Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101012689/iz1015sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270101012689/iz1015Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270101012689/iz1015IVsup3.hkl |
CCDC references: 175056; 175057
For related literature, see: Barton et al. (1996, 1997); Beckett et al. (1986); Bould et al. (1983, 1991, 1995); Bould, Rath & Barton (1996); Bould, Rath, Fang & Barton (1996); Brennan et al. (1973); Greenwood et al. (1979); Huffman (1974); Kennedy (1984); Nainan & Ryschkewitsch (1969); Sheldrick (1999); Solomon & Porter (1972).
Compound (I) was isolated in high yield (85%) from the reaction of Na[B5H8] and [(CO)(PPh3)3HClOs]. Single crystals of (I) were not grown directly from solutions of the compound; they arose from attempts to grow single crystals of [(PPh3)2(CO)-nido-OsB4H7(BH2·PPh3)], (III). In solution at ambient temperature, (III) loses PPh3 to form an equilibrium mixture from which (I) preferentially crystallizes. Compound (IV), previously unreported, was isolated as a minor product from the preparation of (I). Soluble residues from the preparation of (I) gave, after reduction in volume, a grey precipitate. Preparative thin-layer chromatography (TLC) of the filtrate (silica gel, Aldrich standard TLC grade, with gypsum binder and fluorescent indicator) gave a series of colourless bands, identified as, in order, [(CO)(PPh3)2OsB4H8], (III), [(CO)H(PPh3)2-arachno-OsB3H8] and [BH3PPh3] (Bould et al., 1983; Bould, Rath & Barton, 1996 correct ref?; Barton et al., 1997; Nainan & Ryschkewitsch, 1969). Repeated TLC on solutions of the grey precipitate gave an orange band, identified as [6,6,6-(CO)(PPh3)2-6-nido-Os(B9H13)], (IV). Orange single crystals were obtained by diffusion of hexane into a CD2Cl2 solution of the compound. NMR data (CD2Cl2, 300 K, Bruker 500 AMX spectrometer, p.p.m.) in the above order; assignment δ(11B) [δ(1H) in square brackets]: B1,3 + 12.5 [+4.42], B2 - 28.5 [-0.26], B4 - 28.2 [+2.04], B5 + 8.9 [+5.27], B7 + 14.5 [+4.90], B(8 or 10) +0.81 [+2.69], B(10 or 8) -2.5 [+2.56], B9 + 6.5 [+2.53]; additional 1H data, p.p.m/: H(6/5) -10.26 [2J(31P-1H) 35 Hz], H(6/7) -8.80, H(89/910) -4.54 and -4.45; δ(31P) +8.7 and +14.9.
For (I), cluster-associated H atoms were located from the difference Fourier syntheses and refined freely, with the exception of the bridging atom H23, which was located from the Fourier synthesis and for which the positional parameters were treated as riding on Os2. Bridging atom H26 could not be located. For (IV), cage H atoms were located from the difference Fourier synthesis and, for some, the positions were refined, while for the rest an appropriate riding model was used. The H atoms bridging B8—B9 and B9—B10 could not be located. One of the phenyl rings (C8—C13) in (IV) is disordered. This was resolved and the disorder atoms were refined with anisotropic displacement parameter constraints (EADP command in SHELXTL; Sheldrick, 1999). Non-boron-cage H atoms for both compounds were included in their idealized geometry and refined with appropriate riding models (AFIX command in SHELXTL). The highest residual peaks were found close to the Os atoms [0.89 and 0.99 Å for (I) and (IV), respectively]. Please provide CIF-format data for bonds and angles involving H atoms for both compounds.
For both compounds, data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXTL (Sheldrick, 1999); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[(B5H9Os)(C18H15P)2(CO)] | F(000) = 1600 |
Mr = 805.87 | Dx = 1.544 Mg m−3 |
Monoclinic, Cc | Mo Kα radiation, λ = 0.71073 Å |
a = 16.0054 (1) Å | Cell parameters from 8192 reflections |
b = 13.0200 (1) Å | θ = 2–33° |
c = 17.2445 (1) Å | µ = 3.80 mm−1 |
β = 105.29 (1)° | T = 153 K |
V = 3466.39 (4) Å3 | Irregular, colourless |
Z = 4 | 0.25 × 0.20 × 0.08 mm |
Bruker SMART Query CCD area-detector diffractometer | 9961 independent reflections |
Radiation source: normal-focus sealed tube | 9460 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
ϕ and ω scans | θmax = 30.0°, θmin = 2.1° |
Absorption correction: empirical (using intensity measurements) (SADABS; Blessing, 1995) | h = −22→22 |
Tmin = 0.450, Tmax = 0.751 | k = −18→18 |
31883 measured reflections | l = −24→24 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.026 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.059 | w = 1/[σ2(Fo2) + (0.0182P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max = 0.001 |
9961 reflections | Δρmax = 2.20 e Å−3 |
443 parameters | Δρmin = −1.78 e Å−3 |
2 restraints | Absolute structure: Flack, 1983 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.002 (4) |
[(B5H9Os)(C18H15P)2(CO)] | V = 3466.39 (4) Å3 |
Mr = 805.87 | Z = 4 |
Monoclinic, Cc | Mo Kα radiation |
a = 16.0054 (1) Å | µ = 3.80 mm−1 |
b = 13.0200 (1) Å | T = 153 K |
c = 17.2445 (1) Å | 0.25 × 0.20 × 0.08 mm |
β = 105.29 (1)° |
Bruker SMART Query CCD area-detector diffractometer | 9961 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Blessing, 1995) | 9460 reflections with I > 2σ(I) |
Tmin = 0.450, Tmax = 0.751 | Rint = 0.041 |
31883 measured reflections |
R[F2 > 2σ(F2)] = 0.026 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.059 | Δρmax = 2.20 e Å−3 |
S = 1.03 | Δρmin = −1.78 e Å−3 |
9961 reflections | Absolute structure: Flack, 1983 |
443 parameters | Absolute structure parameter: 0.002 (4) |
2 restraints |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Os2 | 0.50112 (1) | 0.80164 (1) | 0.27089 (1) | 0.01393 (3) | |
H23 | 0.5044 | 0.8033 | 0.3700 | 0.017* | |
P1 | 0.60724 (6) | 0.67533 (9) | 0.26835 (7) | 0.01696 (19) | |
P2 | 0.59124 (5) | 0.94852 (7) | 0.28822 (5) | 0.01514 (15) | |
O | 0.44307 (19) | 0.7775 (3) | 0.09035 (17) | 0.0304 (6) | |
C1 | 0.5621 (2) | 0.5612 (3) | 0.2099 (2) | 0.0224 (7) | |
C2 | 0.4959 (3) | 0.5072 (3) | 0.2305 (3) | 0.0314 (9) | |
H2A | 0.4726 | 0.5324 | 0.2721 | 0.038* | |
C3 | 0.4640 (3) | 0.4182 (4) | 0.1915 (4) | 0.0474 (13) | |
H3A | 0.4202 | 0.3811 | 0.2074 | 0.057* | |
C4 | 0.4951 (3) | 0.3820 (4) | 0.1290 (4) | 0.0539 (16) | |
H4A | 0.4718 | 0.3212 | 0.1012 | 0.065* | |
C5 | 0.5601 (3) | 0.4345 (4) | 0.1072 (3) | 0.0466 (13) | |
H5A | 0.5824 | 0.4091 | 0.0650 | 0.056* | |
