 = 0.1589 Extinction coefficient 0.0 Largest diff. peak and hole 1.661 and -1.626 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for 98SRC091. ________________________________________________________________ x y z U(eq) ________________________________________________________________ Re(1) 0 9420(1) 2500 33(1) Fe(1) 0 6645(1) 2500 39(1) Cl(1) 669(2) 10532(1) 3165(1) 46(1) Cl(2) 2282(3) 9221(3) 2243(2) 27(1) O(1) 1775(11) 9255(9) 2247(7) 27(1) P(1) 500(2) 8430(1) 3356(1) 23(1) C(1) -1445(8) 7134(5) 3098(3) 44(2) C(2) -1600(12) 6234(5) 3075(4) 69(3) C(3) -299(13) 5887(5) 3245(5) 70(3) C(4) 706(10) 6549(4) 3364(3) 48(2) C(5) -40(6) 7337(4) 3264(3) 30(1) C(6) 2359(6) 8417(4) 3560(3) 27(1) C(7) 3326(8) 7884(6) 3274(4) 56(2) C(8) 4737(8) 7890(8) 3431(5) 66(3) C(9) 5221(8) 8451(6) 3870(4) 54(2) C(10) 4287(9) 8961(6) 4153(4) 59(2) C(11) 2861(8) 8952(5) 4009(3) 46(2) C(12) -422(8) 8698(4) 4064(3) 36(2) C(13) -391(14) 8110(7) 4520(5) 86(4) C(14) -1034(18) 8273(8) 5062(5) 113(6) C(15) -1800(12) 9001(6) 5150(4) 73(3) C(16) -1857(9) 9583(5) 4700(3) 51(2) C(17) -1206(8) 9422(4) 4162(3) 38(2) ________________________________________________________________ Table 3. Bond lengths [A] and angles [deg] for 98SRC091. _____________________________________________________________ Re(1)-O(1)#1 1.782(10) Re(1)-O(1) 1.783(10) Re(1)-Cl(2)#1 2.245(3) Re(1)-Cl(2) 2.245(3) Re(1)-Cl(1) 2.368(2) Re(1)-Cl(1)#1 2.368(2) Re(1)-P(1)#1 2.497(2) Re(1)-P(1) 2.497(2) Fe(1)-C(5) 2.011(7) Fe(1)-C(5)#1 2.011(7) Fe(1)-C(4)#1 2.033(7) Fe(1)-C(4) 2.033(7) Fe(1)-C(1) 2.048(8) Fe(1)-C(1)#1 2.048(8) Fe(1)-C(3) 2.054(9) Fe(1)-C(3)#1 2.054(9) Fe(1)-C(2) 2.076(10) Fe(1)-C(2)#1 2.076(10) P(1)-C(5) 1.800(7) P(1)-C(6) 1.809(6) P(1)-C(12) 1.843(7) C(1)-C(5) 1.410(9) C(1)-C(2) 1.419(11) C(2)-C(3) 1.39(2) C(3)-C(4) 1.429(12) C(4)-C(5) 1.439(9) C(6)-C(11) 1.386(9) C(6)-C(7) 1.390(10) C(7)-C(8) 1.373(11) C(8)-C(9) 1.389(14) C(9)-C(10) 1.344(13) C(10)-C(11) 1.380(11) C(12)-C(13) 1.367(12) C(12)-C(17) 1.372(10) C(13)-C(14) 1.371(14) C(14)-C(15) 1.365(14) C(15)-C(16) 1.352(12) C(16)-C(17) 1.365(10) O(1)#1-Re(1)-O(1) 163.2(9) Cl(2)#1-Re(1)-Cl(2) 164.0(2) O(1)#1-Re(1)-Cl(1) 99.3(5) O(1)-Re(1)-Cl(1) 93.1(5) Cl(2)#1-Re(1)-Cl(1) 101.48(12)Cl(2)-Re(1)-Cl(1) 90.32(12) O(1)#1-Re(1)-Cl(1)#1 93.1(5) O(1)-Re(1)-Cl(1)#1 99.3(5) Cl(2)#1-Re(1)-Cl(1)#1 90.32(12)Cl(2)-Re(1)-Cl(1)#1 