Inorg. Chem., 1996, 35(3), 549-550, DOI:10.1021/ic9508637

Terms & ConditionsElectronic Supporting Information files are available without a subscription to ACS Web Editions. The American ChemicalSociety holds a copyright ownership interest in any copyrightable Supporting Information. Files available from the ACSwebsite may be downloaded for personal use only. Users are not otherwise permitted to reproduce, republish,redistribute, or sell any Supporting Information from the ACS website, either in whole or in part, in either machine-readable form or any other form without permission from the American Chemical Society. For permission to reproduce,republish and redistribute this material, requesters must process their own requests via the RightsLink permissionsystem. Information about how to use the RightsLink permission system can be found athttp://pubs.acs.org/page/copyright/permissions.html

Copyright © 1996 American Chemical Society

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 161

161

Table S23. Intramolecular Bond Angles (0) Involving Nonhydrogen Atoms for [Rh2(dimen) 4 1-

[TFPB]2 (cont.). Estimated standard deviations in the last digit are given in parentheses.

atom atom atom angle atom atom

C8F C18F F16F 38(5) C8F F16F

F4F C18F F5F 104(2) C8F F16F

F4F C18F F6F 127(2) F5F F16F

F4F C18F F14F 83(2) F5F F16F

F4F C18F Fl5F 29(2) F6F F16F

F4F C18F F16F 133(3) NIA' C12

F5F C18F F6F 98(2) N1A' C12

F5F C18F F14F 141(2) NIA' C12

F5F C18F F15F 76(2) N1A' C12

F5F C18F F16F 39(2) N1A' C12

F6F C18F F14F 51(2) NIA' C12

F6F C18F F15F 138(2) N1A' C12

F6F C18F F16F 60(2) C3 C12

F14F C18F F15F 110(2) C3 C12

F14F C18F F16F 110(3) C3 C12

F15F C18F F16F 109(3) C3 C12

C8F F14F F4F 49(1) C3 C12

C3 C12 C19 103(7) C2 C13

C7 C12 Clo 95(1) C2 C13

C7 C12 Cli 112(2) C2 C13

C7 C12 C14 145(2) C4 C13

C7 C12 C15 53(2) C4 C13

C7 C12 C19 61(1) C4 C13

atom

F6F

C18F

F6F

C18F

C18F

C3

C7

C1o

Cl

C14

C15

C19

C7

C10

C11

C14

C15

C17

C20

C21

C5

C9

C17

angle

66(2)

9(1)

140(4)

84(3)

58(2)

78(5)

101(2)

100(2)

124(2)

113(2)

100(2)

114(2)

42(6)

-65(6)

153(7)

136(7)

29(5)

160(7)

87(6)

53(6)

108(2)

102(2)

146(2)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 162

162

Table S23. Intramolecular Bond Angles (0) Involving Nonhydrogen Atoms for [Rh2(dimen) 4 1-

[TFPB] 2 (cont.). Estimated standard deviations in the last digit are given in parentheses.

atom atom atom angle atom atom atom angle

C1O C12 C1l 120(2) C4 C13 C20 63(2)

C1O C12 C14 71(2) C4 C13 C21 52(2)

C1O C12 C15 42(2) C5 C13 C9 124(2)

C1O C12 C19 141(2) C5 C13 C17 67(1)

Cli C12 C14 55(2) C5 C13 C20 46(2)

C11 C12 C15 135(2) C5 C13 C21 141(2)

C1l C12 C19 56(2) C9 C13 C17 62(1)

C14 C12 C15 109(2) C9 C13 C20 141(2)

C14 C12 C19 109(2) C9 C13 C21 51(2)

C15 C12 C19 109(2) C17 C13 C20 109(2)

N1A C13 C2 66(6) C17 C13 C21 109(2)

NIA C13 C4 97(1) C20 C13 C21 109(3)

NIA C13 C5 114(2) C3 C14 C1l 57(2)

N1A C13 C9 108(2) C3 C14 C12 .7(1)

N1A C13 C17 116(2) Cli C14 C12 51(2)

N1A C13 C20 110(2) C3 C15 C7 67(2)

NIA C13 C21 102(2) C3 C15 C1O 79(2)

C2 C13 C4 34(6) C3 C15 C12 7(1)

C2 C13 C5 131(7) C3 C15 C16 103(2)

C2 C13 C9 99(7) C7 C15 C1O 144(2)

C7 C15 C12 71(2) C5 C17 C9 105(2)

C7 C15 C16 52(1) C5 C17 C13 51(1)

C1O C15 C12 74(2) C5 C17 C16 70(1)

f 2 ~5o-rn/&9a-'

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 163 ,' , jI

163

Table S23. Intramolecular Bond Angles (0) Involving Nonhydrogen Atoms for [Rh2(dimen) 4 1-

[TFPBJ2 (cont.). Estimated standard deviations in the last digit are given in parentheses.

atom atom atom angle atom atom atom angle

C10 C15 C16 155(3) C5 C17 C18 155(2)

C12 C15 C16 109(2) C6 C17 C7 68(1)

C5 C16 C6 29(4) C6 C17 C8 118(2)

C5 C16 C7 105(2) C6 C17 C9 151(1)

C5 C16 C15 147(2) C6 C17 C13 97(2)

C5 C16 C17 57(1) C6 C17 C16 12(1)

C6 C16 C7 126(6) C6 C17 C18 117(2)

C6 C16 C15 167(6) C7 C17 C8 71(1)

C6 C16 C17 77(5) C7 C17 C9 130(2)

C7 C16 C15 62(2) C7 C17 C13 158(2)

C7 C16 C17 50(1) C7 C17 C16 56(1)

C15 C16 C17 109(2) C7 C17 C18 67(2)

C2 C17 C5 54(1) C8 C17 C9 62(1)

C2 C17 C6 100(1) C8 C17 C13 105(2)

C2 C17 C7 159(2) C8 C17 C16 111(2)

C2 C17 C8 103(1) C8 C17 C18 4(1)

C2 C17 C9 55(1) C9 C17 C13 57(1)

C2 C17 C13 3(1) C9 C17 C16 159(2)

C2 C17 C16 112(1) C9 C17 C18 65(2)

C2 C17 C18 107(2) C13 C17 C16 109(2)

C5 C17 C6 59(1) C13 C17 C18 109(2)

C5 C17 C7 124(2) C16 C17 C18 109(2)

C5 C17 C8 151(2) C7 C18 C8 86(11)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 164

164

Table S23. Intramolecular Bond Angles (0) Involving Nonhydrogen Atoms for [Rh2(dimen) 4 1-

[TFPB]2 (cont.). Estimated standard deviations in the last digit are given in parentheses.

atom atom atom angle atom atom atom angle

C7 C18 C9 103(1) C2 C20 C13 9(1)

C7 C18 C17 47(1) C4 C20 C5 122(2)

C7 C18 C19 66(2) C4 C20 C13 64(2)

C8 C18 C9 34(12) C5 C20 C13 59(2)