C6 | 0.5927 (3) | 0.5240 (4) | 0.1465 (3) | 0.0325 (9) | |
H6A | 0.6366 | 0.5607 | 0.1302 | 0.039* | |
C7 | 0.6679 (2) | 0.6194 (3) | 0.3641 (2) | 0.0207 (7) | |
C8 | 0.7004 (2) | 0.6852 (3) | 0.4292 (2) | 0.0229 (7) | |
H8A | 0.6910 | 0.7572 | 0.4231 | 0.028* | |
C9 | 0.7467 (2) | 0.6448 (3) | 0.5033 (2) | 0.0252 (8) | |
H9A | 0.7685 | 0.6895 | 0.5475 | 0.030* | |
C10 | 0.7609 (2) | 0.5405 (3) | 0.5125 (2) | 0.0292 (8) | |
H10A | 0.7921 | 0.5135 | 0.5631 | 0.035* | |
C11 | 0.7299 (3) | 0.4753 (3) | 0.4482 (3) | 0.0345 (9) | |
H11A | 0.7398 | 0.4035 | 0.4545 | 0.041* | |
C12 | 0.6840 (3) | 0.5146 (3) | 0.3740 (2) | 0.0302 (8) | |
H12A | 0.6635 | 0.4694 | 0.3298 | 0.036* | |
C13 | 0.6914 (2) | 0.7085 (3) | 0.2180 (2) | 0.0217 (7) | |
C14 | 0.6701 (3) | 0.7659 (4) | 0.1479 (2) | 0.0286 (8) | |
H14A | 0.6154 | 0.7991 | 0.1321 | 0.034* | |
C15 | 0.7276 (3) | 0.7760 (4) | 0.1001 (3) | 0.0348 (10) | |
H15A | 0.7121 | 0.8146 | 0.0517 | 0.042* | |
C16 | 0.8081 (3) | 0.7284 (4) | 0.1246 (3) | 0.0423 (12) | |
H16A | 0.8472 | 0.7329 | 0.0918 | 0.051* | |
C17 | 0.8318 (3) | 0.6752 (4) | 0.1957 (3) | 0.0384 (11) | |
H17A | 0.8880 | 0.6459 | 0.2128 | 0.046* | |
C18 | 0.7740 (2) | 0.6637 (4) | 0.2429 (3) | 0.0292 (8) | |
H18A | 0.7903 | 0.6258 | 0.2917 | 0.035* | |
C19 | 0.7028 (2) | 0.9426 (3) | 0.3524 (2) | 0.0185 (6) | |
C20 | 0.7169 (2) | 0.9623 (3) | 0.4342 (2) | 0.0231 (7) | |
H20A | 0.6695 | 0.9812 | 0.4548 | 0.028* | |
C21 | 0.7997 (3) | 0.9548 (3) | 0.4863 (3) | 0.0292 (8) | |
H21A | 0.8085 | 0.9677 | 0.5421 | 0.035* | |
C22 | 0.8688 (3) | 0.9286 (3) | 0.4565 (3) | 0.0333 (9) | |
H22A | 0.9255 | 0.9246 | 0.4916 | 0.040* | |
C23 | 0.8555 (2) | 0.9082 (4) | 0.3756 (3) | 0.0309 (9) | |
H23A | 0.9033 | 0.8903 | 0.3553 | 0.037* | |
C24 | 0.7727 (2) | 0.9134 (3) | 0.3231 (2) | 0.0224 (7) | |
H24A | 0.7639 | 0.8972 | 0.2678 | 0.027* | |
C25 | 0.5962 (2) | 1.0180 (3) | 0.1969 (2) | 0.0181 (6) | |
C26 | 0.6693 (2) | 1.0726 (3) | 0.1903 (2) | 0.0235 (7) | |
H26A | 0.7220 | 1.0670 | 0.2313 | 0.028* | |
C27 | 0.6651 (3) | 1.1347 (3) | 0.1242 (2) | 0.0289 (8) | |
H27A | 0.7152 | 1.1708 | 0.1198 | 0.035* | |
C28 | 0.5889 (3) | 1.1444 (3) | 0.0650 (2) | 0.0277 (8) | |
H28A | 0.5864 | 1.1873 | 0.0198 | 0.033* | |
C29 | 0.5152 (3) | 1.0913 (3) | 0.0712 (2) | 0.0248 (7) | |
H29A | 0.4623 | 1.0980 | 0.0304 | 0.030* | |
C30 | 0.5194 (3) | 1.0288 (4) | 0.1370 (3) | 0.0215 (9) | |
H30A | 0.4692 | 0.9928 | 0.1412 | 0.026* | |
C31 | 0.5505 (2) | 1.0522 (3) | 0.3407 (2) | 0.0184 (6) | |
C32 | 0.4913 (3) | 1.0363 (4) | 0.3863 (3) | 0.0223 (9) | |
H32A | 0.4660 | 0.9705 | 0.3871 | 0.027* | |
C33 | 0.4691 (3) | 1.1159 (4) | 0.4304 (3) | 0.0301 (9) | |
H33A | 0.4285 | 1.1041 | 0.4610 | 0.036* | |
C34 | 0.5054 (3) | 1.2125 (3) | 0.4305 (3) | 0.0317 (9) | |
H34A | 0.4906 | 1.2662 | 0.4617 | 0.038* | |
C35 | 0.5632 (3) | 1.2305 (3) | 0.3848 (3) | 0.0342 (9) | |
H35A | 0.5874 | 1.2969 | 0.3839 | 0.041* | |
C36 | 0.5858 (3) | 1.1510 (3) | 0.3401 (3) | 0.0298 (8) | |
H36A | 0.6255 | 1.1638 | 0.3088 | 0.036* | |
C37 | 0.4674 (2) | 0.7903 (3) | 0.1589 (2) | 0.0192 (7) | |
B1 | 0.3802 (3) | 0.7122 (4) | 0.2865 (3) | 0.0242 (10) | |
B3 | 0.4699 (3) | 0.7120 (3) | 0.3741 (3) | 0.0223 (8) | |
B4 | 0.3650 (3) | 0.7230 (4) | 0.3865 (3) | 0.0288 (10) | |
B5 | 0.3015 (3) | 0.7933 (4) | 0.3151 (3) | 0.0282 (10) | |
B6 | 0.3559 (3) | 0.8382 (4) | 0.2475 (3) | 0.0239 (8) | |
H1 | 0.354 (3) | 0.649 (4) | 0.251 (3) | 0.028 (12)* | |
H3 | 0.516 (3) | 0.649 (4) | 0.406 (3) | 0.024 (11)* | |
H4 | 0.352 (4) | 0.660 (5) | 0.425 (3) | 0.045 (15)* | |
H5 | 0.232 (4) | 0.791 (4) | 0.289 (4) | 0.042 (16)* | |
H6 | 0.327 (3) | 0.883 (3) | 0.192 (2) | 0.017 (10)* | |
H34 | 0.434 (4) | 0.765 (5) | 0.426 (3) | 0.043 (14)* | |
H56 | 0.319 (3) | 0.880 (4) | 0.301 (3) | 0.027 (12)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Os2 | 0.01132 (4) | 0.01635 (5) | 0.01419 (5) | −0.00172 (8) | 0.00348 (3) | −0.00039 (8) |
P1 | 0.0150 (4) | 0.0181 (5) | 0.0178 (5) | −0.0003 (4) | 0.0044 (3) | −0.0024 (4) |
P2 | 0.0123 (3) | 0.0178 (4) | 0.0153 (4) | −0.0014 (3) | 0.0035 (3) | 0.0009 (3) |
O | 0.0271 (14) | 0.0445 (19) | 0.0183 (13) | −0.0012 (12) | 0.0039 (11) | −0.0027 (12) |
C1 | 0.0187 (15) | 0.0193 (18) | 0.0291 (19) | −0.0027 (13) | 0.0061 (14) | −0.0061 (14) |
C2 | 0.035 (2) | 0.023 (2) | 0.042 (2) | −0.0080 (16) | 0.0205 (18) | −0.0140 (17) |
C3 | 0.044 (3) | 0.037 (3) | 0.071 (4) | −0.021 (2) | 0.031 (2) | −0.024 (2) |
C4 | 0.044 (3) | 0.047 (3) | 0.081 (4) | −0.023 (2) | 0.033 (3) | −0.043 (3) |
C5 | 0.040 (2) | 0.050 (3) | 0.058 (3) | −0.014 (2) | 0.027 (2) | −0.031 (2) |
C6 | 0.0274 (18) | 0.038 (2) | 0.035 (2) | −0.0095 (17) | 0.0139 (17) | −0.0175 (18) |
C7 | 0.0194 (15) | 0.0197 (17) | 0.0233 (17) | 0.0026 (13) | 0.0059 (13) | −0.0006 (13) |
C8 | 0.0225 (16) | 0.0220 (19) | 0.0237 (18) | 0.0031 (13) | 0.0049 (14) | 0.0005 (14) |
C9 | 0.0198 (16) | 0.033 (2) | 0.0202 (17) | 0.0023 (15) | 0.0003 (13) | −0.0030 (14) |
C10 | 0.0245 (18) | 0.039 (2) | 0.0209 (18) | 0.0078 (16) | 0.0012 (15) | 0.0064 (16) |
C11 | 0.041 (2) | 0.024 (2) | 0.035 (2) | 0.0097 (18) | 0.0034 (19) | 0.0029 (17) |
C12 | 0.036 (2) | 0.023 (2) | 0.028 (2) | 0.0046 (16) | 0.0026 (16) | −0.0025 (15) |
C13 | 0.0152 (14) | 0.026 (2) | 0.0250 (18) | −0.0055 (13) | 0.0079 (14) | −0.0098 (14) |
C14 | 0.0218 (17) | 0.039 (2) | 0.027 (2) | −0.0070 (17) | 0.0087 (15) | −0.0032 (17) |
C15 | 0.031 (2) | 0.046 (3) | 0.031 (2) | −0.0153 (19) | 0.0138 (18) | −0.0057 (19) |
C16 | 0.030 (2) | 0.054 (3) | 0.051 (3) | −0.018 (2) | 0.026 (2) | −0.022 (2) |
C17 | 0.0198 (18) | 0.042 (3) | 0.057 (3) | −0.0033 (17) | 0.0164 (19) | −0.013 (2) |
C18 | 0.0182 (16) | 0.030 (2) | 0.040 (2) | 0.0004 (15) | 0.0090 (16) | −0.0068 (18) |
C19 | 0.0151 (14) | 0.0187 (17) | 0.0205 (16) | −0.0042 (12) | 0.0026 (12) | 0.0021 (13) |
C20 | 0.0225 (16) | 0.0245 (19) | 0.0199 (17) | −0.0008 (14) | 0.0014 (14) | 0.0004 (14) |
C21 | 0.0272 (18) | 0.028 (2) | 0.027 (2) | 0.0000 (15) | −0.0025 (16) | −0.0016 (16) |
C22 | 0.0205 (17) | 0.034 (2) | 0.037 (2) | 0.0029 (16) | −0.0076 (16) | 0.0014 (17) |
C23 | 0.0160 (15) | 0.033 (2) | 0.041 (2) | 0.0020 (15) | 0.0031 (15) | −0.0020 (18) |
C24 | 0.0170 (14) | 0.0235 (18) | 0.0258 (18) | 0.0003 (13) | 0.0043 (13) | −0.0008 (14) |
