Calcd for C14H13Cl5N4Os∙H2O (1∙ H2O) (Mr = 622.79 g/mol): C, 27.00; H, 2.43; N, 9.00. Found: C, 27.41; H, 2.56; N, 8.85. ESI-MS in MeOH (negative): m/z 485 [OsIVCl5(Hind)]−, 367 [OsIVCl5]−, 333 [OsCl4]−. MIR, cm− 1: 603, 626, 664, 736, 784, 846, 872, 928, 978, 1077, 1136, 1181, 1238, 1309, 1382, 1441, 1505, 1584, 1618, 2348, 2933, 2975, 3135, 3487 and 3547. FIR, cm− 1: 159, 171, 203, 223, 283, 293, 308, 319, 350, 398, 427, 443, 537, 561 and 614.
UV–vis (H2O), λmax, nm (ε, M− 1 cm− 1): 288 (10 095), 362 (8 912), 406 sh (3 236), 560 (5 075), 598 (4 443). UV–vis (THF), λmax, nm (ε, M− 1 cm− 1): 367 (9 147), 408 sh (3 996), 518 (3 853), 593 (326). UV–vis (DMF), λmax, nm (ε, M− 1 cm− 1): 368 (10 000), 408 sh (3 949), 510 (4 080), 595 (251). UV–vis (DMSO), λmax, nm (ε, M− 1 cm− 1): 367 (5 687), 409 sh (2 752), 521 (2 794), Obeticholic Acid order 597 (304). 1H NMR (DMSO-d6, 500.32 MHz): δ − 14.54 (s, 1H, H3), − 0.43 (t, 1H, J = 7.67 Hz, H6), 2.81 (d, 1H, J = 8.56 Hz, H4), 4.52 (d, 1H, J = 8.83 Hz, H7), 6.66 (t, 1H, J = 6.91 Hz, H5), 7.11 (t, 1H, J = 7.19 Hz, H5′), 7.34 (t, 1H, J = 7.34 Hz, H6′), 7.54 (d, 1H, J = 8.42 Hz, H7′), 7.76 (d, 1H, J = 8.12 Hz, H4′), 8.07 (s, 1H, H3′), 14.25 (s, 1H, H2) ppm. 13C1H NMR (DMSO-d6, 125.82 MHz): I BET 762 δ 58.55 (C9), 99.06 (C7), 104.60 (C5), 110.56 (C7′),
120.67 (C5′), 120.98 (C4′), 123.22 (C9′), 126.41 (C6′), 133.82 (C3′), 140.32 (C8′), 157.09 (C4), 177.15 (C6), Amobarbital 184.29 (C8), 299.7 (C3) ppm. 15N NMR (DMSO-d6, 50.70 MHz): δ 85.9 (N2) ppm. Suitable crystals of 1·H2O for X-ray diffraction study were grown from a solution of 1 in DMSO. Analytical data for 2: ESI-MS in MeOH (negative): m/z 485 [OsIVCl5(Hind)]−, 367 [OsIVCl5]−. UV–vis (H2O), λmax, nm (ε, M− 1 cm− 1): 250 (11 134), 257 (10 982), 271 (10 841), 279 (11 395), 284 (11 751) 294 sh (9 593), 358 (8 882), 401 sh (4 770), 449 sh (2 411), 556 (669), 594 (632). UV–vis (THF), λmax, nm (ε, M− 1 cm− 1):
253 (10 264), 287 (12 955), 294 sh (11 844), 365 (9 728), ~ 510 sh (356). UV–vis (DMF), λmax, nm (ε, M− 1 cm− 1): 287 (15 146), 294 sh (13297), 366 (12 140), ~ 510 sh (244). UV–vis (DMSO), λmax, nm (ε, M− 1 cm− 1): 285 (11 680), 295 sh (9 562), 364 (8 249), 514 (503), 596 (51). UV–vis (MeOH), λmax, nm (ε, M− 1 cm− 1): 249 (9 450), 284 (12 152), 293 (10 019), 361 (8 780), 524 (562). 1H NMR (DMSO-d6, 500.32 MHz): δ − 4.54 (s, 1H, H3), 3.06 (t, 1H, J = 7.7 Hz, H6), 5.90 (d, 1H, J = 7.5 Hz, H4), 7.11 (t, 1H, J = 7.4 Hz, H5′), 7.34 (t, 1H, J = 7.6 Hz, H6′), 7.53 (d, 1H, J = 8.4 Hz, H7′), 7.76 (d, 1H, J = 8.1 Hz, H4′), 8.07 (s, 1H, H3′), 8.23 (t, 1H, J = 7.6 Hz, H5), 10.85 (d, 1H, J = 8.5 Hz, H7), 17.76 (s, 1H, H1) ppm.