C8 C18 C17 42(9) C2 C21 C4 65(2)

C8 C18 C19 152(11) C2 C21 C9 69(2)

C9 C18 C17 57(.1) C2 C21 C13 8.1(9)

C9 C18 C19 144(2) C4 C21 C9 132(3)

C17 C18 C19 109(2) C4 C21 C13 71(2)

C3 C19 C7 55(1) C9 C21 C13 62(2)

C3 C19 C8 98(1) NIB' C32 C23 74(3)

C3 C19 C1I 61(2) NIB' C32 C30 101(1)

C3 C19 C12 11(1) NIB' C32 C31 118(2)

C3 C19 C18 100(2) NIB' C32 C34 013(2)

C7 C19 C8 54(1) NiB' C32 C35 108(1)

C7 C19 C1l 113(2) NIB' C32 C39 107(1)

C7 C19 C12 66(1) C23 C32 C30 74(3)

C7 C19 C18 57(1) C23 C32 C31 140(4)

C8 C19 C1l 157(2) C23 C32 C34 155(3)

C8 C19 C12 108(2) C23 C32 C35 47(3)

C8 C19 C18 2.6(9) C23 C32 C39 89(3)

C1l C19 C12 51(2) C30 C32 C31 132(2)

C1l C19 C18 158(2) C30 C32 C34 81(1)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 165 P- 65om j&6

165

Table S23. Intramolecular Bond Angles (0) Involving Nonhydrogen Atoms for [Rh2(dimen) 41-

[TFPB]2 (cont.). Estimated standard deviations in the last digit are given in parentheses.

atom atom atom angle atom atom atom angle

C12 C19 C18 109(2) C30 C32 C35 36(1)

C2 C20 C4 56(1) C30 C32 C39 143(2)

C2 C20 C5 68(2) C31 C32 C34 59(2)

C31 C32 C35 134(2) C31 C34 C32 46(1)

C31 C32 C39 51(2) C23 C35 C27 63(1)

C34 C32 C35 109(1) C23 C35 C30 86(2)

C34 C32 C39 109(1) C23 C35 C32 16(1)

C35 C32 C39 109(2) C23 C35 C36 94(1)

NIB C33 C22 75(3) C27 C35 C30 148(2)

NIB C33 C25 117(2) C27 C35 C32 74(1)

NiB C33 C29 107(1) C27 C35 C36 47.6(8)

NiB C33 C37 118(2) C30 C35 C32 75(2)

NiB C33 C40 112(2) C30 C35 C36 142(2)

NiB C33 C41 98(1) C32 C35 C36 109(1)

C22 C33 C25 131(4) C26 C36 C27 106(2)

C22 C33 C29 78(3) C26 C36 C35 176(3)

C22 C33 C37 144(3) C26 C36 C37 67(2)

C22 C33 C40 93(4) C27 C36 C35 70(1)

C22 C33 C41 35(3) C27 C36 C37 43(1)

C25 C33 C29 132(2) C35 C36 C37 109(1)

C25 C33 C37 75(1) C25 C37 C26 59(1)

C25 C33 C40 38(1) C25 C37 C27 132(1)

C25 C33 C41 138(2) C25 C37 C28 143(1)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 166

166

Table S23. Intramolecular Bond Angles (0) Involving Nonhydrogen Atoms for [Rh2(dimen) 4 1-

[TFPB] 2 (cont.). Estimated standard deviations in the last digit are given in parentheses.

atom atom atom angle atom atom atom angle

C29 C33 C37 66(1) C25 C37 C29 96(1)

C29 C33 C40 137(2) C25 C37 C33 42.9(9)

C29 C33 C41 45(1) C25 C37 C36 77(1)

C37 C33 C40 109(1) C25 C37 C38 149(1)

C37 C33 C41 109(1) C26 C37 C27 76(1)

C40 C33 C41 109(2) C26 C37 C28 125(2)

C26 C37 C29 143(1) C29 C38 C37 59.9(9)

C26 C37 C33 88(1) C29 C38 C39 141(1)

C26 C37 C36 22(1) C37 C38 C39 109(1)

C26 C37 C38 118(1) C23 C39 C27 54(1)

C27 C37 C28 75(1) C23 C39 C28 95(1)

C27 C37 C29 131(1) C23 C39 C31 64(2)

C27 C37 C33 156(2) C23 C39 C32 17(1)

C27 C37 C36 55(1) C23 C39 C38 93(1)

C27 C37 C38 65(1) C27 C39 C28 51.3(8)

C28 C37 C29 58(1) C27 C39 C31 114(2)

C28 C37 C33 101(1) C27 C39 C32 70(1)

C28 C37 C36 118(1) C27 C39 C38 51.7(9)

C28 C37 C38 10.1(9) C28 C39 C31 159(2)

C29 C37 C33 58(1) C28 C39 C32 112(1)

C29 C37 C36 162(1) C28 C39 C38 4.7(9)

C29 C37 C38 68(1) C31 C39 C32 47(1)

C33 C37 C36 109(1) C31 C39 C38 155(2)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 167,0, 1,1 -M~ 7 4

167

Table S23. Intramolecular Bond Angles (0) Involving Nonhydrogen Atoms for [Rh2(dimen)41-

[TFPB12 (cont.). Estimated standard deviations in the last digit are given in parentheses.

atom atom atom angle atom atom atom angle

C33 C37 C38 109(1) C32 C39 C38 109(1)

C36 C37 C38 109(1) C22 C40 C25 67(2)

C27 C38 C28 102(4) C22 C40 C33 16.7(9)

C27 C38 C29 100(1) C25 C40 C33 50(1)

C27 C38 C37 40.9(9) C22 C41 C24 71(2)

C27 C38 C39 72(1) C22 C41 C29 81(2)

C28 C38 C29 8(5) C22 C41 C33 13(1)

C28 C38 C37 61(3) C24 C41 C29 146(2)

C28 C38 C39 149(6) C24 C41 C33 81(2)

C29 C41 C33 68(1)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 168

168

Table S24. Uij Thermal Parameters for [Rh2(dimen)411[TFPB2 Estimated standard deviations in

the least significant figure.are given in parenthesis.

atom U 11 U2 2 U3 3 U 12 U1 3 U2 3

RH1 0.0649(9) 0.0668(8) 0.0625(6) -0.0225(6) 0.0012(5) -0.0017(5)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 169

169Table S25. Crystallographic Data and Collection Parameters for [Rh2(dimen) 4rB(C6H 5)412.

A. Crystal Data

Empirical Formula C96H1 12B 2N8Rh2

Formula Weight 1605.43

Crystal Color, Habit red, prism

Crystal Dimensions (mm) 0.41 x 0.33 x 0.30

Crystal System orthorhombic

Space Group Pbca (No. 61)

No. Reflections Used for Unit Cell 25

Determination (20 range) , -- (28 - 32')

Omega Scan Peak Width at Half-Height 0.00

Lattice Parameters (esd)

a, A 19.390(5)

b, A 29.492(7)

c, A 30.970(7)

v, A3 17710(7)

Z 8

Pcalc, g cm-3 1.204

F0 00 6752

P{Mo Koc), cm-1 4.125

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 170

170

Table S25. Crystallographic Data and Collection Parameters for [Rh2(dimen) 41[B(C 6H 5)412

(cont.).