C25 | 0.0180 (14) | 0.0199 (17) | 0.0170 (15) | −0.0011 (12) | 0.0058 (12) | 0.0001 (12) |
C26 | 0.0181 (15) | 0.029 (2) | 0.0236 (18) | −0.0046 (14) | 0.0063 (13) | 0.0017 (14) |
C27 | 0.0276 (18) | 0.029 (2) | 0.032 (2) | −0.0061 (15) | 0.0117 (16) | 0.0076 (16) |
C28 | 0.037 (2) | 0.026 (2) | 0.0214 (18) | 0.0004 (16) | 0.0105 (16) | 0.0063 (15) |
C29 | 0.0261 (17) | 0.024 (2) | 0.0204 (18) | 0.0016 (15) | −0.0002 (15) | 0.0035 (15) |
C30 | 0.0203 (18) | 0.022 (2) | 0.022 (2) | 0.0002 (14) | 0.0051 (15) | 0.0022 (16) |
C31 | 0.0157 (14) | 0.0229 (18) | 0.0160 (15) | 0.0009 (12) | 0.0031 (12) | −0.0004 (12) |
C32 | 0.0228 (18) | 0.023 (2) | 0.023 (2) | −0.0003 (15) | 0.0105 (16) | −0.0032 (16) |
C33 | 0.0285 (19) | 0.036 (2) | 0.028 (2) | 0.0034 (17) | 0.0124 (17) | −0.0027 (18) |
C34 | 0.044 (2) | 0.025 (2) | 0.028 (2) | 0.0122 (17) | 0.0128 (19) | −0.0016 (16) |
C35 | 0.049 (3) | 0.0166 (18) | 0.041 (2) | −0.0042 (18) | 0.019 (2) | −0.0027 (17) |
C36 | 0.036 (2) | 0.022 (2) | 0.036 (2) | −0.0036 (16) | 0.0181 (18) | −0.0026 (16) |
C37 | 0.0118 (13) | 0.0217 (18) | 0.0233 (18) | −0.0015 (12) | 0.0033 (13) | 0.0018 (13) |
B1 | 0.022 (2) | 0.024 (2) | 0.027 (2) | −0.0070 (18) | 0.0063 (18) | −0.0030 (19) |
B3 | 0.0239 (18) | 0.021 (2) | 0.024 (2) | −0.0028 (15) | 0.0106 (16) | 0.0045 (15) |
B4 | 0.026 (2) | 0.030 (2) | 0.036 (3) | −0.0044 (18) | 0.018 (2) | 0.0029 (19) |
B5 | 0.0177 (18) | 0.030 (2) | 0.041 (3) | −0.0028 (16) | 0.0149 (18) | −0.0043 (19) |
B6 | 0.0171 (17) | 0.030 (2) | 0.025 (2) | −0.0003 (16) | 0.0052 (15) | −0.0029 (17) |
Os2—C37 | 1.869 (4) | C20—C21 | 1.394 (5) |
Os2—B3 | 2.291 (4) | C20—H20A | 0.9500 |
Os2—B6 | 2.301 (4) | C21—C22 | 1.381 (6) |
Os2—B1 | 2.335 (5) | C21—H21A | 0.9500 |
Os2—P2 | 2.3664 (9) | C22—C23 | 1.381 (6) |
Os2—P1 | 2.3729 (11) | C22—H22A | 0.9500 |
Os2—H23 | 1.6961 | C23—C24 | 1.395 (5) |
P1—C7 | 1.831 (4) | C23—H23A | 0.9500 |
P1—C1 | 1.833 (4) | C24—H24A | 0.9500 |
P1—C13 | 1.836 (4) | C25—C30 | 1.388 (6) |
P2—C25 | 1.835 (3) | C25—C26 | 1.399 (5) |
P2—C19 | 1.838 (3) | C26—C27 | 1.384 (5) |
P2—C31 | 1.838 (4) | C26—H26A | 0.9500 |
O—C37 | 1.155 (5) | C27—C28 | 1.375 (6) |
C1—C2 | 1.393 (5) | C27—H27A | 0.9500 |
C1—C6 | 1.399 (5) | C28—C29 | 1.396 (6) |
C2—C3 | 1.369 (6) | C28—H28A | 0.9500 |
C2—H2A | 0.9500 | C29—C30 | 1.383 (6) |
C3—C4 | 1.384 (7) | C29—H29A | 0.9500 |
C3—H3A | 0.9500 | C30—H30A | 0.9500 |
C4—C5 | 1.376 (7) | C31—C32 | 1.398 (5) |
C4—H4A | 0.9500 | C31—C36 | 1.406 (5) |
C5—C6 | 1.379 (6) | C32—C33 | 1.386 (6) |
C5—H5A | 0.9500 | C32—H32A | 0.9500 |
C6—H6A | 0.9500 | C33—C34 | 1.385 (6) |
C7—C12 | 1.391 (6) | C33—H33A | 0.9500 |
C7—C8 | 1.399 (5) | C34—C35 | 1.384 (6) |
C8—C9 | 1.400 (6) | C34—H34A | 0.9500 |
C8—H8A | 0.9500 | C35—C36 | 1.393 (6) |
C9—C10 | 1.379 (6) | C35—H35A | 0.9500 |
C9—H9A | 0.9500 | C36—H36A | 0.9500 |
C10—C11 | 1.381 (6) | B1—B6 | 1.777 (7) |
C10—H10A | 0.9500 | B1—B3 | 1.788 (7) |
C11—C12 | 1.394 (6) | B1—B5 | 1.808 (7) |
C11—H11A | 0.9500 | B1—B4 | 1.809 (8) |
C12—H12A | 0.9500 | B1—H1 | 1.04 (5) |
C13—C14 | 1.386 (6) | B3—B4 | 1.753 (6) |
C13—C18 | 1.404 (5) | B3—H23 | 1.3202 |
C14—C15 | 1.394 (6) | B3—H3 | 1.15 (5) |
C14—H14A | 0.9500 | B3—H34 | 1.37 (6) |
C15—C16 | 1.391 (7) | B4—B5 | 1.652 (8) |
C15—H15A | 0.9500 | B4—H4 | 1.10 (6) |
C16—C17 | 1.371 (8) | B4—H34 | 1.25 (6) |
C16—H16A | 0.9500 | B5—B6 | 1.730 (6) |
C17—C18 | 1.392 (6) | B5—H5 | 1.09 (6) |
C17—H17A | 0.9500 | B5—H56 | 1.20 (5) |
C18—H18A | 0.9500 | B6—H6 | 1.11 (4) |
C19—C20 | 1.392 (5) | B6—H56 | 1.33 (4) |
C19—C24 | 1.396 (5) | ||
C37—Os2—B3 | 134.42 (15) | C24—C23—H23A | 119.6 |
C37—Os2—B6 | 80.32 (15) | C23—C24—C19 | 119.6 (4) |
B3—Os2—B6 | 79.87 (16) | C23—C24—H24A | 120.2 |
C37—Os2—B1 | 93.31 (17) | C19—C24—H24A | 120.2 |
B3—Os2—B1 | 45.46 (18) | C30—C25—C26 | 118.8 (3) |
B6—Os2—B1 | 45.07 (19) | C30—C25—P2 | 117.3 (3) |
C37—Os2—P2 | 101.22 (11) | C26—C25—P2 | 123.1 (3) |
B3—Os2—P2 | 124.35 (12) | C27—C26—C25 | 120.3 (3) |
B6—Os2—P2 | 114.12 (13) | C27—C26—H26A | 119.9 |
B1—Os2—P2 | 152.23 (15) | C25—C26—H26A | 119.9 |
C37—Os2—P1 | 86.53 (11) | C28—C27—C26 | 120.4 (3) |
B3—Os2—P1 | 88.02 (11) | C28—C27—H27A | 119.8 |
B6—Os2—P1 | 146.59 (13) | C26—C27—H27A | 119.8 |
B1—Os2—P1 | 106.00 (16) | C27—C28—C29 | 120.0 (3) |
P2—Os2—P1 | 98.46 (3) | C27—C28—H28A | 120.0 |
C37—Os2—H23 | 165.0 | C29—C28—H28A | 120.0 |
B3—Os2—H23 | 34.8 | C30—C29—C28 | 119.6 (4) |
B6—Os2—H23 | 86.3 | C30—C29—H29A | 120.2 |
B1—Os2—H23 | 72.3 | C28—C29—H29A | 120.2 |
P2—Os2—H23 | 90.4 | C29—C30—C25 | 120.9 (4) |
P1—Os2—H23 | 101.3 | C29—C30—H30A | 119.6 |
C7—P1—C1 | 102.19 (18) | C25—C30—H30A | 119.6 |
C7—P1—C13 | 103.80 (17) | C32—C31—C36 | 118.3 (4) |
C1—P1—C13 | 99.39 (17) | C32—C31—P2 | 123.3 (3) |
C7—P1—Os2 | 118.11 (12) | C36—C31—P2 | 118.2 (3) |
C1—P1—Os2 | 113.06 (12) | C33—C32—C31 | 120.5 (4) |
C13—P1—Os2 | 117.63 (14) | C33—C32—H32A | 119.7 |
C25—P2—C19 | 106.43 (15) | C31—C32—H32A | 119.7 |
C25—P2—C31 | 99.31 (16) | C34—C33—C32 | 120.7 (4) |
C19—P2—C31 | 98.54 (16) | C34—C33—H33A | 119.6 |
C25—P2—Os2 | 116.90 (11) | C32—C33—H33A | 119.6 |
C19—P2—Os2 | 120.33 (12) | C35—C34—C33 | 119.8 (4) |
C31—P2—Os2 | 111.87 (11) | C35—C34—H34A | 120.1 |
C2—C1—C6 | 118.1 (3) | C33—C34—H34A | 120.1 |
C2—C1—P1 | 119.1 (3) | C34—C35—C36 | 120.0 (4) |
C6—C1—P1 | 122.8 (3) | C34—C35—H35A | 120.0 |
C3—C2—C1 | 120.8 (4) | C36—C35—H35A | 120.0 |
C3—C2—H2A | 119.6 | C35—C36—C31 | 120.7 (4) |
C1—C2—H2A | 119.6 | C35—C36—H36A | 119.6 |
C2—C3—C4 | 120.4 (4) | C31—C36—H36A | 119.6 |
C2—C3—H3A | 119.8 | O—C37—Os2 | 175.2 (3) |
C4—C3—H3A | 119.8 | B6—B1—B3 | 111.6 (3) |
C5—C4—C3 | 119.7 (4) | B6—B1—B5 | 57.7 (3) |
C5—C4—H4A | 120.1 | B3—B1—B5 | 103.5 (4) |
C3—C4—H4A | 120.1 | B6—B1—B4 | 102.6 (4) |
C4—C5—C6 | 120.1 (4) | B3—B1—B4 | 58.3 (3) |
C4—C5—H5A | 119.9 | B5—B1—B4 | 54.3 (3) |
C6—C5—H5A | 120.0 | B6—B1—Os2 | 66.5 (2) |
C5—C6—C1 | 120.7 (4) | B3—B1—Os2 | 66.0 (2) |
C5—C6—H6A | 119.6 | B5—B1—Os2 | 113.5 (3) |
C1—C6—H6A | 119.6 | B4—B1—Os2 | 113.3 (3) |
C12—C7—C8 | 119.0 (3) | B6—B1—H1 | 119 (3) |
C12—C7—P1 | 122.6 (3) | B3—B1—H1 | 127 (3) |
C8—C7—P1 | 118.4 (3) | B5—B1—H1 | 115 (3) |
C7—C8—C9 | 119.8 (4) | B4—B1—H1 | 120 (3) |
C7—C8—H8A | 120.1 | Os2—B1—H1 | 122 (3) |
