Inorg. Chem. 1982, 21, 435-431 Table 11. Bond Distances (A) and Angles (Deg) for Rh, (O,CCF,), (Me, S O 4 ) , Distances F(4)-C(4) Rh(1)-Rh(1’) 2.409 (1) 0(1) 2.032 (3) F(5)-C(4) F(6)-C(4) 2.026 (3) O(2) F(7)-C(6) O(3’) 2.042 (3) F(8)-C(6) O(4‘) 2.040 (3) F(9)-C(6) O(1Oj 2.263 (3) F(10)-C(8) Rh(2)-Rh(2) 2.407 (1) F(ll)-C(8) 2.039 (3) O(5‘) F(12)-C(8) 2.033 (3) O(6) O(l)-C(l) O(7) 2.040 (2) 0(2)-C(3) O(8‘) 2.029 (3) 0(3)-C(1) O(20) 2.234 (3) 0(4)-C(3) S(lO)-O(lO) 1.515 (3) 0(5)-C(S) C(10) 1.781 (6) 0(6)-C(7) S(lO)-C(ll) 1.749 (7) 0(7)-C(5) S(20)-0(20) 1.516 (3) C(20) 1.771 (6) 0(8)-C(7) C(l)-C(2) C(21) 1.776 (6) C(3)-C(4) 1.303 (6) F(l)-C(2) C(5)-C(6) F(2)-C(2) 1.296 (6) C(7)-C(8) F(3)-C(2) 1.273 (6) Rh(1‘)-Rh(1)-O(1) O(2) O(3‘) O(4’) O(10) O(l)-Rh(l)-O(2) O(3’) oi4’j O(1)-Rh(1)-O(l0) 0(2)-Rh(l)-0(3‘) O(2)-Rh( 1)-O(4‘) O(10) 0(3‘)-Rh(l)-0(4’) O(10) 0(4‘)-Rh(l)-0(10) Rh(2’)-Rh(2)-0(5‘) O(6) O(7) O(8‘) O(20) 0(5’)-Rh(2)-0(6) O(7) O(8‘) O(20) 0(6)-Rh(2)-0(7) O(8’) O(20) 0(7)-Rh(2)-0(8’) O(20) 0(8’)-Rh(2)-0(20) O(lO)-S(lO)-C(lO) C(11) C(l0)-S(l0)-C(l1) 0(20)-S(20)-C(20) C(21) C(2O)-S(2O)-C(21) Rh(1)-O(1)-C(1) Rh(l)-0(2)-C(3) Rh(l)-0(3’)-C( 1’) Rh(l)-0(4’)-C(3’) Rh( 2)-0(5‘)-C(5‘)
1.319 ( 5 ) 1.324 ( 5 ) 1.314 (5) 1.315 ( 5 ) 1.311 (5) 1.302 ( 5 ) 1.300 (6) 1.312 (5) 1.261 (6) 1.253 (5) 1.245 (4) 1.243 ( 5 ) 1.250 (4) 1.252 ( 5 ) 1.249 ( 5 ) 1.245 ( 5 ) 1.254 ( 5 ) 1.533 (6) 1.530 (5) 1.520 (5) 1.513 (6)
Angles 88.00 (8) Rh(2)-0(6)-C(7) 87.83 (7) Rh(2)-0(7)-C(S) 87.88 (8) Rh(2)-0(8‘)-C(7’) 87.76 (7) Rh(l)-O(lO)-S(lO) 176.29 (7) Rh(2)-0(20)-S(20) 89.8 (1) O(l)-C(l)-O(3) 175.9 (1) C(2) 89.5 i i j o(~)-c(I)-c(~) 91.4 (1) F(l)-C(2)-F(2) 89.6 (1) F(l)-C(2)-F(3) 175.6 (1) F(l)-C(2)-C(l) 88.5 (1) F(2)-C(2)-F(3) 90.7 (1) C(1) 92.7 (1) F(3)-C(2)-C(l) 95.9 (1) 0(2)-C(3)-0(4) 88.45 (8) 0(2)-C(3)-C(4) 88.08 (8) 0(4)-C(3)-C(4) 87.30 (7) F(4)-C(4)-F(5) 87.70 (8) F(6) 176.31 (8) C(3) 88.9 (1) F(5)-C(4)-F(6) 175.7 (1) C(3 ) 90.8 (1) F(6)-C(4)-C(3) 88.1 (1) 0(5) 1 (1.434 (2) A) > (H2N),S02 (1.391 (8) A). This ordering follows the electronegativities of the amide groups. The crystal structure appears to be held together by weak hydrogen bonds between H(1) and the O(2) of an adjacent molecule. The N-H-.O angle is 180°, and the H.-0 separation is 2.06 A. The N - - 0 distance for a normal hydrogen bond is 2.9 A;14 in 1 it is 3.06 A. Acknowledgment. We are grateful to the Office of Naval Research (Contract N00014-76-C-0577, Task No. N R 053612) and the National Science Foundation (Grant Nos. CHE79-10155 and CHE78-09729) for generous financial support. Registry No. 1, 13952-67-5. Supplementary Material Available: A table of observed and calculated structure factors (8 pages). Ordering information is given on any current masthead page. (13) For example, dsN = 1.648 (2) A in (Me2N)2SF2(Cowley,A. H.: Riley, P. E.; Szobota, J. S.;Walker, M. L. J. Am. Chem. SOC.1979, 101, 562C-5624). For a discussion of this phenomenon in aminophosphines, see: Cowlev. A. H.: Davis, R. E.; Remadna, K. Znora. Chem. 1981,20, 2146-215fand references therein. (14) Hamilton, W. C.; Ibers, J. A. "Hydrogen Bonding in Solids: Methods of Molecular Structure Determination"; W. A. Benjamin: New York, 1968; p 16.