101.48(12) Cl(1)-Re(1)-Cl(1)#1 85.20(10)O(1)#1-Re(1)-P(1)#1 88.4(5) O(1)-Re(1)-P(1)#1 81.2(5) Cl(2)#1-Re(1)-P(1)#1 85.74(11) Cl(2)-Re(1)-P(1)#1 84.33(12)Cl(1)-Re(1)-P(1)#1 168.85(6) Cl(1)#1-Re(1)-P(1)#1 86.28(6) O(1)#1-Re(1)-P(1) 81.2(5) O(1)-Re(1)-P(1) 88.4(5) Cl(2)#1-Re(1)-P(1) 84.33(12) Cl(2)-Re(1)-P(1) 85.74(11)Cl(1)-Re(1)-P(1) 86.28(6) Cl(1)#1-Re(1)-P(1) 168.85(6) P(1)#1-Re(1)-P(1) 103.02(7) C(5)-Fe(1)-C(5)#1 114.6(4) C(5)-Fe(1)-C(4)#1 145.7(3) C(5)#1-Fe(1)-C(4)#1 41.7(3) C(5)-Fe(1)-C(4) 41.7(3) C(5)#1-Fe(1)-C(4) 145.7(3) C(4)#1-Fe(1)-C(4) 171.5(4) C(5)-Fe(1)-C(1) 40.6(3) C(5)#1-Fe(1)-C(1) 110.8(3) C(4)#1-Fe(1)-C(1) 114.8(3) C(4)-Fe(1)-C(1) 68.6(3) C(5)-Fe(1)-C(1)#1 110.8(3) C(5)#1-Fe(1)-C(1)#1 40.6(3) C(4)#1-Fe(1)-C(1)#1 68.6(3) C(4)-Fe(1)-C(1)#1 114.8(3) C(1)-Fe(1)-C(1)#1 136.0(4) C(5)-Fe(1)-C(3) 68.5(3) C(5)#1-Fe(1)-C(3) 172.5(3) C(4)#1-Fe(1)-C(3) 132.1(3) C(4)-Fe(1)-C(3) 40.9(3) C(1)-Fe(1)-C(3) 66.8(4) C(1)#1-Fe(1)-C(3) 145.9(4) C(5)-Fe(1)-C(3)#1 172.5(3) C(5)#1-Fe(1)-C(3)#1 68.5(3) C(4)#1-Fe(1)-C(3)#1 40.9(3) C(4)-Fe(1)-C(3)#1 132.1(3) C(1)-Fe(1)-C(3)#1 145.9(4) C(1)#1-Fe(1)-C(3)#1 66.8(4) C(3)-Fe(1)-C(3)#1 109.3(6) C(5)-Fe(1)-C(2) 68.7(3) C(5)#1-Fe(1)-C(2) 134.2(3) C(4)#1-Fe(1)-C(2) 108.5(4) C(4)-Fe(1)-C(2) 68.7(4) C(1)-Fe(1)-C(2) 40.2(3) C(1)#1-Fe(1)-C(2) 174.5(3) C(3)-Fe(1)-C(2) 39.4(4) C(3)#1-Fe(1)-C(2) 114.5(4) C(5)-Fe(1)-C(2)#1 134.2(3) C(5)#1-Fe(1)-C(2)#1 68.7(3) C(4)#1-Fe(1)-C(2)#1 68.7(4) C(4)-Fe(1)-C(2)#1 108.5(4) C(1)-Fe(1)-C(2)#1 174.5(4) C(1)#1-Fe(1)-C(2)#1 40.2(3) C(3)-Fe(1)-C(2)#1 114.5(4) C(3)#1-Fe(1)-C(2)#1 39.4(4) C(2)-Fe(1)-C(2)#1 143.9(5) C(5)-P(1)-C(6) 106.9(3) C(5)-P(1)-C(12) 100.4(3) C(6)-P(1)-C(12) 104.2(3) C(5)-P(1)-Re(1) 117.0(2) C(6)-P(1)-Re(1) 112.3(2) C(12)-P(1)-Re(1) 114.6(2) C(5)-C(1)-C(2) 109.3(7) C(5)-C(1)-Fe(1) 68.3(4) C(2)-C(1)-Fe(1) 70.9(6) C(3)-C(2)-C(1) 106.7(8) C(3)-C(2)-Fe(1) 69.4(6) C(1)-C(2)-Fe(1) 68.8(5) C(2)-C(3)-C(4) 110.4(7) C(2)-C(3)-Fe(1) 71.1(5) C(4)-C(3)-Fe(1) 68.8(4) C(3)-C(4)-C(5) 105.8(7) C(3)-C(4)-Fe(1) 70.3(5) C(5)-C(4)-Fe(1) 68.3(4) C(1)-C(5)-C(4) 107.7(6) C(1)-C(5)-P(1) 120.7(5) C(4)-C(5)-P(1) 131.5(5) C(1)-C(5)-Fe(1) 71.1(4) C(4)-C(5)-Fe(1) 70.0(4) P(1)-C(5)-Fe(1) 127.2(4) C(11)-C(6)-C(7) 117.9(6) C(11)-C(6)-P(1) 120.3(5) C(7)-C(6)-P(1) 121.8(5) C(8)-C(7)-C(6) 121.0(8) C(7)-C(8)-C(9) 120.0(9) C(10)-C(9)-C(8) 119.3(7) C(9)-C(10)-C(11) 