C9—C8—H8A | 120.1 | B4—B3—B1 | 61.4 (3) |
C10—C9—C8 | 120.5 (4) | B4—B3—Os2 | 117.8 (3) |
C10—C9—H9A | 119.8 | B1—B3—Os2 | 68.6 (2) |
C8—C9—H9A | 119.8 | B4—B3—H23 | 111.2 |
C9—C10—C11 | 119.9 (4) | B1—B3—H23 | 102.0 |
C9—C10—H10A | 120.0 | Os2—B3—H23 | 47.1 |
C11—C10—H10A | 120.0 | B4—B3—H3 | 121 (2) |
C10—C11—C12 | 120.2 (4) | B1—B3—H3 | 133 (2) |
C10—C11—H11A | 119.9 | Os2—B3—H3 | 120 (2) |
C12—C11—H11A | 119.9 | H23—B3—H3 | 116.9 |
C7—C12—C11 | 120.6 (4) | B4—B3—H34 | 45 (2) |
C7—C12—H12A | 119.7 | B1—B3—H34 | 99 (2) |
C11—C12—H12A | 119.7 | Os2—B3—H34 | 117 (3) |
C14—C13—C18 | 119.1 (4) | H23—B3—H34 | 80.4 |
C14—C13—P1 | 119.8 (3) | H3—B3—H34 | 112 (3) |
C18—C13—P1 | 120.4 (3) | B5—B4—B3 | 112.0 (3) |
C13—C14—C15 | 121.2 (4) | B5—B4—B1 | 62.8 (3) |
C13—C14—H14A | 119.4 | B3—B4—B1 | 60.2 (3) |
C15—C14—H14A | 119.4 | B5—B4—H4 | 133 (3) |
C16—C15—C14 | 118.7 (5) | B3—B4—H4 | 110 (3) |
C16—C15—H15A | 120.6 | B1—B4—H4 | 127 (3) |
C14—C15—H15A | 120.6 | B5—B4—H34 | 116 (3) |
C17—C16—C15 | 120.8 (4) | B3—B4—H34 | 51 (3) |
C17—C16—H16A | 119.6 | B1—B4—H34 | 103 (3) |
C15—C16—H16A | 119.6 | H4—B4—H34 | 106 (4) |
C16—C17—C18 | 120.5 (4) | B4—B5—B6 | 111.7 (3) |
C16—C17—H17A | 119.7 | B4—B5—B1 | 62.9 (3) |
C18—C17—H17A | 119.7 | B6—B5—B1 | 60.2 (3) |
C17—C18—C13 | 119.6 (4) | B4—B5—H5 | 131 (3) |
C17—C18—H18A | 120.2 | B6—B5—H5 | 112 (3) |
C13—C18—H18A | 120.2 | B1—B5—H5 | 126 (3) |
C20—C19—C24 | 119.1 (3) | B4—B5—H56 | 123 (2) |
C20—C19—P2 | 118.3 (3) | B6—B5—H56 | 50 (2) |
C24—C19—P2 | 122.5 (3) | B1—B5—H56 | 106 (2) |
C19—C20—C21 | 120.8 (4) | H5—B5—H56 | 102 (3) |
C19—C20—H20A | 119.6 | B5—B6—B1 | 62.0 (3) |
C21—C20—H20A | 119.6 | B5—B6—Os2 | 118.5 (3) |
C22—C21—C20 | 119.7 (4) | B1—B6—Os2 | 68.5 (2) |
C22—C21—H21A | 120.1 | B5—B6—H6 | 126 (2) |
C20—C21—H21A | 120.1 | B1—B6—H6 | 144 (2) |
C23—C22—C21 | 119.9 (3) | Os2—B6—H6 | 116 (2) |
C23—C22—H22A | 120.0 | B5—B6—H56 | 44 (2) |
C21—C22—H22A | 120.0 | B1—B6—H56 | 102 (2) |
C22—C23—C24 | 120.9 (4) | Os2—B6—H56 | 125.0 (19) |
C22—C23—H23A | 119.6 | H6—B6—H56 | 103 (3) |
[(B9H13Os)(C18H15P)2(CO)] | F(000) = 1696 |
Mr = 853.14 | Dx = 1.526 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 10.4617 (1) Å | Cell parameters from 8192 reflections |
b = 15.6821 (1) Å | θ = 2–25° |
c = 22.6315 (3) Å | µ = 3.55 mm−1 |
β = 91.08 (1)° | T = 223 K |
V = 3712.29 (7) Å3 | Irregular, orange |
Z = 4 | 0.28 × 0.20 × 0.04 mm |
Bruker SMART Query CCD area-detector diffractometer | 6483 independent reflections |
Radiation source: normal-focus sealed tube | 5001 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.01 |
ϕ and ω scans | θmax = 25.0°, θmin = 1.8° |
Absorption correction: empirical (using intensity measurements) (SADABS; Blessing, 1995) | h = −12→12 |
Tmin = 0.436, Tmax = 0.871 | k = −18→18 |
74813 measured reflections | l = −26→26 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.057 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.116 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.18 | w = 1/[σ2(Fo2) + (0.0197P)2 + 26.7668P] where P = (Fo2 + 2Fc2)/3 |
6483 reflections | (Δ/σ)max = 0.002 |
491 parameters | Δρmax = 1.26 e Å−3 |
36 restraints | Δρmin = −1.16 e Å−3 |
[(B9H13Os)(C18H15P)2(CO)] | V = 3712.29 (7) Å3 |
Mr = 853.14 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 10.4617 (1) Å | µ = 3.55 mm−1 |
b = 15.6821 (1) Å | T = 223 K |
c = 22.6315 (3) Å | 0.28 × 0.20 × 0.04 mm |
β = 91.08 (1)° |
Bruker SMART Query CCD area-detector diffractometer | 6483 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Blessing, 1995) | 5001 reflections with I > 2σ(I) |
Tmin = 0.436, Tmax = 0.871 | Rint = 0.01 |
74813 measured reflections |
R[F2 > 2σ(F2)] = 0.057 | 36 restraints |
wR(F2) = 0.116 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.18 | w = 1/[σ2(Fo2) + (0.0197P)2 + 26.7668P] where P = (Fo2 + 2Fc2)/3 |
6483 reflections | Δρmax = 1.26 e Å−3 |
491 parameters | Δρmin = −1.16 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Os6 | 0.11446 (3) | 0.22460 (2) | 0.13120 (2) | 0.03850 (12) | |
P1 | −0.0532 (2) | 0.32366 (14) | 0.14111 (11) | 0.0399 (5) | |
P2 | 0.0107 (2) | 0.09573 (14) | 0.15819 (10) | 0.0364 (5) | |
O1 | 0.2200 (8) | 0.2474 (5) | 0.2554 (4) | 0.084 (3) | |
B1 | 0.3129 (12) | 0.1735 (13) | 0.0156 (6) | 0.083 (5) | |
H1 | 0.348 (11) | 0.105 (7) | −0.010 (5) | 0.100* | |
B2 | 0.2998 (11) | 0.1722 (8) | 0.0920 (6) | 0.053 (3) | |
H2 | 0.349 (9) | 0.123 (6) | 0.117 (4) | 0.063* | |
B3 | 0.4027 (13) | 0.2443 (9) | 0.0580 (6) | 0.071 (4) | |
H3 | 0.516 (10) | 0.240 (6) | 0.072 (4) | 0.085* | |
B4 | 0.3619 (17) | 0.2673 (14) | −0.0170 (7) | 0.101 (5) | |
H4 | 0.454 (13) | 0.246 (8) | −0.051 (6) | 0.121* | |
B5 | 0.1630 (11) | 0.1549 (8) | 0.0442 (5) | 0.050 (3) | |
H5 | 0.115 (9) | 0.096 (6) | 0.029 (4) | 0.060* | |
H56 | 0.075 (8) | 0.207 (6) | 0.068 (4) | 0.060* | |
B7 | 0.3100 (11) | 0.2834 (9) | 0.1105 (7) | 0.068 (4) | |
H7 | 0.375 (10) | 0.315 (6) | 0.147 (4) | 0.081* | |
H67 | 0.172 (10) | 0.313 (6) | 0.108 (4) | 0.081* | |
B8 | 0.3455 (16) | 0.3468 (10) | 0.0398 (7) | 0.092 (5) | |
H8 | 0.4170 | 0.4154 | 0.0452 | 0.111* | |
B9 | 0.2314 (16) | 0.3380 (13) | −0.0178 (8) | 0.114 (7) | |
H9 | 0.2026 | 0.3838 | −0.0580 | 0.136* | |
B10 | 0.2055 (16) | 0.2272 (13) | −0.0270 (7) | 0.103 (6) | |
H10 | 0.159 (12) | 0.228 (8) | −0.073 (6) | 0.124* | |
C1 | 0.1748 (8) | 0.2389 (6) | 0.2087 (5) | 0.054 (3) | |
C2 | −0.0018 (9) | 0.4309 (5) | 0.1624 (4) | 0.045 (2) | |
C3 | 0.1242 (8) | 0.4531 (6) | 0.1773 (4) | 0.045 (2) | |
H3A | 0.1879 | 0.4109 | 0.1783 | 0.054* | |
C4 | 0.1564 (9) | 0.5373 (6) | 0.1907 (4) | 0.051 (2) | |
H4A | 0.2416 | 0.5513 | 0.2006 | 0.061* | |
C5 | 0.0647 (10) | 0.6001 (6) | 0.1895 (5) | 0.061 (3) | |
H5A | 0.0868 | 0.6569 | 0.1979 | 0.074* | |
C6 | −0.0609 (10) | 0.5786 (7) | 0.1755 (5) | 0.070 (3) | |
H6A | −0.1244 | 0.6210 | 0.1756 | 0.085* | |
C7 | −0.0935 (9) | 0.4958 (6) | 0.1616 (5) | 0.062 (3) | |
H7A | −0.1788 | 0.4827 | 0.1513 | 0.075* | |
C8 | −0.1305 (7) | 0.3459 (5) | 0.0696 (4) | 0.042 (2) | |
C11 | −0.2348 (11) | 0.3868 (9) | −0.0419 (5) | 0.087 (4) | |
H11A | −0.2682 | 0.3908 | −0.0806 | 0.104* | |
C9 | −0.0595 (19) | 0.3687 (10) | 0.0218 (7) | 0.076 (7) | 0.610 (10) |