B. Collection and Reduction of X-ray Diffraction Data

Diffractometer Enraf-Nonius CAD-4

X, A

T, oC

Attenuator

Take-off Angle, deg

Scan Type

Scan Rate, deg/min ,

2 0 max, deg

Total Reflections

Transmission Coeff., cm-1

C. Solution and Refinement of Structure

Technique of Solution

Refinement

Function Minimized

Least-squares Weights

p-factor

No. of Observations (I>3.00a(I))

No. of Variables

R

Goodness of Fit

Maximum Shift/Error in Final Cycle

Maximum Peak in Final Diff. Map

Minimum Peak in Final Diff. Map

0.7107 (graphite monochromated)

296

Cu foil, (factor = 17.8)

6.08

to

4 (in co)

40

16793 (7821 unique) (Rint = 0.0311)

0.98 - 1.02

Rh via Patterson; Fourier maps

Full-matrix least-squares

I co (Fo02 - Fc2)2.

1/y2 (F02)

0.02

5481

505

0.1034

0.080

2.74

0.56

1.21/eA-3

-1.10eA-3

1P- 5 0-M ) 7D

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 171

171

Table S26. Atomic Positional Parameters and Equivalent Isotropic Displacement Parameters

and Their Estimated Standard Deviations for [Rh2(dimen)41 [B(C 6H5)4 12.

atom

Rh1

Rh2

Cl

N1

C2

C3

C4

C5

C6

C7

C8

C9

C1o

C1l

N2

C12

C15

N3

C16

C17

C18

C19

C20

x

0.1210(4)

0.3101(4)

0.1410(5)

0.1524(4)

0.1662(6)

0.1021(8)

0.1736(7)

0.2360(7)

0.2957(6)

0.3662(7)

0.3581(7)

0.2965(8)

0.2260(6)

0.4189(8)

0.3424(4)

0.3270(5)

0.1402(5)

0.1496(4)

0.1665(6)

0.1001(6)

0.2031(6)

0.2675(6)

0.3163(6)

0.1190(3)

0.1588(2)

0.0790(3)

0.0521(3)

0.0189(4)

0.0197(5)

-0.0270(5)

0.0338(4)

0.0274(4)

0.0462(5)

0.0927(4)

0.0989(5)

0.0827(4)

0.1134(5)

0.1207(3)

0.1357(3)

0.0701(3)

0.0399(3)

-0.0014(4)

-0.0202(4)

-0.0337(4)

-0.0143(3)

0.0031(4)

z

0.1420(2)

0.1521(2)

0.1892(3)

0.2160(3)

0.2527(4)

0.2794(4)

0.2323(5)

0.2738(4)

0.2469(4)

0.2683(4)

0.2822(4)

0.3107(5)

0.2926(4)

0.3034(5)

0.2420(3)

0.2088(3)

0.1030(3)

0.0797(3)

0.0539(3)

0.0363(4)

0.0841(4)

0.1050(3)

0.0699(3)

B(eq)a

5.07(2)

4.57(2).

4.0(2)

5.2(2)

5.8(3)

13.85(59)

12.52(52)

8.0(3)

6.7(3)

9.3(4)

6.9(3)

10.7(4)

7.1(3)

16.26(60)

4.8(2)

4.1(2)

4.1(2)

4.7(2)

5.0(3)

9.64(42)

7.0(3)

5.5(3)

5.8(3)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 172

172

Table S26. Atomic Positional Parameters and Equivalent Isotropic Displacement Parameters

and Their Estimated Standard Deviations for [Rh2(dimen)41 [B(C 6H5 )4 12.

atom x z

C21

C22

C23

C24

C25

N4

C26

C31

N5

C32

C33

C34

C35

C36

C37

C38

C39

C40

C41

N6

C42

C45

N7

0.2835(5)

0.2153(6)

0.3808(6)

0.4183(8)

0.4314(6)

0.3580(4)

0.3395(5)

0.1001(5)

0.0860(5)

0.0819(9)

0.0463(12)

0.0348(10)

0.1551(8)

0.1987(6)

0.2733(8)

0.3066(7)

0.2601(8)

0.1868(7)

0.3802(8)

0.3068(4)

0.3058(5)

0.0898(6)

0.0679(5)

0.0342(4)

0.0146(4)

0.0256(4)

-0.0022(4)

0.0427(5)

0.0675(3)

0.1011(3)

0.1550(3)

0.1713(3)

0.1898(6)

0.1537(11)

0.2331(10)

0.2014(5)

0.1570(4)

0.1673(5)

0.2063(4)

0.2470(5)

0.2385(4)

0.2165(7)

0.1915(3)

0.1797(3)

0.1665(4)

0.1942(3)

0.0386(3)

0.0188(3)

0.0910(4)

0.1247(4)

0.0573(4)

0.1145(3)

0.1287(3)

0.0915(3)

0.0592(3)

0.0134(5)

-0.0094(6)

0.0182(8)

-0.0013(5)

-0.0021(3)

-0.0132(5)

0.0105(4)

0.0092(5)

0.0216(4)

-0.0011(5)

0.0575(3)

0.0936(3)

0.1787(4)

0.2017(3)

B(eg)a

5.4(3)

5.7(3).

5.8(3)

12.28(52)

11.28(50)

5.2(2)

4.5(2)

4.8(3)

6.2(2)

10.0(5)

21.18(123)

23.84(130)

6.6(4)

6.2(3)

7.0(4)

6.1(3)

7.2(4)

6.9(3)

12.90(79)

5.2(2)

4.6(2)

5.7(3)

7.4(3)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 173

173

Table S26. Atomic Positional Parameters and Equivalent Isotropic Displacement Parameters

and Their Estimated Standard Deviations for [Rh2(dimen)41[B(C 6 H5)412 (cont.).

xatom

C46

C47

C48

C50

C51

C52

C53

C54

C55

N8

C56

BI

CB1

CB2

CB3

CB4

CB5

CB6

CB7

CB8

CB9

CB10

CB11

0.0495(10)

-0.0150(7)

0.0662(8)

0.1878(9)

0.1682(7)

0.1025(9)

0.2528(6)

0.2697(13)

0.3123(9)

0.2725(4)

0.2854(5)

0.0568(6)

0.1323(5)

0.1941(6)

0.2587(6)

0.2621(6)

0.2047(6)

0.1397(5)

-0.0072(5)

-0.0480(5)

-0.1021(6)

-0.1167(6)

-0.0773(5)

0.2261(6)

0.2196(5)

0.2735(5)

0.2822(5)

0.2407(5)

0.2264(6)

0.2899(4)

0.3335(6)

0.2984(9)

0.2500(3)

0.2160(3)

0.3850(4)

0.3614(3)

0.3842(3)

0.3646(4)

