- Page 1 and 2:
Homogeneous <stron
- Page 3 and 4:
I. General Considerations. All air-
- Page 5 and 6:
characteristics that matched the pu
- Page 7 and 8:
Figure S3. 1 H NMR timecourse. Reac
- Page 9 and 10:
Reaction of [1-Ph 2][BF 4] with [HP
- Page 11 and 12:
NMR Scale Reaction of [1-Ph 2][BF 4
- Page 13 and 14:
Synthesis of mer,trans-(PPh 3) 2Re(
- Page 15 and 16:
III. Synthesis of Complexes with Pe
- Page 17 and 18:
Figure S13. 31 P{ 1 H} NMR. Figure
- Page 19 and 20:
vessel was sealed and heated to 120
- Page 21 and 22:
Figure S18. 13 C{ 1 H} NMR. Figure
- Page 23 and 24:
Figure S20. 1 H NMR. Figure S21. 31
- Page 25 and 26:
Synthesis of mer,trans-(Ph 2PCHCH 2
- Page 27 and 28:
Figure S26. 13 C{ 1 H} NMR. Synthes
- Page 29 and 30:
Figure S29. 13 C{ 1 H} NMR. Synthes
- Page 31 and 32:
Figure S31. 31 P{ 1 H} NMR. Figure
- Page 33 and 34:
NMR (CD 2Cl 2, 125 MHz): δ 35.88 (
- Page 35 and 36:
Synthesis of trans-[(Ph 2PCH 2CHCH
- Page 37 and 38:
Figure S39. 13 C{ 1 H} NMR (with re
- Page 39 and 40:
Figure S41. 31 P{ 1 H} NMR. Figure
- Page 41 and 42:
Figure S43. 1 H NMR. Figure S44. 31
- Page 43 and 44:
Synthesis of [(Ph 2P(CH 2) 2B(C 8H
- Page 45 and 46:
Figure S49. 19 F NMR. Figure S50. 1
- Page 47 and 48:
= 10.2, 16.4, 2H, Ph 2PCH 2CH 2B(C
- Page 49 and 50:
Figure S55. 11 B{ 1 H} NMR (broad u
- Page 51 and 52:
Figure S57. 31 P{ 1 H} NMR. Figure
- Page 53 and 54:
(C 6D 5Cl, 300 MHz): δ 1.08 (br m,
- Page 55 and 56:
Figure S63. 11 B{ 1 H} NMR (broad u
- Page 57 and 58:
Figure S64. 1 H NMR. Figure S65. 31
- Page 59 and 60:
Figure S67. 1 H NMR (formyl region)
- Page 61 and 62:
environments could be B-O bond brea
- Page 63 and 64:
Figure S69. 1 H NMR (
- Page 65 and 66:
Figure S73. 1 H- 1 H gCO</s
- Page 67 and 68:
Reaction of 2-M 2 with pyridine. A
- Page 69 and 70:
€ B. Pulsed Gradient Spin-Echo Di
- Page 71 and 72:
epeated. If 2-E 2 were strictly mon
- Page 73 and 74:
Figure S80. 31 P{ 1 H} NMR. Thermol
- Page 75 and 76:
Figure S81. 1 H NMR of in-situ gene
- Page 77 and 78:
Figure S85. 13 C{ 1 H} NMR. Figure
- Page 79 and 80:
Figure S89. 1 H- 13 C gHMBC. Reacti
- Page 81 and 82:
location as [1-E 2][BF 4]. Thus we
- Page 83 and 84:
D. Mechanism Studies on the Reducti
- Page 85 and 86:
emoved from the cold bath and allow
- Page 87 and 88:
Figure S95. 31 P{ 1 H} NMR. Figure
- Page 89 and 90:
Figure S98. 1 H NMR (20 °C), hydri
- Page 91 and 92:
of H 2), with the other P-containin
- Page 93 and 94:
was apparent. Attempts to isolate a
- Page 95 and 96:
Figure S105. 13 C{ 1 H} NMR. Figure
- Page 97 and 98:
Reaction of [1-E 2-Mn][BF 4] with 2
- Page 99 and 100:
(br), 20.3, 24.7, 26.4, 28.7 (br),
- Page 101 and 102:
Figure S114. 31 P{ 1 H} NMR. Figure
- Page 103 and 104:
Figure S116. 1 H NMR. Figure S117.
- Page 105 and 106:
Figure S119. 31 P{ 1 H} NMR. Reacti
- Page 107 and 108:
and instead a mixture of 2-M 2, unr
- Page 109 and 110:
(0.0264 mmol) solid [1-E 2][BF 4],
- Page 111 and 112:
Figure S124. 31 P{ 1 H} NMR. Reacti
- Page 113 and 114:
of ~2:1 formyl:hydride, which conve
- Page 115 and 116: Figure S127. 31 P{ 1 H} NMR. Figure
- Page 117 and 118: Decomposition of 2-M 1. While searc
- Page 119 and 120: Figure S133. 1 H{ 31 P} NMR. Figure
- Page 121 and 122: Reaction of [1-M 1][BAr F 4] with [
- Page 123 and 124: Figure S138. 31 P{ 1 H} NMR. Figure
- Page 125 and 126: Figure S140. 1 H NMR time course. B
- Page 127 and 128: the only Re species, but after 2.5
- Page 129 and 130: Figure S143. 1 H NMR. Figure S144.