H9A | 0.0298 | 0.3684 | 0.0271 | 0.091* | 0.610 (10) |
C10 | −0.1054 (16) | 0.3918 (12) | −0.0329 (10) | 0.075 (7) | 0.610 (10) |
H10A | −0.0507 | 0.4103 | −0.0627 | 0.090* | 0.610 (10) |
C12 | −0.3158 (16) | 0.3763 (16) | 0.0032 (6) | 0.091 (7) | 0.610 (10) |
H12 | −0.4045 | 0.3836 | −0.0018 | 0.109* | 0.610 (10) |
C13 | −0.2609 (12) | 0.3540 (11) | 0.0570 (7) | 0.060 (4) | 0.610 (10) |
H13 | −0.3169 | 0.3434 | 0.0881 | 0.072* | 0.610 (10) |
C9' | −0.084 (3) | 0.4160 (16) | 0.0401 (13) | 0.076 (7) | 0.390 (10) |
H9' | −0.0202 | 0.4512 | 0.0570 | 0.091* | 0.390 (10) |
C10' | −0.135 (2) | 0.4319 (19) | −0.0159 (14) | 0.075 (7) | 0.390 (10) |
H10' | −0.0994 | 0.4767 | −0.0377 | 0.090* | 0.390 (10) |
C12' | −0.265 (3) | 0.3130 (19) | −0.0079 (11) | 0.091 (7) | 0.390 (10) |
H12' | −0.3271 | 0.2772 | −0.0254 | 0.109* | 0.390 (10) |
C13' | −0.217 (2) | 0.2848 (16) | 0.0477 (9) | 0.060 (4) | 0.390 (10) |
H13' | −0.2396 | 0.2338 | 0.0667 | 0.072* | 0.390 (10) |
C14 | −0.1820 (8) | 0.3111 (5) | 0.1942 (4) | 0.041 (2) | |
C15 | −0.1684 (11) | 0.3461 (7) | 0.2490 (5) | 0.067 (3) | |
H15A | −0.0950 | 0.3786 | 0.2578 | 0.080* | |
C16 | −0.2602 (12) | 0.3354 (7) | 0.2926 (5) | 0.075 (3) | |
H16A | −0.2475 | 0.3586 | 0.3306 | 0.090* | |
C17 | −0.3685 (11) | 0.2905 (6) | 0.2788 (6) | 0.069 (3) | |
H17A | −0.4327 | 0.2843 | 0.3070 | 0.083* | |
C18 | −0.3843 (11) | 0.2538 (7) | 0.2234 (6) | 0.072 (3) | |
H18A | −0.4588 | 0.2226 | 0.2143 | 0.086* | |
C19 | −0.2920 (9) | 0.2630 (7) | 0.1820 (5) | 0.061 (3) | |
H19A | −0.3025 | 0.2368 | 0.1448 | 0.074* | |
C20 | 0.0986 (8) | −0.0011 (5) | 0.1381 (4) | 0.041 (2) | |
C21 | 0.0474 (9) | −0.0656 (6) | 0.1040 (4) | 0.046 (2) | |
H21A | −0.0351 | −0.0591 | 0.0875 | 0.055* | |
C22 | 0.1153 (10) | −0.1404 (6) | 0.0936 (4) | 0.057 (3) | |
H22A | 0.0787 | −0.1839 | 0.0702 | 0.069* | |
C23 | 0.2354 (11) | −0.1500 (7) | 0.1174 (5) | 0.064 (3) | |
H23A | 0.2822 | −0.2001 | 0.1104 | 0.077* | |
C24 | 0.2872 (10) | −0.0860 (7) | 0.1516 (5) | 0.062 (3) | |
H24A | 0.3694 | −0.0933 | 0.1684 | 0.075* | |
C25 | 0.2217 (9) | −0.0114 (6) | 0.1621 (4) | 0.048 (2) | |
H25A | 0.2594 | 0.0321 | 0.1850 | 0.058* | |
C26 | −0.0092 (8) | 0.0785 (6) | 0.2374 (4) | 0.044 (2) | |
C27 | −0.0404 (10) | 0.1444 (7) | 0.2746 (4) | 0.062 (3) | |
H27A | −0.0472 | 0.1999 | 0.2591 | 0.074* | |
C28 | −0.0619 (12) | 0.1320 (8) | 0.3336 (5) | 0.076 (3) | |
H28A | −0.0849 | 0.1783 | 0.3575 | 0.091* | |
C29 | −0.0499 (10) | 0.0518 (8) | 0.3580 (5) | 0.064 (3) | |
H29A | −0.0606 | 0.0435 | 0.3988 | 0.077* | |
C30 | −0.0224 (9) | −0.0150 (7) | 0.3223 (4) | 0.058 (3) | |
H30A | −0.0174 | −0.0702 | 0.3384 | 0.069* | |
C31 | −0.0014 (8) | −0.0035 (6) | 0.2622 (4) | 0.051 (2) | |
H31A | 0.0179 | −0.0506 | 0.2383 | 0.061* | |
C32 | −0.1498 (8) | 0.0770 (5) | 0.1274 (4) | 0.039 (2) | |
C33 | −0.1737 (9) | 0.0861 (8) | 0.0683 (4) | 0.066 (3) | |
H33A | −0.1072 | 0.1034 | 0.0437 | 0.079* | |
C34 | −0.2943 (10) | 0.0704 (8) | 0.0435 (5) | 0.078 (4) | |
H34A | −0.3076 | 0.0748 | 0.0024 | 0.093* | |
C35 | −0.3935 (9) | 0.0485 (6) | 0.0793 (5) | 0.057 (3) | |
H35A | −0.4761 | 0.0399 | 0.0633 | 0.068* | |
C36 | −0.3704 (9) | 0.0395 (7) | 0.1377 (5) | 0.063 (3) | |
H36A | −0.4378 | 0.0234 | 0.1622 | 0.075* | |
C37 | −0.2497 (9) | 0.0534 (6) | 0.1630 (5) | 0.053 (2) | |
H37A | −0.2363 | 0.0467 | 0.2039 | 0.064* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Os6 | 0.0303 (2) | 0.0371 (2) | 0.0479 (2) | 0.0012 (2) | −0.0065 (1) | −0.0054 (2) |
P1 | 0.0346 (12) | 0.0330 (12) | 0.0517 (14) | −0.0004 (10) | −0.0055 (10) | −0.0041 (11) |
P2 | 0.0355 (12) | 0.0365 (12) | 0.0372 (13) | 0.0040 (10) | 0.0000 (10) | −0.0040 (10) |
O1 | 0.099 (6) | 0.081 (6) | 0.072 (5) | 0.020 (4) | −0.047 (5) | −0.023 (4) |
B1 | 0.047 (7) | 0.150 (15) | 0.053 (8) | −0.025 (9) | 0.011 (6) | 0.012 (9) |
B2 | 0.044 (6) | 0.049 (7) | 0.065 (8) | 0.009 (6) | 0.001 (6) | 0.003 (6) |
B3 | 0.063 (8) | 0.073 (10) | 0.077 (9) | 0.008 (7) | −0.006 (7) | 0.002 (7) |
B4 | 0.087 (11) | 0.140 (16) | 0.076 (10) | −0.014 (12) | −0.013 (9) | −0.004 (11) |
B5 | 0.043 (6) | 0.053 (7) | 0.055 (7) | −0.003 (5) | 0.005 (5) | −0.010 (6) |
B7 | 0.037 (6) | 0.054 (7) | 0.111 (11) | −0.006 (6) | −0.007 (7) | 0.002 (8) |
B8 | 0.106 (13) | 0.082 (11) | 0.088 (11) | −0.020 (9) | −0.012 (9) | 0.039 (9) |
B9 | 0.081 (11) | 0.133 (16) | 0.126 (15) | −0.024 (11) | −0.028 (10) | 0.075 (13) |
B10 | 0.098 (12) | 0.136 (15) | 0.076 (10) | −0.057 (12) | −0.019 (9) | 0.051 (11) |
C1 | 0.037 (5) | 0.043 (5) | 0.083 (8) | 0.006 (4) | −0.007 (5) | 0.001 (5) |
C2 | 0.045 (5) | 0.032 (5) | 0.059 (6) | −0.002 (4) | −0.004 (4) | −0.002 (4) |
C3 | 0.036 (5) | 0.046 (5) | 0.052 (6) | 0.001 (4) | −0.009 (4) | −0.003 (4) |
C4 | 0.044 (5) | 0.044 (5) | 0.065 (7) | −0.002 (4) | −0.010 (5) | −0.010 (5) |
C5 | 0.058 (6) | 0.040 (5) | 0.085 (8) | −0.007 (5) | −0.010 (6) | −0.013 (5) |
C6 | 0.052 (6) | 0.052 (6) | 0.108 (9) | 0.009 (5) | −0.013 (6) | −0.029 (6) |
C7 | 0.038 (5) | 0.049 (6) | 0.100 (9) | 0.002 (5) | −0.015 (5) | −0.023 (6) |
C8 | 0.031 (4) | 0.045 (5) | 0.051 (6) | 0.000 (4) | 0.002 (4) | −0.008 (4) |
C11 | 0.077 (9) | 0.138 (12) | 0.044 (7) | 0.008 (8) | −0.013 (6) | 0.005 (7) |
C9 | 0.060 (10) | 0.083 (16) | 0.084 (15) | −0.010 (12) | −0.030 (10) | 0.044 (13) |
C10 | 0.073 (12) | 0.063 (16) | 0.088 (15) | 0.001 (10) | −0.004 (11) | 0.036 (12) |
C12 | 0.035 (10) | 0.18 (2) | 0.059 (10) | 0.011 (10) | −0.013 (8) | 0.002 (13) |
C13 | 0.047 (8) | 0.076 (11) | 0.057 (9) | −0.002 (8) | 0.001 (7) | 0.020 (9) |
C9' | 0.060 (10) | 0.083 (16) | 0.084 (15) | −0.010 (12) | −0.030 (10) | 0.044 (13) |
C10' | 0.073 (12) | 0.063 (16) | 0.088 (15) | 0.001 (10) | −0.004 (11) | 0.036 (12) |
C12' | 0.035 (10) | 0.18 (2) | 0.059 (10) | 0.011 (10) | −0.013 (8) | 0.002 (13) |
C13' | 0.047 (8) | 0.076 (11) | 0.057 (9) | −0.002 (8) | 0.001 (7) | 0.020 (9) |
C14 | 0.039 (5) | 0.030 (4) | 0.053 (6) | 0.004 (4) | 0.003 (4) | 0.003 (4) |
C15 | 0.063 (7) | 0.058 (7) | 0.080 (8) | −0.015 (6) | 0.020 (6) | −0.013 (6) |
C16 | 0.104 (10) | 0.043 (6) | 0.079 (8) | −0.009 (7) | 0.033 (7) | −0.013 (6) |
C17 | 0.077 (8) | 0.031 (6) | 0.100 (10) | 0.013 (5) | 0.042 (7) | 0.023 (6) |
C18 | 0.055 (6) | 0.073 (8) | 0.088 (9) | −0.012 (6) | 0.007 (6) | 0.028 (7) |