0.3233(4)

0.2993(3)

0.3185(3)

0.3568(3)

0.3730(4)

0.3480(4)

0.3057(4)

0.2880(3)

z

0.2395(6)

0.2538(5)

0.2159(4)

0.2391(5)

0.2600(4)

0.2777(5)

0.2207(4)

0.1968(8)

0.2484(8)

0.1939(2)

0.1770(3)

0.3372(3)

0.3469(3)

0.3384(3)

0.3467(3)

0.3635(3)

0.3728(3)

0.3646(3)

0.3596(3)

0.3932(3)

0.4109(3)

0.3952(3)

0.3632(3)

B(eg)a

2.7(4)

13.22(55)

1.4(3)

2.5(4)

8.5(4)

3.1(4)

5.4(3)

23.15(102)

25.81(116)

4.6(2)

4.2(2)

3.5(3)

3.8(2)

5.2(2)

5.8(3)

5.8(3)

5.2(3)

4.2(2)

3.2(2)

5.2(3)

6.0(3)

5.3(3)

5.1(3)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 174

174

Table S26. Atomic Positional Parameters and Equivalent Isotropic Displacement Parameters

and Their Estimated Standard Deviations for [Rh2(dimen) 41[B(C6 H5)4] 2 (cont.).

atom x

CB12

CB13

CB14

CB15

CB16

CB17

CB18

CB19

CB20

CB21

CB22

CB23

CB24

B2

CB25

CB26

CB27

CB28

CB29

CB30

CB31

CB32

CB33

-0.0244(5)

0.0555(5)

0.0944(5)

0.0896(6)

0.0454(6)

0.0062(5)

0.0113(5)

0.0418(5)

-0.0234(5)

-0.0366(6)

0.0145(6)

0.0799(6)

0.0922(5)

0.1695(6)

0.1064(5)

0.0791(5)

0.0246(6)

-0.0002(6)

0.0271(6)

0.0814(6)

0.1697(5)

0.2176(5)

0.3132(3)

0.4368(3)

0.4506(3)

0.4953(4)

0.5252(4)

0.5130(3)

0.4695(3)

0.3879(3)

0.3828(3)

0.3883(4)

0.4001(3)

0.4058(4)

0.3999(3)

0.1081(4)

0.1302(3)

0.1088(3)

0.1274(4)

0.1691(4)

0.1924(4)

0.1733(4)

0.0530(3)

0.0318(3)

z

0.3458(3)

0.3560(3)

0.3915(3)

0.4088(3)

0.3914(3)

0.3571(4)

0.3398(3)

0.2845(3)

0.2668(3)

0.2229(4)

0.1954(3)

0.2103(4)

0.2544(3)

0.4460(3)

0.4164(3)

0.3814(3)

0.3565(3)

0.3677(3)

0.4010(4)

0.4249(4)

0.4372(3)

0.4098(3)

B(eq)a

4.7(2)

3.3(2).

5.0(3)

5.7(3)

5.3(3)

5.5(3)

4.8(2)

3.8(2)

4.8(2)

5.9(3)

5.4(3)

6.4(3)

5.0(3)

3.8(3)

3.7(2)

4.4(2)

5.6(3)

5.8(3)

6.5(3)

6.0(3)

3.6(2)

4.9(3)

5.6(3)0.2139(6) -0.0144(4) 0.3994(3)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 175

175

Table S26. Atomic Positional Parameters and Equivalent Isotropic Displacement Parameters

and Their Estimated Standard Deviations for [Rh2(dimen)41[B(C 6HS) 412 (cont.).

atom x y z B(eq)a

CB34 0.1608(6) -0.0402(4) 0.4144(3) 5.4(3)

CB35 0.1122(5) -0.0217(3) 0.4414(3) 4.9(2)

CB36 0.1197(5) 0.0245(3) 0.4520(3) 4.3(2)

CB37 0.1501(5) 0.1178(3) 0.4972(3) 4.3(2)

CB38 0.0824(6) 0.1147(4) 0.5122(4) 5.8(3)

CB39 0.0650(6) 0.1226(4) 0.5561(4) 7.6(3)

CB40 0.1172(7) '0.1339(4) 0.5836(4) 6.8(3)

CB41 0.1822(7) 0.1379(4) 0.5712(4) 6.6(3)

CB42 0.1995(5) 0.1302(3) 0.5281(3) 5.0(3)

CB43 0.2419(5) 0.1311(3) 0.4332(3) 4.1(2)

CB44 0.2501(6) 0.1693(3) 0.4070(3) 5.1(3)

CB45 0.3143(7) 0.1886(4) 0.3967(4) 6.8(3)

CB46 0.3731(7) 0.1706(4) 0.4136(4) 7.2(3)

CB47 0.3688(7) 0.1336(4) 0.4390(4) 7.1(3)

CB48 0.3055(6) 0.1139(4) 0.4489(3) 5.8(3)

33a B(eq) =(87 2/3) Uijai*aj*A 1 where Aij is the dot product of the ith and jth direct space

i=1 j=1

unit cell vectors.

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 176

176

Table S27. Calculated Atomic Positional Parameters and Equivalent Isotropic Displacement

Parameters for [Rh2(dimenl) 41[B(C 6H5)4 12.a

atom x Y z B(eq)b

C33A 0.0069 0.1885 -0.0014 7.3(22)

C35A 0.1102 0.2378 0.0130 9.0(19)

C35B 0.1263 0.1588 -0.0157 7.1(15)

C37A 0.2319 0.2047 -0.0065 4.2(12)

C41A 0.3350 0.2544 0.0073 6.5(16)

C41B 0.3517 0.1734 -0.0158 7.0(16)

C49 0.1398 0.2835 0.1962 3.7

C46A 0.0293 0.2432 0.2126 6.6

C47A -0.0271 0.2601 0.1820 10.0

C48A 0.1955 0.3068 0.1888 9.0

C49A 0.1289 0.2805 0.2108 10.0

C50A 0.1016 0.2526 0.2383 10.0

C52A 0.2157 0.2731 0.2659 9.0

H3A 0.0980 0.0490 0.2926 11.3

H3B 0.0636 0.0139 0.2621 11.3

H3C 0.1057 -0.0025 0.3017 11.3

H4A 0.2149 -0.0280 0.2149 11.3

H4B 0.1774 -0.0498 0.2540 11.3

H4C 0.1353 -0.0334 0.2144 11.3

H5 0.2469 0.0149 0.2977 8.9

H6A 0.2879 0.0424 0.2204 8.2

H6B 0.3003 -0.0044 0.2419 8.2

H7A 0.4008 0.0444 0.2474 10.7

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 177P-50 Ifn!/77

177

Table S27. Calculated Atomic Positional Parameters and Equivalent Isotropic Displacement

