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Homogeneous <stron
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I. General Considerations. All air-
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characteristics that matched the pu
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Figure S3. 1 H NMR timecourse. Reac
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Reaction of [1-Ph 2][BF 4] with [HP
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NMR Scale Reaction of [1-Ph 2][BF 4
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Synthesis of mer,trans-(PPh 3) 2Re(
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III. Synthesis of Complexes with Pe
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Figure S13. 31 P{ 1 H} NMR. Figure
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vessel was sealed and heated to 120
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Figure S18. 13 C{ 1 H} NMR. Figure
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Figure S20. 1 H NMR. Figure S21. 31
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Synthesis of mer,trans-(Ph 2PCHCH 2
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Figure S26. 13 C{ 1 H} NMR. Synthes
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Figure S29. 13 C{ 1 H} NMR. Synthes
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Figure S31. 31 P{ 1 H} NMR. Figure
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NMR (CD 2Cl 2, 125 MHz): δ 35.88 (
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Synthesis of trans-[(Ph 2PCH 2CHCH
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Figure S39. 13 C{ 1 H} NMR (with re
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Figure S41. 31 P{ 1 H} NMR. Figure
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Figure S43. 1 H NMR. Figure S44. 31
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Synthesis of [(Ph 2P(CH 2) 2B(C 8H
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Figure S49. 19 F NMR. Figure S50. 1
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= 10.2, 16.4, 2H, Ph 2PCH 2CH 2B(C
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Figure S55. 11 B{ 1 H} NMR (broad u
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Figure S57. 31 P{ 1 H} NMR. Figure
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(C 6D 5Cl, 300 MHz): δ 1.08 (br m,
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Figure S63. 11 B{ 1 H} NMR (broad u
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Figure S64. 1 H NMR. Figure S65. 31
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Figure S67. 1 H NMR (formyl region)
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environments could be B-O bond brea
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Figure S69. 1 H NMR (
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Figure S73. 1 H- 1 H gCO</s
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Reaction of 2-M 2 with pyridine. A
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€ B. Pulsed Gradient Spin-Echo Di
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epeated. If 2-E 2 were strictly mon
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Figure S80. 31 P{ 1 H} NMR. Thermol
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Figure S81. 1 H NMR of in-situ gene
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Figure S85. 13 C{ 1 H} NMR. Figure
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Figure S89. 1 H- 13 C gHMBC. Reacti
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location as [1-E 2][BF 4]. Thus we
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D. Mechanism Studies on the Reducti
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emoved from the cold bath and allow
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Figure S95. 31 P{ 1 H} NMR. Figure
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Figure S98. 1 H NMR (20 °C), hydri
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of H 2), with the other P-containin
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was apparent. Attempts to isolate a
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Figure S105. 13 C{ 1 H} NMR. Figure
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Reaction of [1-E 2-Mn][BF 4] with 2
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(br), 20.3, 24.7, 26.4, 28.7 (br),
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Figure S114. 31 P{ 1 H} NMR. Figure
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Figure S116. 1 H NMR. Figure S117.
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Figure S119. 31 P{ 1 H} NMR. Reacti
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and instead a mixture of 2-M 2, unr
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(0.0264 mmol) solid [1-E 2][BF 4],
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Figure S124. 31 P{ 1 H} NMR. Reacti
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of ~2:1 formyl:hydride, which conve
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Figure S127. 31 P{ 1 H} NMR. Figure
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Decomposition of 2-M 1. While searc
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Figure S133. 1 H{ 31 P} NMR. Figure
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Reaction of [1-M 1][BAr F 4] with [
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Figure S138. 31 P{ 1 H} NMR. Figure
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Figure S140. 1 H NMR time course. B
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the only Re species, but after 2.5
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Figure S143. 1 H NMR. Figure S144.