C19 | 0.056 (6) | 0.059 (6) | 0.068 (7) | −0.010 (5) | −0.005 (5) | 0.015 (6) |
C20 | 0.047 (5) | 0.039 (5) | 0.039 (5) | 0.002 (4) | −0.005 (4) | 0.005 (4) |
C21 | 0.044 (5) | 0.056 (6) | 0.038 (5) | 0.009 (5) | −0.002 (4) | −0.005 (4) |
C22 | 0.066 (7) | 0.052 (6) | 0.054 (6) | 0.004 (5) | 0.002 (5) | −0.015 (5) |
C23 | 0.069 (7) | 0.060 (7) | 0.063 (7) | 0.019 (6) | 0.019 (6) | 0.003 (6) |
C24 | 0.047 (6) | 0.068 (7) | 0.072 (7) | 0.021 (5) | 0.001 (5) | 0.021 (6) |
C25 | 0.051 (6) | 0.046 (5) | 0.049 (6) | −0.002 (5) | −0.006 (5) | 0.003 (5) |
C26 | 0.041 (5) | 0.056 (6) | 0.035 (5) | −0.002 (4) | −0.004 (4) | −0.004 (4) |
C27 | 0.077 (7) | 0.069 (7) | 0.039 (6) | 0.020 (6) | −0.002 (5) | −0.001 (5) |
C28 | 0.093 (9) | 0.091 (9) | 0.043 (6) | 0.021 (7) | 0.008 (6) | −0.006 (6) |
C29 | 0.061 (7) | 0.090 (9) | 0.041 (6) | 0.005 (6) | 0.009 (5) | 0.007 (6) |
C30 | 0.046 (6) | 0.075 (7) | 0.052 (6) | −0.010 (5) | 0.003 (5) | 0.015 (6) |
C31 | 0.041 (5) | 0.060 (6) | 0.051 (6) | 0.001 (5) | 0.000 (4) | −0.008 (5) |
C32 | 0.030 (4) | 0.030 (4) | 0.055 (6) | 0.002 (4) | −0.004 (4) | −0.002 (4) |
C33 | 0.037 (5) | 0.115 (10) | 0.045 (6) | −0.018 (6) | 0.000 (5) | 0.005 (6) |
C34 | 0.051 (7) | 0.120 (11) | 0.062 (7) | −0.014 (7) | −0.020 (6) | 0.007 (7) |
C35 | 0.034 (5) | 0.061 (6) | 0.076 (8) | 0.006 (5) | −0.002 (5) | −0.015 (6) |
C36 | 0.042 (6) | 0.067 (7) | 0.079 (8) | −0.011 (5) | 0.014 (6) | 0.012 (6) |
C37 | 0.049 (6) | 0.053 (6) | 0.058 (6) | −0.011 (5) | 0.007 (5) | 0.005 (5) |
Os6—C1 | 1.866 (11) | C11—C10 | 1.367 (14) |
Os6—B2 | 2.299 (11) | C11—C10' | 1.382 (18) |
Os6—B7 | 2.300 (12) | C11—C12' | 1.428 (17) |
Os6—B5 | 2.317 (11) | C11—H11A | 0.9400 |
Os6—P1 | 2.357 (2) | C9—C10 | 1.367 (14) |
Os6—P2 | 2.379 (2) | C9—H9A | 0.9400 |
Os6—H56 | 1.51 (8) | C10—H10A | 0.9400 |
Os6—H67 | 1.61 (10) | C12—C13 | 1.381 (13) |
P1—C2 | 1.828 (9) | C12—H12 | 0.9400 |
P1—C8 | 1.829 (9) | C13—H13 | 0.9400 |
P1—C14 | 1.833 (9) | C9'—C10' | 1.389 (18) |
P2—C26 | 1.829 (9) | C9'—H9' | 0.9400 |
P2—C32 | 1.830 (8) | C10'—H10' | 0.9400 |
P2—C20 | 1.837 (9) | C12'—C13' | 1.418 (17) |
O1—C1 | 1.159 (12) | C12'—H12' | 0.9400 |
B1—B10 | 1.69 (2) | C13'—H13' | 0.9400 |
B1—B4 | 1.73 (2) | C14—C15 | 1.361 (13) |
B1—B5 | 1.732 (16) | C14—C19 | 1.400 (13) |
B1—B3 | 1.73 (2) | C15—C16 | 1.400 (14) |
B1—B2 | 1.737 (18) | C15—H15A | 0.9400 |
B1—H1 | 1.28 (11) | C16—C17 | 1.367 (16) |
B2—B3 | 1.749 (19) | C16—H16A | 0.9400 |
B2—B7 | 1.796 (17) | C17—C18 | 1.387 (16) |
B2—B5 | 1.798 (16) | C17—H17A | 0.9400 |
B2—H2 | 1.09 (9) | C18—C19 | 1.366 (14) |
B3—B7 | 1.66 (2) | C18—H18A | 0.9400 |
B3—B8 | 1.76 (2) | C19—H19A | 0.9400 |
B3—B4 | 1.78 (2) | C20—C21 | 1.375 (12) |
B3—H3 | 1.22 (11) | C20—C25 | 1.396 (12) |
B4—B9 | 1.76 (3) | C21—C22 | 1.394 (13) |
B4—B10 | 1.76 (2) | C21—H21A | 0.9400 |
B4—B8 | 1.80 (3) | C22—C23 | 1.366 (14) |
B4—H4 | 1.29 (13) | C22—H22A | 0.9400 |
B5—B10 | 2.026 (19) | C23—C24 | 1.374 (15) |
B5—H5 | 1.11 (9) | C23—H23A | 0.9400 |
B5—H56 | 1.35 (9) | C24—C25 | 1.379 (13) |
B7—B8 | 1.93 (2) | C24—H24A | 0.9400 |
B7—H7 | 1.18 (10) | C25—H25A | 0.9400 |
B7—H67 | 1.52 (10) | C26—C27 | 1.376 (13) |
B8—B9 | 1.76 (2) | C26—C31 | 1.405 (13) |
B8—H8 | 1.3151 | C27—C28 | 1.372 (13) |
B9—B10 | 1.77 (3) | C27—H27A | 0.9400 |
B9—H9 | 1.1933 | C28—C29 | 1.378 (15) |
B10—H10 | 1.14 (13) | C28—H28A | 0.9400 |
C2—C3 | 1.398 (12) | C29—C30 | 1.358 (14) |
C2—C7 | 1.399 (12) | C29—H29A | 0.9400 |
C3—C4 | 1.394 (12) | C30—C31 | 1.392 (13) |
C3—H3A | 0.9400 | C30—H30A | 0.9400 |
C4—C5 | 1.375 (13) | C31—H31A | 0.9400 |
C4—H4A | 0.9400 | C32—C33 | 1.362 (12) |
C5—C6 | 1.386 (13) | C32—C37 | 1.382 (12) |
C5—H5A | 0.9400 | C33—C34 | 1.393 (13) |
C6—C7 | 1.378 (13) | C33—H33A | 0.9400 |
C6—H6A | 0.9400 | C34—C35 | 1.373 (14) |
C7—H7A | 0.9400 | C34—H34A | 0.9400 |
C8—C9 | 1.370 (14) | C35—C36 | 1.346 (14) |
C8—C9' | 1.381 (18) | C35—H35A | 0.9400 |
C8—C13 | 1.395 (12) | C36—C37 | 1.393 (13) |
C8—C13' | 1.403 (17) | C36—H36A | 0.9400 |
C11—C12 | 1.348 (13) | C37—H37A | 0.9400 |
C1—Os6—B2 | 97.7 (4) | B1—B10—B4 | 60.0 (10) |
C1—Os6—B7 | 81.8 (5) | B1—B10—B9 | 108.9 (12) |
B2—Os6—B7 | 46.0 (4) | B4—B10—B9 | 59.7 (10) |
C1—Os6—B5 | 141.3 (4) | B1—B10—B5 | 54.7 (7) |
B2—Os6—B5 | 45.8 (4) | B4—B10—B5 | 108.4 (10) |
B7—Os6—B5 | 78.8 (5) | B9—B10—B5 | 119.5 (12) |
C1—Os6—P1 | 94.0 (3) | B1—B10—H10 | 142 (7) |
B2—Os6—P1 | 155.1 (3) | B4—B10—H10 | 120 (7) |
B7—Os6—P1 | 114.9 (3) | B9—B10—H10 | 99 (7) |
B5—Os6—P1 | 124.5 (3) | B5—B10—H10 | 129 (7) |
C1—Os6—P2 | 90.5 (3) | O1—C1—Os6 | 175.6 (9) |
B2—Os6—P2 | 100.8 (3) | C3—C2—C7 | 117.7 (8) |
B7—Os6—P2 | 143.6 (3) | C3—C2—P1 | 124.4 (7) |
B5—Os6—P2 | 85.8 (3) | C7—C2—P1 | 117.8 (7) |
P1—Os6—P2 | 101.04 (8) | C4—C3—C2 | 120.7 (8) |
C1—Os6—H56 | 175 (3) | C4—C3—H3A | 119.6 |
B2—Os6—H56 | 78 (3) | C2—C3—H3A | 119.6 |
B7—Os6—H56 | 96 (3) | C5—C4—C3 | 120.5 (9) |
B5—Os6—H56 | 34 (3) | C5—C4—H4A | 119.8 |
P1—Os6—H56 | 91 (3) | C3—C4—H4A | 119.8 |
P2—Os6—H56 | 88 (3) | C4—C5—C6 | 119.3 (9) |
C1—Os6—H67 | 95 (3) | C4—C5—H5A | 120.4 |
B2—Os6—H67 | 82 (4) | C6—C5—H5A | 120.4 |
B7—Os6—H67 | 41 (4) | C7—C6—C5 | 120.7 (10) |
B5—Os6—H67 | 92 (3) | C7—C6—H6A | 119.6 |
P1—Os6—H67 | 75 (4) | C5—C6—H6A | 119.6 |
P2—Os6—H67 | 174 (3) | C6—C7—C2 | 121.0 (9) |
H56—Os6—H67 | 87 (5) | C6—C7—H7A | 119.5 |
C2—P1—C8 | 100.5 (4) | C2—C7—H7A | 119.5 |
C2—P1—C14 | 98.2 (4) | C9—C8—C9' | 37.7 (12) |
C8—P1—C14 | 106.4 (4) | C9—C8—C13 | 110.9 (13) |
C2—P1—Os6 | 114.5 (3) | C9'—C8—C13 | 100.5 (14) |
C8—P1—Os6 | 111.0 (3) | C9—C8—C13' | 104.8 (13) |
C14—P1—Os6 | 123.3 (3) | C9'—C8—C13' | 127 (2) |
C26—P2—C32 | 103.2 (4) | C13—C8—C13' | 50.8 (12) |
C26—P2—C20 | 100.8 (4) | C9—C8—P1 | 120.8 (10) |
C32—P2—C20 | 103.5 (4) | C9'—C8—P1 | 115.1 (15) |
C26—P2—Os6 | 116.0 (3) | C13—C8—P1 | 127.8 (9) |
C32—P2—Os6 | 117.3 (3) | C13'—C8—P1 | 117.0 (11) |
C20—P2—Os6 | 113.9 (3) | C12—C11—C10 | 121.9 (15) |
B10—B1—B4 | 62.1 (10) | C12—C11—C10' | 102.8 (18) |
B10—B1—B5 | 72.6 (9) | C10—C11—C10' | 33.9 (13) |
B4—B1—B5 | 125.5 (13) | C12—C11—C12' | 49.1 (15) |
B10—B1—B3 | 110.1 (14) | C10—C11—C12' | 101.3 (15) |
B4—B1—B3 | 61.9 (9) | C10'—C11—C12' | 111 (2) |
B5—B1—B3 | 112.7 (11) | C12—C11—H11A | 119.0 |
B10—B1—B2 | 120.6 (12) | C10—C11—H11A | 119.0 |