Parameters for [Rh 2 (dimen)4[B(C6H5 )412.a

atom x y z B(eq)b

H7B 0.3764 0.0276 0.2923 10.7

H9A 0.2904 0.1303 0.3172 10.7

H9B 0.3029 0.0827 0.3370 10.7

H10A 0.1925 0.0820 0.3150 8.2

HIOB 0.2115 0.1026 0.2704 8.2

H11A 0.4279 0.0981 0.3300 11.3

H11B 0.4558 0.1144 0.2857 11.3

H11C 0.4058 0.1449 0.3118 11.3

H17A 0.1108 -0.0465 0.0197 11.3

H17B 0.0714 -0.0280 0.0596 11.3

H17C 0.0793 0.0018 0.0186 11.3

H18A 0.2156 -0.0602 0.0688 10.7

H18B 0.1718 -0.0417 0.1069 10.7

H19A 0.2903 -0.0373 0.1214 8.2

H19B 0.2556 0.0100 0.1237 8.2

H20 0.3307 -0.0225 0.0535 8.9

H21A 0.3146 0.0401 0.0156 8.2

H21B 0.2726 0.0619 0.0529 8.2

H22A 0.2264 -0.0105 0.0009 10.7

H22B 0.1931 0.0373 0.0024 10.7

H24A 0.3856 -0.0126 0.1459 11.3

H24B 0.4403 -0.0270 0.1120 11.3

H24C 0.4512 0.0167 0.1391 11.3

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 178

178

Table S27. Calculated Atomic Positional Parameters and Equivalent Isotropic Displacement

Parameters for [Rh2(dimei)41[B(C 6H5)4 12 (cont.).a

atom x y z B(eg)b

H25A 0.4069 0.0598 0.0366 11.3

H25B 0.4643 0.0615 0.0714 11.3

H25C 0.4534 0.0178 0.0443 11.3

H33A 0.0757 0.1278 -0.0110 11.3

H33B 0.0057 0.1459 0.0060 11.3

H33C 0.0353 0.1639 -0.0372 11.3

H34A 0.0619 0.2557 0.0336 11.3

H34B 0.0251 0.2444 -0.0096 11.3

H34C -0.0045 0.2264 0.0337 11.3

H33D 0.0044 0.1994 -0.0302 11.3

H33E -0.0105 0.1584 -0.0003 11.3

H33F -0.0198 0.2074 0.0170 11.3

H35 0.1518 0.2135 -0.0297 8.9.

H35A 0.0875 0.2551 0.0347 10.7

H35B 0.1015 0.2509 -0.0145 10.7

H35C 0.1243 0.1705 -0.0442 10.7

H35D 0.1080 0.1289 -0.0153 10.7

H36A 0.1803 0.1368 -0.0231 8.2

H36B 0.1969 0.1429 0.0255 8.2

H36C 0.2230 0.1360 -0.0199 8.2

H36D 0.2013 0.1472 0.0271 8.2

H37A 0.2760 0.1733 -0.0433 10.7

H37B 0.2999 0.1403 -0.0073 10.7

P1D-fnoill

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 179

179

Table S27. Calculated Atomic Positional Parameters and Equivalent Isotropic Displacement

Parameters for [Rh2(dimeti) 4 1[B(C 6H5 )412 (cont.).

atom x Y z B(eq)b

H37C 0.2333 0.2130 -0.0361 8.9

H39A 0.2598 0.2593 -0.0191 10.7

H39B 0.2773 0.2693 0.0289 10.7

H40A 0.1605 0.2649 0.0160 8.2

H40B 0.1853 0.2315 0.0515 8.2

H40C 0.2028 0.2681 0.0163 8.2

H40D 0.1935 0.2307 0.0510 8.2

H41A 0.3820 0.2251 -0.0303 11.3

H41B 0.3964 0.2394 0.0171 11.3

H41C 0.4067 0.1894 0.0031 11.3

H41D 0.3067 0.2743 0.0236 11.3

H41E 0.3807 0.2552 0.0182 11.3

H41F 0.3351 0.2638 -0.0221 11.3

H41G 0.3338 0.1435 -0.0136 11.3

H41H 0.3518 0.1826 -0.0452 11.3

H411 0.3974 0.1740 -0.0048 11.3

H47A -0.0408 0.2439 0.2664 11.5

H47B -0.0439 0.1983 0.2416 11.5

H47C 0.0149 0.2071 0.2745 11.5

H47D -0.0456 0.2879 0.1923 11.5

H47E -0.0071 0.2646 0.1544 11.5

H47F -0.0630 0.2383 0.1799 11.5

H48A 0.0926 0.2669 0.2458 9.5

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 180

180

Table S27. Calculated Atomic Positional Parameters and Equivalent Isotropic Displacement

Parameters for [Rh2(dimei) 4 ][B(C 6HS)4 12 (cont.).

atom x Y z B(eq)b

H48B 0.0435 0.2978 0.2193 9.5

H48C 0.1904 0.3388 0.1895 9.5

H48D 0.2035 0.2972 0.1599 9.5

H49A 0.1242 0.3129 0.1770 7.0

H49B 0.1394 0.2621 0.1685 7.0

H49C 0.1027 0.3065 0.2182 7.0

H49D 0.1107 0.2673 0.1853 7.0

H50 0.1844 0.3048 0.2607 7.9

H50A 0.0608 0.2645 0.2510 7.9

H51A 0.1996 0.2384 0.2850 7.0

H51B 0.1842 0.2165 0.2405 7.0

H51C 0.1926 0.2173 0.2427 7.0

H51D 0.1608 0.2272 0.2877 7.0

H52A 0.0874 0.2455 0.2991 9.5

H52B 0.0987 0.1962 0.2831 9.5

H52C 0.2502 0.2632 0.2855 9.5

H52D 0.1919 0.2983 0.2778 9.5

H54A 0.2324 0.3353 0.1735 11.5

H54B 0.2624 0.3580 0.2146 11.5

H54C 0.3107 0.3321 0.1833 11.5

H55A 0.3174 0.2759 0.2693 11.5

H55B 0.3532 0.3016 0.2317 11.5

H55C 0.3049 0.3275 0.2631 11.5

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 181

181

Table S27. Calculated Atomic Positional Parameters and Equivalent Isotropic Displacement

Parameters for [Rh2(dimen)4 ][B(C6H5 )4 12 (cont.).

atom x y z B(eq)b

HB2 0.1926 0.4140 0.3258 5.8.

