Table 1. Crystal data and structure refinement for [WI2(CO)3(NCPh)2]. Identification code 93SRC099 Empirical formula C8.50 H5 I N O1.50 W0.50 Formula weight 363.96 Temperature 150(2) K Wavelength 0.71069 A Crystal system Orthorhombic Space group Pnam Unit cell dimensions a = 7.815(3) A b = 13.839(5) A c = 18.475(3) A Volume 1998.1(11) A^3 Z 8 Density (calculated) 2.420 Mg/m^3 Absorption coefficient 8.888 mm^-1 F(000) 1320 Crystal size ? x ? x ? mm Theta range for data collection 1.84 to 24.94 deg. Index ranges -9<=h<=6, -15<=k<=15, -19<=l<=20 Reflections collected 5755 Independent reflections 1643 [R(int) = 0.0850] Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 1643 / 0 / 126 Goodness-of-fit on F^2 0.693 Final R indices [I>2sigma(I)] R1 = 0.0346, wR2 = 0.0780 R indices (all data) R1 = 0.0378, wR2 = 0.0813 Largest diff. peak and hole 1.267 and -2.144 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for [WI2(CO)3(NCPh)2].U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________ x y z U(eq) ________________________________________________________________ I(1) -456(1) 11859(1) 2500 20(1) I(2) 2694(1) 8237(1) 2500 21(1) W(1) 507(1) 9862(1) 2500 11(1) N(1) 2285(7) 10459(4) 3292(3) 18(1) O(10) -3483(10) 9959(5) 2500 35(2) O(20) -794(7) 8692(4) 3843(3) 33(1) C(1) 3258(9) 10737(5) 3706(4) 17(2) C(2) 4440(8) 11067(5) 4253(4) 15(2) C(3) 6107(10) 11332(5) 4061(4) 21(2) C(4) 7212(10) 11602(5) 4601(4) 27(2) C(5) 6675(11) 11644(5) 5306(4) 26(2) C(6) 5029(10) 11388(5) 5488(4) 26(2) C(7) 3884(10) 11089(4) 4966(3) 17(2) C(10) -1993(15) 9955(7) 2500 21(2) C(20) -346(8) 9112(5) 3336(4) 19(2) ________________________________________________________________ _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: Table 4. Bond lengths [A] and angles [deg] for [WI2(CO)3(NCPh)2]. _____________________________________________________________ I(1)-W(1) 2.8651(12) I(2)-W(1) 2.8242(11) W(1)-C(10) 1.958(12) W(1)-C(20)#1 1.977(7) W(1)-C(20) 1.977(7) W(1)-N(1) 2.180(6) W(1)-N(1)#1 2.180(6) N(1)-C(1) 1.146(8) O(10)-C(10) 1.164(13) O(20)-C(20) 1.156(8) C(1)-C(2) 1.444(9) C(2)-C(7) 1.386(9) C(2)-C(3) 1.399(10) C(3)-C(4) 1.371(10) C(4)-C(5) 1.371(11) C(5)-C(6) 1.376(11) C(6)-C(7) 1.380(10) C(10)-W(1)-C(20) 72.4(2) C(20)#1-W(1)-C(20) 102.8(4) C(10)-W(1)-N(1) 127.7(2) C(20)#1-W(1)-N(1) 159.8(2) C(20)-W(1)-N(1) 83.7(2) C(10)-W(1)-N(1)#1 127.7(2) C(20)#1-W(1)-N(1)#1 83.7(2) C(20)-W(1)-N(1)#1 159.8(2) N(1)-W(1)-N(1)#1 84.3(3) C(10)-W(1)-I(2) 131.0(3) C(20)#1-W(1)-I(2) 77.7(2) C(20)-W(1)-I(2) 77.7(2) N(1)-W(1)-I(2) 85.2(2) N(1)#1-W(1)-I(2) 85.2(2) C(10)-W(1)-I(1) 71.0(3) C(20)#1-W(1)-I(1) 114.7(2) C(20)-W(1)-I(1) 114.7(2) N(1)-W(1)-I(1) 78.6(2) N(1)#1-W(1)-I(1) 78.6(2) I(2)-W(1)-I(1) 158.00(2) C(1)-N(1)-W(1) 177.1(6) N(1)-C(1)-C(2) 177.5(7) C(7)-C(2)-C(3) 121.8(6) C(7)-C(2)-C(1) 118.1(6) C(3)-C(2)-C(1) 120.0(6) C(4)-C(3)-C(2) 118.2(7) C(5)-C(4)-C(3) 120.7(7) C(4)-C(5)-C(6) 120.5(7) C(5)-C(6)-C(7) 120.8(7) C(6)-C(7)-C(2) 117.9(7) O(10)-C(10)-W(1) 176.5(8) O(20)-C(20)-W(1) 177.2(6) _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: #1 x,y,-z+1/2 Table 5. Anisotropic displacement parameters (A^2 x 10^3) for [WI2(CO)3(NCPh)2]. 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 _______________________________________________________________________ I(1) 19(1) 14(1) 29(1) 0 0 -1(1) I(2) 26(1) 20(1) 16(1) 0 0 7(1) W(1) 12(1) 13(1) 8(1) 0 0 -2(1) N(1) 24(3) 21(3) 10(3) 0(2) -3(3) -3(3) O(10) 14(5) 39(5) 53(6) 0 0 -5(3) O(20) 44(3) 37(3) 17(3) 11(3) 14(2) -9(3) C(1) 19(4) 16(4) 16(4) 3(3) 4(3) 3(3) C(2) 24(4) 7(3) 15(4) -4(3) -6(3) 1(3) C(3) 31(4) 19(4) 12(4) 0(3) -4(3) -5(3) C(4) 26(5) 22(4) 35(5) 0(3) -2(3) -7(3) C(5) 38(5) 16(4) 24(5) -2(3) -13(4) -6(3) C(6) 41(5) 24(4) 13(4) -2(3) 1(4) 4(4) C(7) 22(4) 18(4) 12(4) -1(3) 1(3) -1(3) C(10) 28(7) 14(5) 21(6) 0 0 1(4) C(20) 18(4) 22(4) 18(4) -4(3) 0(3) -1(3) _______________________________________________________________________ Table 6. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for [WI2(CO)3(NCPh)2]. ________________________________________________________________ x y z U(eq) ________________________________________________________________ H(3) 6457(10) 11325(5) 3580(4) 14(17) H(4) 8337(10) 11759(5) 4487(4) 19(19) H(5) 7430(11) 11847(5) 5665(4) 46(27) H(6) 4684(10) 11417(5) 5970(4) 39(25) H(7) 2775(10) 10908(4) 5088(3) 0(15) ________________________________________________________________