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Figure S147. 1 H- 1 H gCO</
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Figure S151. Reaction time course (
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one broad doublet), 188.27 (d, J PC
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Low temperature monitoring of the r
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D. Reductions of trans-[(PPh 3)(Ph
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Figure S159. 1 H NMR (with some res
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Figure S163. 1 H- 1 H gCO</
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Reaction of [Na][(PPh 3)(Ph 2P(CH 2
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Figure S168. 13 C{ 1 H} NMR. E. Red
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Figure S170. 31 P{ 1 H} NMR (initia
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VII. Crystallographic Details. Tabl
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Table 1 (cont.) Structure solution
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S155
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S157
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S159
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S161
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S163
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C(17A) 7415(2) 3268(1) 5199(1) 15(1
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C(20B) 5314(2) 1139(1) 8060(1) 20(1
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Table 3. Selected bond lengths [Å]
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C(38A)-C(39A) 1.381(4) C(39A)-C(40A
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O(4A)-C(4A)-Re(1) 122.6(2) C(6A)-C(
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C(28B)-C(23B)-P(2B) 121.5(2) C(25B)
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Table 5. Anisotropic displacement p
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C(46A) 430(20) 201(18) 420(20) -37(
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C(52C) 620(30) 500(30) 620(30) 30(2
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Completeness to θ = 36.56° 86.5 %
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Refinement of F 2 against ALL refle
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S187
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S189
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S191
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S193
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S195
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B(1) 1715(2) 6994(1) 4782(1) 20(1)
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F(17) 4266(1) 11296(1) 3213(1) 32(1
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Table 3. Selected bond lengths [Å]
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C(39A)-C(40A) 1.535(3) C(39A)-C(46A
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C(14)-C(15)-C(16) 119.7(2) C(15)-C(
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F(15)-C(68)-C(67) 115.0(2) C(63)-C(
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Table 5. Anisotropic displacement p
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C(44B) 1370(60) 630(40) 580(30) 20(
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Table 1. Crystal data and structure
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Table 1 (cont.) Structure solution
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S217
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S219
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S221
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S223
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S225
- Page 227 and 228: Table 2. Atomic coordinates ( x 10
- Page 229 and 230: F(2) 6539(1) 330(1) 6074(1) 63(1) 1
- Page 231 and 232: Table 4. Bond lengths [Å] and angl
- Page 233 and 234: C(20A)-C(15A)-P(1) 119.8(2) C(17A)-
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- Page 237 and 238: O(8) 465(10) 298(8) 275(8) 14(6) 66
- Page 239 and 240: Index ranges -20 ≤ h ≤ 21, -38
- Page 241 and 242: e even larger. All esds (except the
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- Page 247 and 248: Table 2. Atomic coordinates ( x 10
- Page 249 and 250: C(34) 6283(2) 5342(1) 3204(1) 36(1)
- Page 251 and 252: C(92) -899(2) 7522(1) 2196(1) 50(1)
- Page 253 and 254: Table 3. Selected bond lengths [Å]
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- Page 257 and 258: C(75)-C(80) 1.393(3) C(76)-C(77) 1.
- Page 259 and 260: C(71)-B(3)-C(66) 111.6(2) O(10)-B(4
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- Page 265 and 266: C(34) 354(19) 227(18) 490(20) -17(1
- Page 267 and 268: C(92) 660(20) 480(20) 303(18) -43(1
- Page 269 and 270: Completeness to θ = 26.41° 98.1 %
- Page 271 and 272: e even larger. All esds (except the
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- Page 277: Table 2. Atomic coordinates ( x 10
- Page 281 and 282: C(6)-Re(2)-P(2) 94.7(4) C(7)-Re(2)-
- Page 283 and 284: C(33)-C(34) 1.360(17) C(33)-C(38) 1
- Page 285 and 286: C(40)-C(39)-P(2) 121.6(10) C(44)-C(
- Page 287 and 288: Table 5. Anisotropic displacement p
- Page 289 and 290: C(39) 270(80) 380(70) 170(70) 100(6
- Page 291 and 292: θ range for data collection 1.84 t
- Page 293 and 294: covariance matrix. The cell esds ar
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- Page 299 and 300: Table 2. Atomic coordinates ( x 10
- Page 301 and 302: Table 3. Selected bond lengths [Å]
- Page 303 and 304: C(31)-C(32) 1.499(7) C(32)-C(33) 1.
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- Page 307 and 308: C(13) 200(30) 200(30) 190(30) -50(2
- Page 309 and 310: θ range for data collection 1.76 t
- Page 311 and 312: covariance matrix. The cell esds ar
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- Page 317 and 318: Table 2. Atomic coordinates ( x 10
- Page 319 and 320: C(42) 8268(1) 4361(1) 5254(1) 21(1)
- Page 321 and 322: Table 4. Bond lengths [Å] and angl
- Page 323 and 324: O(7)-Na(1)-O(6) 99.94(3) O(3)-Na(1)
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- Page 327 and 328: C(13) 117(2) 100(2) 95(2) -17(2) -2
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Table 1. Crystal data and structure
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Table 1 (cont.) Structure solution
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S333
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S335
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S337
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C(17) 2210(1) 7422(1) 2046(1) 21(1)
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Table 3. Selected bond lengths [Å]
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C(38)-C(39) 1.3936(11) C(40)-C(45)
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C(1A)-C(2A)-C(3A) 120.0 C(4A)-C(3A)
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Table 5. Anisotropic displacement p
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C(4A) 499(16) 390(14) 387(15) -71(1
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