HB3 0.2995 0.3811 0.3411 6.7

HB4 0.3065 0.3107 0.3689 6.7

HB5 0.2087 0.2694 0.3845 6.7

HB6 0.0995 0.3014 0.3713 5.8

HB8 -0.0389 0.4026 0.4040 5.8

HB9 -0.1301 0.3604 0.4332 6.7

HB10 -0.1534 0.2887 0.4070 6.7

HB11 -0.0861 0.2586 0.3528 6.7

HB 12 0.0020 0.3005 0.3230 5.8

HB14 0.1257 0.4297 0.4040 5.8

HB15 0.1171 0.5036 0.4326 6.7

HB16 0.0416 0.5547 0.4030 6.7

HB17 -0.0259 0.5334 0.3450 6.7

HB18 -0.0165 0.4622 0.3150 5.8

HB20 -0.0610 0.3758 0.2858 5.8

HB21 -0.0815 0.3821 0.2124 6.7

HB22 0.0037 0.4042 0.1657 6.7

HB23 0.1156 0.4134 0.1916 6.7

HB24 0.1370 0.4049 0.2650 5.8

HB26 0.0964 0.0797 0.3736 5.8

HB27 0.0070 0.1108 0.3318 6.7

HB28 -0.0364 0.1816 0.3513 6.7

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 182

182

Table S27. Calculated Atomic Positional Parameters and Equivalent Isotropic Displacement

Parameters for [Rh2(dimen) 4 11B(C 6HS) 412 (cont.).

atom x Y z B(eq)b

HB29 0.0097 0.2217 0.4079 6.7

HB30 0.1005 0.1901 0.4483 5.8

HB32 0.2537 0.0494 0.3979 5.8

HB33 0.2482 -0.0279 0.3816 6.7

HB34 0.1576 -0.0710 0.4060 6.7

HB35 0.0754 -0.0399 0.4523 6.7

HB36 0.0870 0.0367 0.4718 5.8

HB38 0.0471 0.1063 0.4927 5.8

HB39 0.0185 0.1209 0.5657 6.7

HB40 0.1059 0.1396 0.6131 6.7

HB41 0.2173 0.1460 0.5916 6.7

HB42 0.2461 0.1327 0.5193 5.8

HB44 0.2109 0.1828 0.3947 5.8

HB45 0.3175 0.2141 0.3782 6.7

HB46 0.4168 0.1839 0.4081 6.7

HB47 0.4103 0.1209 0.4499 6.7

HB48 0.3062 0.0882 0.4678 5.8

a Heavy atoms without esd's for positional parameters are placed as per the dimen ligand disorder

model. See the Supplementary Materials paragraph for further detail.

33b B(eq) = (87r 2/3) Uijai*a/*Aj where AUj is the dot product of the ith and jth direct spacei=lj=1

unit cell vectors.

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 183

183

Table S28. Bond Distances (A) for [Rh 2(dimen)4 1[B(C 6H 5)412. Estimated standard

deviations in the least significant figure are given in parentheses.

atom atom distance atom atom distance

Rh1 Rh2 3.862(1) C2 C4 1.500(18)

C23 N4 1.501(14) C36 C37 1.518(18)

Rh1 C1 1.919(9) C2 C5 1.566(18)

N4 C26 1.143(13) C36 C35B 1.466

Rh1 C15 1.917(9) C5 C6 1.439(17)

C31 N5 1.143(14) C36 C37A 1.554

Rh1 C31 1.932(jO) C5 C10 1.569(17)

N5 C32 1.52(2) C37 C38 1.509(19)

Rh1 C45 1.902(11) C6 C7 1.617(18)

C32 C33 1.45(3) C38 C39 1.502(19)

Rh2 C12 1.913(9) C7 C8 1.445(19)

C32 C34 1.58(3) C38 C41 1.50(2)

Rh2 C26 1.936(10) C8 C9 1.497(19)

C32 C35 1.53(2) C38 N6 1.520(14)

Rh2 C42 1.914(10) C8 C11 1.481(19)

C32 C33A 1.524 C38 C37A 1.540

Rh2 C56 1.913(9) C8 N2 1.526(15)

C32 C35A 1.519 C38 C41A 1.527

C1 NI 1.170(12) C9 C10 1.552(19)

C32 C35B 1.546 C38 C41B 1.538

N1 C2 1.523(15) N2 C12 1.157(12)

C35 C36 1.559(18) C39 C40 1.494(19)

C2 C3 1.494(19) C15 N3 1.163(12)

C35 C40 1.443(19) C40 C35A 1.509

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 184 P / i

184

Table S28. Bond Distances (A) for [Rh2(dimen) 4][B(C 6H5)4 12. Estimated standard

deviations in the least significant figure are given in parentheses (cont.).

atom atom distance atom atom distance

N3 C16 1.492(13) C50 C53 1.40(2)

C40 C37A 1.587 CB17 CB18 1.395(14)

C16 C17 1.503(16) C51 C52 1.45(2)

N6 C42 1.173(13) CB19 CB20 1.385(13)

C16 C18 1.513(16) C51 C50A 1.498

C45 N7 1.164(15) CB19 CB24 1.396(14)

C16 C22 1.514(15) C51 C52A 1.338

N7 C46 1.54(2) CB20 CB21 1.395(15)

C18 C19 1.519(16) C53 C54 1.52(3)

N7 C46A 1.663 CB21 CB22 1.350(15)

C19 C20 1.527(15) C53 C55 1.46(3)

C46 C47 1.34(2) CB22 CB23 1.360(16)

C20 C21 1.480(15) C53 N8 1.489(14)

C46 C48 1.61(2) CB23 CB24 1.396(15)

C20 C23 1.560(16) C53 C48A 1.569

C46 C52 1.57(2) B2 CB25 1.662(14)

C21 C22 1.567(15) C53 C52A 1.649

C47 C46A 1.689 B2 CB31 1.647(14)

C23 C24 1.511(18) N8 C56 1.160(12)

C48 C49 1.579 B2 CB37 1.653(14)

C23 C25 1.520(17) C46A C47A 1.530

C49 C50 1.623 B2 CB43 1.610(14)

C50 C51 1.43(2) C46A C50A 1.636

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 185

185

Table S28. Bond Distances (A) for [Rh2(dimen) 4 1[B(C 6 H5 )4 12. Estimated standard

deviations in the least significant figure are given in parentheses (cont.).

atom atom distance atom atom distance

CB16 CB17 1.355(15) CB25 CB26 1.361(13)

C48A C49A 1.655 CB37 CB38 1.395(14)

CB25 CB30 1.387(14) CB7 CB8 1.392(13)

C49A C50A 1.295 CB37 CB42 1.403(14)

CB26 CB27 1.417(14) CB7 CB12 1.395(13)

B1 CB1 1.649(14) CB38 CB39 1.421(17)

CB27 CB28 1.367(15) CB8 CB9 1.396(15)

BI CB7 1.647(14) CB39 CB40 1.364(17)

CB28 CB29 1.348(16) CB9 CB10 1.369(15)

B1 CB13 1.636(14) CB40 CB41 1.323(17)

CB29 CB30 1.405(16) CB10 CB11 1.354(14)

B1 CB19 1.662(14) CB41 CB42 1.396(15)

CB31 CB32 1.405(13) CB11 CB12 1.377(14)

CB1 CB2 1.398(14) CB43 CB44 1.399(14)

CB31 CB36 1.364(13) CB13 CB14 1.395(13)

CB1 CB6 1.385(13) CB43 CB48 1.419(14)

CB32 CB33 1.401(15) CB13 CB18 1.383(13)

CB2 CB3 1.404(15) CB44 CB45 1.405(16)

CB33 CB34 1.363(15) CB14 CB15 1.425(15)

CB3 CB4 1.325(15) CB45 CB46 1.362(17)