B4—B1—B2 | 117.7 (13) | C10'—C11—H11A | 128.9 |
B5—B1—B2 | 62.4 (7) | C12'—C11—H11A | 118.3 |
B3—B1—B2 | 60.5 (8) | C10—C9—C8 | 126.7 (18) |
B10—B1—H1 | 111 (5) | C10—C9—H9A | 116.7 |
B4—B1—H1 | 116 (5) | C8—C9—H9A | 116.7 |
B5—B1—H1 | 107 (5) | C11—C10—C9 | 116.7 (18) |
B3—B1—H1 | 129 (5) | C11—C10—H10A | 121.6 |
B2—B1—H1 | 118 (5) | C9—C10—H10A | 121.6 |
B1—B2—B3 | 59.6 (8) | C11—C12—C13 | 116.2 (14) |
B1—B2—B7 | 102.5 (10) | C11—C12—H12 | 121.9 |
B3—B2—B7 | 56.0 (7) | C13—C12—H12 | 121.9 |
B1—B2—B5 | 58.7 (7) | C12—C13—C8 | 126.3 (13) |
B3—B2—B5 | 108.8 (9) | C12—C13—H13 | 116.8 |
B7—B2—B5 | 109.3 (8) | C8—C13—H13 | 116.8 |
B1—B2—Os6 | 117.6 (8) | C8—C9'—C10' | 117 (3) |
B3—B2—Os6 | 118.0 (7) | C8—C9'—H9' | 121.7 |
B7—B2—Os6 | 67.0 (6) | C10'—C9'—H9' | 121.7 |
B5—B2—Os6 | 67.6 (5) | C11—C10'—C9' | 125 (3) |
B1—B2—H2 | 119 (5) | C11—C10'—H10' | 117.5 |
B3—B2—H2 | 114 (5) | C9'—C10'—H10' | 117.5 |
B7—B2—H2 | 123 (5) | C13'—C12'—C11 | 131 (2) |
B5—B2—H2 | 125 (5) | C13'—C12'—H12' | 114.6 |
Os6—B2—H2 | 116 (5) | C11—C12'—H12' | 114.6 |
B7—B3—B1 | 108.3 (10) | C8—C13'—C12' | 108.4 (18) |
B7—B3—B2 | 63.4 (8) | C8—C13'—H13' | 125.8 |
B1—B3—B2 | 59.8 (8) | C12'—C13'—H13' | 125.8 |
B7—B3—B8 | 68.4 (9) | C15—C14—C19 | 118.0 (9) |
B1—B3—B8 | 106.1 (11) | C15—C14—P1 | 119.3 (7) |
B2—B3—B8 | 118.9 (10) | C19—C14—P1 | 122.7 (8) |
B7—B3—B4 | 118.3 (11) | C14—C15—C16 | 122.2 (10) |
B1—B3—B4 | 58.9 (9) | C14—C15—H15A | 118.9 |
B2—B3—B4 | 114.3 (11) | C16—C15—H15A | 118.9 |
B8—B3—B4 | 61.2 (10) | C17—C16—C15 | 118.5 (11) |
B7—B3—H3 | 114 (5) | C17—C16—H16A | 120.8 |
B1—B3—H3 | 128 (5) | C15—C16—H16A | 120.8 |
B2—B3—H3 | 117 (5) | C16—C17—C18 | 120.3 (10) |
B8—B3—H3 | 116 (5) | C16—C17—H17A | 119.8 |
B4—B3—H3 | 118 (5) | C18—C17—H17A | 119.8 |
B1—B4—B9 | 107.7 (12) | C19—C18—C17 | 120.2 (11) |
B1—B4—B10 | 57.9 (9) | C19—C18—H18A | 119.9 |
B9—B4—B10 | 60.3 (11) | C17—C18—H18A | 119.9 |
B1—B4—B3 | 59.2 (9) | C18—C19—C14 | 120.7 (11) |
B9—B4—B3 | 108.0 (13) | C18—C19—H19A | 119.7 |
B10—B4—B3 | 104.8 (12) | C14—C19—H19A | 119.7 |
B1—B4—B8 | 104.5 (12) | C21—C20—C25 | 118.7 (8) |
B9—B4—B8 | 59.1 (11) | C21—C20—P2 | 123.7 (7) |
B10—B4—B8 | 103.7 (13) | C25—C20—P2 | 117.5 (7) |
B3—B4—B8 | 58.9 (8) | C20—C21—C22 | 121.3 (9) |
B1—B4—H4 | 105 (6) | C20—C21—H21A | 119.3 |
B9—B4—H4 | 139 (6) | C22—C21—H21A | 119.3 |
B10—B4—H4 | 122 (6) | C23—C22—C21 | 119.6 (10) |
B3—B4—H4 | 110 (6) | C23—C22—H22A | 120.2 |
B8—B4—H4 | 134 (6) | C21—C22—H22A | 120.2 |
B1—B5—B2 | 58.9 (7) | C22—C23—C24 | 119.5 (10) |
B1—B5—B10 | 52.8 (8) | C22—C23—H23A | 120.3 |
B2—B5—B10 | 102.1 (8) | C24—C23—H23A | 120.3 |
B1—B5—Os6 | 116.9 (8) | C23—C24—C25 | 121.7 (10) |
B2—B5—Os6 | 66.6 (5) | C23—C24—H24A | 119.2 |
B10—B5—Os6 | 117.8 (8) | C25—C24—H24A | 119.2 |
B1—B5—H5 | 115 (5) | C24—C25—C20 | 119.3 (9) |
B2—B5—H5 | 132 (5) | C24—C25—H25A | 120.4 |
B10—B5—H5 | 109 (5) | C20—C25—H25A | 120.4 |
Os6—B5—H5 | 124 (5) | C27—C26—C31 | 117.1 (9) |
B1—B5—H56 | 133 (4) | C27—C26—P2 | 121.5 (8) |
B2—B5—H56 | 102 (4) | C31—C26—P2 | 121.3 (7) |
B10—B5—H56 | 98 (4) | C28—C27—C26 | 122.2 (10) |
Os6—B5—H56 | 38 (4) | C28—C27—H27A | 118.9 |
H5—B5—H56 | 109 (6) | C26—C27—H27A | 118.9 |
B3—B7—B2 | 60.6 (8) | C27—C28—C29 | 120.3 (11) |
B3—B7—B8 | 58.2 (9) | C27—C28—H28A | 119.9 |
B2—B7—B8 | 108.6 (10) | C29—C28—H28A | 119.9 |
B3—B7—Os6 | 122.0 (9) | C30—C29—C28 | 119.0 (10) |
B2—B7—Os6 | 67.0 (5) | C30—C29—H29A | 120.5 |
B8—B7—Os6 | 124.2 (8) | C28—C29—H29A | 120.5 |
B3—B7—H7 | 109 (5) | C29—C30—C31 | 121.3 (10) |
B2—B7—H7 | 128 (5) | C29—C30—H30A | 119.3 |
B8—B7—H7 | 104 (5) | C31—C30—H30A | 119.3 |
Os6—B7—H7 | 122 (5) | C30—C31—C26 | 120.0 (9) |
B3—B7—H67 | 131 (4) | C30—C31—H31A | 120.0 |
B2—B7—H67 | 104 (4) | C26—C31—H31A | 120.0 |
B8—B7—H67 | 90 (4) | C33—C32—C37 | 118.2 (8) |
Os6—B7—H67 | 44 (4) | C33—C32—P2 | 120.5 (7) |
H7—B7—H67 | 116 (6) | C37—C32—P2 | 121.3 (7) |
B9—B8—B3 | 108.9 (12) | C32—C33—C34 | 121.7 (10) |
B9—B8—B4 | 59.2 (11) | C32—C33—H33A | 119.1 |
B3—B8—B4 | 59.9 (10) | C34—C33—H33A | 119.1 |
B9—B8—B7 | 115.9 (11) | C35—C34—C33 | 119.6 (10) |
B3—B8—B7 | 53.5 (7) | C35—C34—H34A | 120.2 |
B4—B8—B7 | 105.0 (11) | C33—C34—H34A | 120.2 |
B9—B8—H8 | 120.7 | C36—C35—C34 | 118.9 (9) |
B3—B8—H8 | 122.3 | C36—C35—H35A | 120.6 |
B4—B8—H8 | 124.8 | C34—C35—H35A | 120.6 |
B7—B8—H8 | 117.6 | C35—C36—C37 | 122.1 (10) |
B8—B9—B4 | 61.7 (10) | C35—C36—H36A | 119.0 |
B8—B9—B10 | 105.3 (11) | C37—C36—H36A | 119.0 |
B4—B9—B10 | 60.0 (11) | C32—C37—C36 | 119.5 (9) |
B8—B9—H9 | 132.5 | C32—C37—H37A | 120.3 |
B4—B9—H9 | 124.9 | C36—C37—H37A | 120.3 |
B10—B9—H9 | 117.8 |
Experimental details
(I) | (IV) | |
Crystal data | ||
Chemical formula | [(B5H9Os)(C18H15P)2(CO)] | [(B9H13Os)(C18H15P)2(CO)] |
Mr | 805.87 | 853.14 |
Crystal system, space group | Monoclinic, Cc | Monoclinic, P21/n |
Temperature (K) | 153 | 223 |
a, b, c (Å) | 16.0054 (1), 13.0200 (1), 17.2445 (1) | 10.4617 (1), 15.6821 (1), 22.6315 (3) |
β (°) | 105.29 (1) | 91.08 (1) |
V (Å3) | 3466.39 (4) | 3712.29 (7) |
Z | 4 | 4 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 3.80 | 3.55 |
Crystal size (mm) | 0.25 × 0.20 × 0.08 | 0.28 × 0.20 × 0.04 |
Data collection | ||
Diffractometer | Bruker SMART Query CCD area-detector diffractometer | Bruker SMART Query CCD area-detector diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Blessing, 1995) | Empirical (using intensity measurements) (SADABS; Blessing, 1995) |
Tmin, Tmax | 0.450, 0.751 | 0.436, 0.871 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 31883, 9961, 9460 | 74813, 6483, 5001 |
Rint | 0.041 | 0.01 |
(sin θ/λ)max (Å−1) | 0.703 | 0.595 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.026, 0.059, 1.03 | 0.057, 0.116, 1.18 |
No. of reflections | 9961 | 6483 |
No. of parameters | 443 | 491 |
No. of restraints | 2 | 36 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
w = 1/[σ2(Fo2) + (0.0182P)2] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0197P)2 + 26.7668P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 2.20, −1.78 | 1.26, −1.16 |
Absolute structure | Flack, 1983 | ? |
Absolute structure parameter | 0.002 (4) | ? |
Computer programs: SMART (Bruker, 1997), SMART, SAINT (Bruker, 1997), SHELXTL (Sheldrick, 1999), SHELXTL.