121.5(8) C(10)-C(11)-C(6) 120.3(7) C(13)-C(12)-C(17) 117.0(7) C(13)-C(12)-P(1) 117.7(6) C(17)-C(12)-P(1) 125.2(5) C(12)-C(13)-C(14) 120.8(9) C(15)-C(14)-C(13) 120.9(9) C(16)-C(15)-C(14) 118.8(8) C(15)-C(16)-C(17) 120.1(8) C(16)-C(17)-C(12) 122.1(7) _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: #1 -x,y,-z+1/2 Table 4. Anisotropic displacement parameters (A^2 x 10^3) for 98SRC091. _______________________________________________________________________ U11 U22 U33 U23 U13 U12 _______________________________________________________________________ Re(1) 54(1) 11(1) 33(1) 0 -16(1) 0 Fe(1) 61(1) 14(1) 41(1) 0 -21(1) 0 Cl(1) 70(1) 25(1) 42(1) -15(1) 10(1) -16(1) Cl(2) 22(2) 28(1) 30(1) 3(1) 8(2) 0(2) O(1) 22(2) 28(1) 30(1) 3(1) 8(2) 0(2) P(1) 29(1) 19(1) 21(1) -1(1) 1(1) -1(1) C(1) 49(4) 35(4) 49(4) 11(3) -4(3) -16(3) C(2) 107(8) 44(5) 55(5) 20(4) -20(5) -33(5) C(3) 131(10) 21(4) 58(6) 15(4) -22(6) -16(5) C(4) 73(5) 28(4) 42(4) 7(3) -32(4) 10(4) C(5) 32(3) 26(3) 31(3) 3(3) -8(2) 4(3) C(6) 28(3) 28(3) 25(3) 2(2) -1(2) -1(3) C(7) 35(4) 80(6) 52(5) -29(4) -12(3) 0(4) C(8) 33(4) 107(9) 57(6) -25(6) 2(4) -2(5) C(9) 36(4) 63(6) 64(6) 4(5) -10(4) -11(4) C(10) 56(5) 55(5) 66(5) -15(4) -32(5) -7(4) C(11) 47(4) 47(4) 45(4) -11(3) -13(3) 12(4) C(12) 48(4) 32(4) 28(3) -2(3) 6(3) -8(3) C(13) 134(10) 60(7) 65(6) 26(5) 46(7) 41(6) C(14) 203(17) 89(8) 48(6) 34(6) 60(8) 41(9) C(15) 118(9) 66(6) 35(5) -7(4) 30(5) -12(6) C(16) 65(5) 52(4) 37(4) -19(4) 9(4) -1(4) C(17) 53(4) 40(4) 23(3) -7(3) 3(3) -4(3) _______________________________________________________________________ Table 5. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for 98SRC091. ________________________________________________________________ x y z U(eq) ________________________________________________________________ H(1) -2158(8) 7527(5) 3016(3) 53 H(2) -2413(12) 5935(5) 2967(4) 83 H(3) -111(13) 5307(5) 3277(5) 84 H(4) 1647(10) 6484(4) 3482(3) 57 H(7) 3013(8) 7517(6) 2972(4) 67 H(8) 5367(8) 7520(8) 3242(5) 79 H(9) 6180(8) 8473(6) 3967(4) 65 H(10) 4609(9) 9328(6) 4453(4) 70 H(11) 2235(8) 9306(5) 4215(3) 55 H(13) 73(14) 7594(7) 4460(5) 103 H(14) -949(18) 7881(8) 5375(5) 136 H(15) -2273(12) 9096(6) 5512(4) 88 H(16) -2340(9) 10093(5) 4758(3) 62 H(17) -1297(8) 9817(4) 3851(3) 46 ________________________________________________________________