Molecular and crystal structure of an open cyclamphosphorane adduct: cyclamphosphane-bis(borane)

A new approach to internal Lewis pairs featuring a phosphenium acid and a pyridine base

“…The nitrogen-boron bond in 2•BH 3 [OTf] (N(3)-B(1) 1.627(6) A ˚) was within the range of observed s donations of nitrogen to BH 3 (1.56-1.66 A ˚). 10, 11 The added steric bulk of BH 3 caused the plane of the pyridine ring to deviate from being parallel with the BIAN plane by 19. In 2•DMAP[OTf] the P(1)-N(4) bond length was within the range of P-N DMAP dative bonds (1.854(3) cf.…”

“…High (HRMS) resolution mass spectrometry was collected using a Finnigan MAT 8200 instrument. (10), 725 (13), 745(4), 764(1), 797 (8), 819 (5), 1037 (15), 1144 (14), 1221 (12), 1261 (9), 1345 (11), 1412 (7), 1437(2), 1448(3), 1487(6) cm -1 . FT-Raman (relative intensities) n = 117(1), 138(2), 168(3), 214 (6), 361 (8), 405 (7), 487 (13), 563 (10), 956 (5), 1210 (12), 1344 (15), 1436 (11), 1471 (9), 1609(4), 3059( 14) cm -1 .…”

“…268-271 • C. 1 (13), 734 (10), 749 (7), 767 (1), 781(4), 817 (6), 980 (8), 1151 (14), 1269 (15), 1361 (9), 1450 (2), 1466(3), 1490 (5), 1571 (12), 1587(11) cm -1 . FT-Raman (relative intensities) n = 175 (11), 215 (15), 564 (6), 735 (12), 953(4), 981(1), 1044 (14), 1210 (8), 1260 (9), 1342 (13), 1439 (7), 1469 (5), 1521(2), 1611(3), 3062(10) cm -1 . HRMS: C 33 H 25 N 3 P calcd (found) 494.1786 (494.1791).…”

“…19 F{ 1 H} NMR (CDCl 3 ): d -78.5 (s). FT-IR (relative intensities) n = 517 (7), 571 (13), 637(2), 733 (12), 768(4), 801 (15), 823 (8), 1028(1), 1153 (5), 1222 (10), 1279(3), 1349 (11), 1458 (6), 1489(9), 1558( 14) cm -1 .…”

“…FT-Raman (relative intensities) n = 176(8), 213 (14), 563(5), 731 (13), 956(1), 976 (6), 1028 (10), 1212 (9), 1255 (11), 1344 (12), 1415 (15), 1437(4), 1483(3), 1614(2), 3061(7) cm -1 . HRMS: C 33 H 25 N 3 P calcd (found) 494.1786 (494.1782).…”