Os2—C37 | 1.869 (4) | B1—B6 | 1.777 (7) |
Os2—B3 | 2.291 (4) | B1—B3 | 1.788 (7) |
Os2—B6 | 2.301 (4) | B1—B5 | 1.808 (7) |
Os2—B1 | 2.335 (5) | B1—B4 | 1.809 (8) |
Os2—P2 | 2.3664 (9) | B3—B4 | 1.753 (6) |
Os2—P1 | 2.3729 (11) | B4—B5 | 1.652 (8) |
O—C37 | 1.155 (5) | B5—B6 | 1.730 (6) |
C37—Os2—B3 | 134.42 (15) | B1—Os2—P2 | 152.23 (15) |
C37—Os2—B6 | 80.32 (15) | C37—Os2—P1 | 86.53 (11) |
B3—Os2—B6 | 79.87 (16) | B3—Os2—P1 | 88.02 (11) |
C37—Os2—B1 | 93.31 (17) | B6—Os2—P1 | 146.59 (13) |
B3—Os2—B1 | 45.46 (18) | B1—Os2—P1 | 106.00 (16) |
B6—Os2—B1 | 45.07 (19) | P2—Os2—P1 | 98.46 (3) |
C37—Os2—P2 | 101.22 (11) | B5—B4—B3 | 112.0 (3) |
B3—Os2—P2 | 124.35 (12) | B4—B5—B6 | 111.7 (3) |
B6—Os2—P2 | 114.12 (13) |
Os6—C1 | 1.866 (11) | Os6—P2 | 2.379 (2) |
Os6—B2 | 2.299 (11) | O1—C1 | 1.159 (12) |
Os6—B7 | 2.300 (12) | B5—B10 | 2.026 (19) |
Os6—B5 | 2.317 (11) | B7—B8 | 1.93 (2) |
Os6—P1 | 2.357 (2) | ||
C1—Os6—B2 | 97.7 (4) | C1—Os6—P2 | 90.5 (3) |
C1—Os6—B7 | 81.8 (5) | B2—Os6—P2 | 100.8 (3) |
C1—Os6—P1 | 94.0 (3) | P1—Os6—P2 | 101.04 (8) |
B2—Os6—P1 | 155.1 (3) |
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Several metallahexaboranes, species in which a transition metal moiety has replaced a BH group in hexaborane(10), are known (Kennedy, 1984). So far, however, only the species [(PPh3)2(CO)-nido-OsB5H9], (I) (Bould et al., 1983), and [(PPh3)2(CO)-nido-IrB5H8], (II) (Greenwood et al., 1979), are available in sufficient yields and stability to be useful reagents. These are important systems because the parent hexaborane(10) is not stable at room temperature and is very air sensitive. Although one report of the derivatization of (II) has been reported (Bould, Rath, Fang & Barton, 1996) correct ref?, species (I) is the only metallahexaborane to have been the subject of significant derivative chemistry, including the construction of polymetallaboranes and studies of cluster degradation. Indeed, structures of several derivatives of (I) have been reported (Bould et al., 1991; Barton et al., 1996, 1997), but until recently crystals of appropriate quality of the parent, (II) surely (I)?, were unavailable. Compound (I) was isolated in high yield (85%) from the reaction of Na[B5H8] and [(CO)(PPh3)3HClOs]. Minor products also isolated from the reaction mixture were [(CO)H(PPh3)2-arachno-OsB3H8] (Bould, Rath & Barton, 1996) correct ref? and [(CO)(PPh3)2-nido-OsB4H7(BH2·PPh3)], (III) (Barton et al., 1997). An additional minor reaction by-product was also formed, namely, [(CO)(PPh3)2-nido-OsB9H13], (IV). Herein, we report the structure of the important metallahexaborane starting material, (I), and also of the related osmadecaborane [(CO)(PPh3)2-nido-OsB9H13], (IV), for comparison purposes. \sch
Single-crystal X-ray diffraction analysis confirms the expected pentagonal-based pyramid structure for (I) (Fig. 1) that had been proposed previously from NMR spectrometry (Bould et al., 1983). All cage-bound H atoms were located from the difference map and refined freely in reasonable positions, with the exception of the Os—H—B bridging H atoms, although four bridging H atoms are indicated by NMR spectroscopy and required from electron-counting considerations. The bridging H atoms, which were not located from the difference Fourier syntheses, lie approximately trans to C37 and P1, as indicated by NMR spectroscopy [2J (31P - 1H) (trans) 40 Hz for µH26; Bould et al., 1983].
The short B4—B5 distance of 1.650 (10) Å in (I) compares closely with that in (III) [1.649 (10) Å] and with the basal `single' bond in the parent borane, B6H10 [1.626 (4) Å; Huffman, 1974]. This determination confirms that the B—B bond opposite the Os atom is the unbridged one. The distances B3—B4 and B5—B6 are 1.754 (6) and 1.734 (6) Å, respectively, suggesting hydrogen-bridged B—B bonds, whereas the shorter B4—B5, at 1.626 (4) Å, does not. Thus the bridging H atoms in (I) are symmetrically disposed, in spite of the observation of four separate resonances in the bridging-hydrogen region of the 1H NMR spectrum. The latter is clearly due to the asymmetric disposition of the two PPh3 ligands on Os.
The short B4—B5 distance in (I) implies that the metallaborane species may have some Lewis base character, as has been noted in hexaborane(10) (Solomon & Porter, 1972; Brennan et al., 1973). Some evidence for this has, for example, been adduced in the reaction of (II) with Fe2(CO)9 to yield closo-[B5H4PPh3{Fe(CO)3}{Ir(CO)PPh3}] via an initial [(PPh3)2(CO)IrB5H8{µ(Fe(CO)4)}] intermediate (Bould et al., 1995).
The molecular structure of (IV) is shown in Fig. 2. Again, as with (I), two of the four cage-bound bridging H atoms were not located in the difference map, although they are shown by NMR spectroscopy to be present bridging B9—B8 and B9—B10 (see Experimental). The hydrogen-bridged Os—B distances in (I) and (IV) are comparable: Os2—B3 2.292 (4) and Os2—B6 2.298 (4) Å in (I), and Os6—B5 2.317 (11) and Os6—B7 2.300 (12) Å in (IV). This gives support to the assumption that the two bridging H atoms not located in the X-ray structure are indeed present in (I).
The cluster in (IV) is seen to be a conventional nido-metalladecaborane cage, with the metal vertex in a `prow' position on the open face of the ten-vertex `boat'. The structure of a similar osmadecaborane, [(PMe2Ph)3-nido-OsB9H13], (V), has been previously reported by Beckett et al. (1986). The main variance between the two structures arises from the differing metal ligation sphere. The smaller steric requirement of the PMe2Ph ligand effects a smaller Os—P distance in (III) surely (V)? compared with (IV) (by ca 0.035 (3) Å). The slight difference between the long B5—B10 and B7—B8 distances in (IV) [2.026 (19) and 1.93 (2) Å, respectively], which might be attributed to the asymmetry introduced by the presence of the equatorial carbonyl ligand, is, however, mirrored in (V) [2.083 (11) versus 2.016 (10) Å]. It is noteworthy that the orientations of the ligands on Os in (IV) and (I) are similar and both asymmetrical. Representations of (I), (II) and (IV) are given in the Scheme to illustrate the orientation of the ligands relative to the boron cages in the three systems.