CB34 CB35 1.373(15) CB15 CB16 1.345(15)

CB4 CB5 1.352(15) CB46 CB47 1.346(17)

CB35 CB36 1.410(14) CB47 CB48 1.392(16)

CB5 CB6 1.406(14)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 186

186

Table S29. Intramolecular Bond Angles (0) Involving Nonhydrogen Atoms for [Rh2(dimen) 41-

[B(C 6H5)4 12. Estimated standard deviations in the last digit are given in parentheses.

atom

Rh1

Rh1

Rh1

Rh1

C1

C1

C1

C15

C15

C31

Rh2

Rh2

Rh2

Rh2

C12

C12

C12

C26

C26

C42

C2

C3

C4

atom

Cl

C15

C31

C45

Rh1

Rh1

Rh1

Rh1

Rh1

Rh1

C12

C26

C42

C56

Rh2

Rh2

Rh2

Rh2

Rh2

Rh2

N1

C2

C2

atom

N1

N3

N5

N7

Cis

C31

C45

C31

C45

C45

N2

N4

N6

N8

C26

C42

C56

C42

C56

C56

C1

N1

N1

angle

175.1(8)

177.6(8)

171.7(9)

176.6(10)

88.8(4)

175.3(4)

93.5(4)

86.8(4)

172.5(4)

90.7(4)

174.6(8)

178.6(9)

176.3(9)

176.4(8)

88.8(4).

172.2(4)

89.3(4)

86.6(4)

177.0(4)

95.0(4)

177.0(10)

104.8(10)

106.4(10)

atom

C5

C4

C5

C5

C6

C1O

C1O

C7

C8

C9

C1l

N2

Cli

C35

N2

C35

N2

C35A

C1O

C35B

C9

C35B

C12

atom

C2

C2

C2

C2

C5

CS

C5

C6

C7

C8

C8

C8

C8

C32

C8

C32

C8

C32

C9

C32

C1O

C32

N2

atom

NI

C3

C3

C4

C2

C2

C6

C5

C6

C7

C7

C7

C9

C33

C9

C34

C1l

C33A

C8

C33A

C5

C35A

C8

angle

106.4(9)

109.1(11)

118.9(11)

110.3(10)

114.7(11)

107.9(10)

115.8(10)

113.5(10)

110.9(11)

112.2(11)

115.9(11)

107.0(10)

108.9(11)

117.5(16)

104.8(10)

112.6(15)

107.3(10)

111.5

116.9(11)

110.0

107.9(10)

110.3

169.3(9)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 187

P-500-M) 7187

Table S29. Intramolecular Bond Angles (0) Involving Nonhydrogen Atoms for [Rh2(dimen) 4 1-

[B(C 6H5)412 . Estimated standard deviations in the last digit are given in parentheses (cont.).

atom atom atom angle atom atom atom angle

C35B C33 C33A 121.8 C23 C20 C21 110.8(9)

C16 N3 C15 173.3(9) C41 C38 C39 113.8(11)

C35A C34 C33A 112.6 C22 C21 C20 112.9(9)

C17 C16 N3 107.8(9) N6 C38 C39 104.8(10)

C36 C35 C32 108.7(12) C21 C22 C16 111.3(8)

C18 C16 N3 106.6(8) N6 C38 C41 106.4(10)

C40 C35 C32 114.8(13) C24 C23 C20 116.4(10)

C22 C16 N3 105.6(8) C37A C38 N6 108.7

C40 C35 C36 114.5(11) C25 C23 C20 111.8(10)

C18 C16 C17 113.2(9) C41A C38 N6 109.1

C37 C36 C35 110.7(10) N4 C23 C20 108.5(9)

C22 C16 C17 112.9(9) C41B C38 N6 108.9

C37A C36 C35B 109.8 C25 C23 C24 110.0(10)

C22 C16 C18 110.3(9) C41A C38 C37A 110.2

C38 C37 C36 116.7(11) N4 C23 C24 104.8(9)

C19 C18 C16 114.3(9) C41B C38 C37A 109.6

C41B C37 C37A 119.3 N4 C23 C25 104.4(9)

C20 C19 C18 109.4(9) C41B C38 C41A 110.3

C39 C38 C37 110.0(11) C26 N4 C23 173.7(10)

C21 C20 C19 114.1(9) C40 C39 C38 115.4(12)

C41 C38 C37 116.3(11) C32 N5 C31 168.1(11)

C23 C20 C19 109.9(9) C41A C39 C37A 119.2

C37 104.4(9) C33 C32N6 C38 N5 102.5(15)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 188

p 550 -InY)I

188

Table S29. Intramolecular Bond Angles (0) Involving Nonhydrogen Atoms for [Rh2(dimen) 4 1-

[B(C6H5) 412. Estimated standard deviations in the last digit are given in parentheses (cont.).

atom atom atom angle atom atom atom angle

C39 C40 C35 114.0(11) C48 C46 N7 97.9(12)

C34 C32 N5 103.4(14) C53 C52A C51 113.6

C37A C40 C35A 115.9 C52 C46 N7 115.1(13)

C35 C32 N5 108.0(12) CB7 B1 CB1 112.3(8)

C41B C41 C41A 119.9 C48 C46 C47 117.5(14)

C33A C32 N5 108.6 CB13 B1 CB1 110.1(7)

C42 N6 C38 178.8(10) C52 C46 C47 111.3(14)

C35A C32 N5 108.7 CB19 B1 CB1 110.9(8)

C40 C35A C32 111.6 C50A C46 C47 146.5

C35B C32 N5 107.6 CB13 BI CB7 108.2(7)

C36 C35B C32 112.8 C52 C46 C48 101.9(13)

C34 C32 C33 111.4(17) CB19 B1 CB7 107.9(7)

C38 C37A C36 112.7 C49 C48 C46 121.3

C40 C37A C36 107.0 CB19 B1 CB13 107.3(7)

C49A C48A C53 98.3 C50 C49 C48 101.4

C40 C37A C38 108.2 CB2 CB1 B1 121.5(8)

C50A C49A C48A 152.5 C51 C50 C49 103.8

C46 N7 C45 167.4(12) CB6 CB1 B1 123.2(8)

C46A C50A C51 156.7 C53 C50 C49 100.3

C46A N7 C45 154.0 CB6 CB1 CB2 115.2(8)

C49A C50A C51 95.2 C53 C50 C51 124.0(14)

C47 C46 N7 112.4(14) CB3 CB2 CB1 122.1(9)

C46A 97.9 C52 C51C49A C50A C50 130.7(13)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 189

189

Table S29. Intramolecular Bond Angles (0) Involving Nonhydrogen Atoms for [Rh2(dimen) 41-

[B(C 6 H5)4 12. Estimated standard deviations in the last digit are given in parentheses (cont.).

atom atom atom angle atom atom atom angle

CB4 CB3 CB2 119.7(10) C56 N8 C53 172.3(9)

C52A C51 C50A 119.2 CB14 CB13 B1 122..9(8)