- Page 131 and 132: Figure S147. 1 H- 1 H gCO</
- Page 133 and 134: Figure S151. Reaction time course (
- Page 135 and 136: one broad doublet), 188.27 (d, J PC
- Page 137 and 138: Low temperature monitoring of the r
- Page 139 and 140: D. Reductions of trans-[(PPh 3)(Ph
- Page 141 and 142: Figure S159. 1 H NMR (with some res
- Page 143 and 144: Figure S163. 1 H- 1 H gCO</
- Page 145 and 146: Reaction of [Na][(PPh 3)(Ph 2P(CH 2
- Page 147 and 148: Figure S168. 13 C{ 1 H} NMR. E. Red
- Page 149 and 150: Figure S170. 31 P{ 1 H} NMR (initia
- Page 151 and 152: VII. Crystallographic Details. Tabl
- Page 153 and 154: Table 1 (cont.) Structure solution
- Page 155 and 156: S155
- Page 157 and 158: S157
- Page 159 and 160: S159
- Page 161 and 162: S161
- Page 163 and 164: S163
- Page 165: C(17A) 7415(2) 3268(1) 5199(1) 15(1
- Page 169 and 170: Table 3. Selected bond lengths [Å]
- Page 171 and 172: C(38A)-C(39A) 1.381(4) C(39A)-C(40A
- Page 173 and 174: O(4A)-C(4A)-Re(1) 122.6(2) C(6A)-C(
- Page 175 and 176: C(28B)-C(23B)-P(2B) 121.5(2) C(25B)
- Page 177 and 178: Table 5. Anisotropic displacement p
- Page 179 and 180: C(46A) 430(20) 201(18) 420(20) -37(
- Page 181 and 182: C(52C) 620(30) 500(30) 620(30) 30(2
- Page 183 and 184: Completeness to θ = 36.56° 86.5 %
- Page 185 and 186: Refinement of F 2 against ALL refle
- Page 187 and 188: S187
- Page 189 and 190: S189
- Page 191 and 192: S191
- Page 193 and 194: S193
- Page 195 and 196: S195
- Page 197 and 198: B(1) 1715(2) 6994(1) 4782(1) 20(1)
- Page 199 and 200: F(17) 4266(1) 11296(1) 3213(1) 32(1
- Page 201 and 202: Table 3. Selected bond lengths [Å]
- Page 203 and 204: C(39A)-C(40A) 1.535(3) C(39A)-C(46A
- Page 205 and 206: C(14)-C(15)-C(16) 119.7(2) C(15)-C(
- Page 207 and 208: F(15)-C(68)-C(67) 115.0(2) C(63)-C(
- Page 209 and 210: Table 5. Anisotropic displacement p
- Page 211 and 212: C(44B) 1370(60) 630(40) 580(30) 20(
- Page 213 and 214: Table 1. Crystal data and structure
- Page 215 and 216: Table 1 (cont.) Structure solution
- Page 217 and 218:
S217
- Page 219 and 220:
S219
- Page 221 and 222:
S221
- Page 223 and 224:
S223
- Page 225 and 226:
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)-
- Page 235 and 236:
Table 5. Anisotropic displacement p
- 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
- Page 243 and 244:
S243
- Page 245 and 246:
S245
- 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]
- Page 255 and 256:
Table 4. Bond lengths [Å] and angl
- 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
- Page 261 and 262:
C(83)-C(82)-C(81) 120.3(3) C(84)-C(
- Page 263 and 264:
Table 5. Anisotropic displacement p
- 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
- Page 273 and 274:
S273
- Page 275 and 276:
S275
- Page 277 and 278:
Table 2. Atomic coordinates ( x 10
- Page 279 and 280:
C(39) 8573(8) 10016(6) 2455(7) 27(3
- 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
- Page 295 and 296:
S295
- Page 297 and 298:
S297
- 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.
- Page 305 and 306:
___________________________________
- 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
- Page 313 and 314:
S313
- Page 315 and 316:
S315
- 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)
- Page 325 and 326:
___________________________________
- Page 327 and 328:
C(13) 117(2) 100(2) 95(2) -17(2) -2
- Page 329 and 330:
Table 1. Crystal data and structure
- Page 331 and 332:
Table 1 (cont.) Structure solution
- Page 333 and 334:
S333
- Page 335 and 336:
S335
- Page 337 and 338:
S337
- Page 339 and 340:
C(17) 2210(1) 7422(1) 2046(1) 21(1)
- Page 341 and 342:
Table 3. Selected bond lengths [Å]
- Page 343 and 344:
C(38)-C(39) 1.3936(11) C(40)-C(45)
- Page 345 and 346:
C(1A)-C(2A)-C(3A) 120.0 C(4A)-C(3A)
- Page 347 and 348:
Table 5. Anisotropic displacement p
- Page 349 and 350:
C(4A) 499(16) 390(14) 387(15) -71(1
Change language