CBS CB4 CB3 121.6(10) C47 C46A N7 91.4

C51 C52 C46 107.0(13) CB18 CB13 B1 122.2(8)

CB6 CBS CB4 119.3(10) C47A C46A N7 118.6

C54 C53 C50 121.9(13) CB18 CB13 CB14 114.7(8)

CB5 CB6 CB1 122.1(9) C50A C46A N7 82.0

C55 C53 C50 120.0(14) CB 15 CB 14 CB13 122.2(9)

CB8 CB7 B1 124.7(8) C47A C46A C47 103.8

N8 C53 C50 109.2(10) CB16 CB15 CB14 119.8(10)

CB12 CB7 B1 121.1(8) C50A C46A C47 97.9

C55 C53 C54 88.3(14) CB17 CB16 CB15 119.8(10)

CB12 CB7 CB8 114.2(8) C50A C46A C47A 149.2

N8 C53 C54 110.0(11) CB18 CB17 CB16 120.5(10)

CB9 CB8 CB7 122.6(9) CB17 CB18 CB13 123.1(9)

N8 C53 C55 105.1(12) CB40 CB39 CB38 117.4(11)

CB1O CB9 CB8 119.9(10) CB20 CB19 B1 122.8(8)

C48A C53 N8 94.7 CB41 CB40 CB39 123.3(12)

CB11 CB1O CB9 119.6(10) CB24 CB19 B1 123.2(8)

C52A C53 N8 110.3 CB42 CB41 CB40 119.4(11)

CB12 CB11 CB10 119.9(9) CB24 CB19 CB20 113.8(9)

C52A C53 C48A 108.7 CB41 CB42 CB37 122.1(9)

CB7 123.8(9) CB21 CB20CB11 CB12 CBl19 122.7(9)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 190

190

Table S29. Intramolecular Bond Angles (o) Involving Nonhydrogen Atoms for [Rh2(dimen) 41-

[B(C 6H 5)4] 2. Estimated standard deviations in the last digit are given in parentheses (cont.).

atom atom atom angle atom atom atom

CB44 CB43 B2 125.6(9) CB30 CB25 B2

CB22 CB21 CB20 120.7(10) CB30 CB25 CB26

CB48 CB43 B2 121.5(9) CB27 CB26 CB25

CB23 CB22 CB21 120.1(10) CB28 CB27 CB26

CB48 CB43 CB44 112.9(9) CB29 CB28 CB27

CB24 CB23 CB22 118.4(10) CB30 CB29 CB28

CB45 CB44 CB43 123.9(10) CB29 CB30 CB25

CB23 CB24 CB19 124.4(9) CB32 CB31 B2

CB46 CB45 CB44 119.8(11) CB36 CB31 B2

CB31 B2 CB25 107.3(8) CB36 CB31 CB32

CB47 CB46 CB45 119.2(12) CB33 CB32 CB31

CB37 B2 CB25 107.1(8) CB34 CB33 CB32

CB48 CB47 CB46 121.5(11) CB35 CB34 CB33

CB43 B2 CB25 110.0(8) CB36 CB35 CB34

CB47 CB48 CB43 122.7(10) CB35 CB36 CB31

CB37 B2 CB31 109.2(8) CB38 CB37 B2

CB43 B2 CB31 111.8(8) CB42 CB37 B2

CB43 B2 CB37 111.3(8) CB42 CB37 CB38

CB26 CB25 B2 123.0(8) CB39 CB38 CB37

angle

120.7(8)

116.1(9)

123.0(9)

118.2(10)

121.0(10)

119.6(10)

121.9(10)

122.8(8)

123.4(8)

113.4(8)

122.7(9)

120.2(10)

120.3(10)

117.2(9)

126.2(9)

121.4(9)

122.9(8)

115.6(9)

122.2(10)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 191

191

Table S30. Uj Thermal Parameters for [Rh2 (dimen)41[B(C 6H5)412 . Estimated standard

deviations in the least significant figure are given in parenthesis.

atom

Rh1

Rh2

C3

C4

C1l

C17

C24

C25

C33

C34

C41

C47

C54

C55

U11

0.0661(7)

0.0549(6)

0.1782(165)

0.1415(143)

0.1858(163)

0.0837(104)

0.1854(154)

0.0739(104)

0.1887(242)

0.0942(176)

0.0657(130)

0.0918(119)

0.2965(294)

0.0919(143)

U22

0.0415(5)

0.0418(5)

0.1549(144)

0.1062(116)

0.1533(140)

0.1042(103)

0.0791(97)

0.1444(129)

0.3658(409)

0.3350(370)

0.2468(231)

0.1562(134)

0.1181(156)

0.4036(339)

U3 3

0.0444(5)

0.0404(5)

0.0825(103)

0.1279(123)

0.1487(135)

0.1012(101)

0.1038(110)

0.1202(116)

0.0808(152)

0.2861(299)

0.0744(116)

0.1486(131)

0.2799(263)

0.2789(249)

U12

0.0040(5)

0.0044(5)

0.0174(122)

0.0067(103)

-0.0957(126)

-0.0209(83)

0.0488(99)

0.0054(91)

-0.1048(295)

0.0890(215)

-0.0412(146)

-0.0198(102)

-0.0341(167)

-0.0199(182)

U1 3

0.0132(5)

0.0031(5)

0.0136(105)

-0.0230(105)

-0.1183(124)

0.0228(80)

-0.0266(101)

0.0016(91)

0.0196(152)

0.0566(183)

0.0232(99)

0.0649(99)

0.0877(235)

0.0144(158)

U23

-0.0046(4)

-0.0009(4)

0.0228(98)

0.0193(97)

0.0728(113)

-0.0295(82)

-0.0198(83)

-0.0471(100)

0.0759(206)

0.2227(288)

0.0275(129)

-0.0831(109)

-0.0579(171)

-0,2702(259)

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 192

C20C19 C17

(a)

C14

N2A

C40 C35C36 C32 C2A

1&VC34 /N3 C3

N3A C3A

C38CIA

C21

C16

N2

C50C2

C46

C4

C1

N1C41

C26

N4

C4A N4A /C44

C49

C24

C29

C30

C31

ORTEP diagrams of Ir2(dimen)42+ cations (viewed down the Ir-Ir axis) from (a)

[Ir2(dimen)4](PF6)2 and (b) [Ir2(dimen)4][B(C 6H5 )412 crystal structures. The dihedral

twist angle reported in the text and in Figure 1 is the average of the C1A-Irl-Ir2-C2A, CIB-

Irl-Ir2-C2B, CIC-Irl-Ir2-C2C, and C1D-Irl-Ir2-C2D angles.

(01996 American Chemical Society Inorganic Chemistry V35 Page 549 Exstrom Supplemental Page 193

C50

C36

I ~A

C34- C38

C40

C37C39

C41

P-tso-rnic

C21 C17 C15 C20

(b) C14

C19 C16C13

C18 C12N1A

N2AC30

C49 C2A CIA

C4446 C

C1C C2C C1C24C45 C28

N1Cr N2C C25