

Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536808019077/ng2467sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536808019077/ng2467Isup2.hkl |
CCDC reference: 696615
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean
(C-C) = 0.003 Å
- R factor = 0.038
- wR factor = 0.106
- Data-to-parameter ratio = 16.5
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 500 Deg.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
A solution of tBu2P–P(SiMe3)Li 1.5 THF (855 mg 3.42 mmol) in 20 ml toluene at -30 °C was dropped to a solution of Ph2PCl (792 mg, 3.59 mmol) in 20 ml toluene. The resulting solution was stirred for 3 h at–30 °C and for 12 h at ambient temp. Then the solvent was removed under vacuum at 1 mTorr for 1 h, the residue dissolved in pentane (40 ml), filtered and concentrated to about 8 ml. After 6 days at -35 oC the solution yielded 688 mg of colourless crystals of (Ph2P)2P(PtBu2) (1).
31P{1H} NMR of (Ph2P1,2)2P3(P4tBu2) (1) (Bruker Av400, C6D6, 298 K, external standard 85% H3PO4)(δ p.p.m.) 37.9 dt, P4; -19.5 dd*, P1, P2; -62.3 dt*, P3. 1J(P3—P4) =–410.7 Hz, 1J(P1—P3) = -253.3 Hz, 2J(P1—P4) = +33.9 Hz (*= multiplet of higher order).
Chemical shifts and coupling constants of (1) were optimized using Bruke software (Bruker 1999, Hägele et al. 1987).
All H atoms were refined as riding on C atoms with aromatic C—H = 0.95 Å, methyl C—H = 0.98 Å, and Uiso(H) = 1.2Ueq(C) for CH groups, 1.5Ueq(C) for CH3 groups.
Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED (Oxford Diffraction, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
C32H38P4 | Z = 2 |
Mr = 546.5 | F(000) = 580 |
Triclinic, P1 | Dx = 1.232 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.0161 (6) Å | Cell parameters from 6775 reflections |
b = 11.9258 (7) Å | θ = 2.4–32.4° |
c = 12.9951 (7) Å | µ = 0.28 mm−1 |
α = 104.831 (5)° | T = 120 K |
β = 100.201 (5)° | Prism, colourless |
γ = 90.900 (5)° | 0.32 × 0.15 × 0.13 mm |
V = 1473.79 (15) Å3 |
Oxford DiffractionKM-4-CCD diffractometer | 4356 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
Detector resolution: 8.1883 pixels mm-1 | θmax = 25.5°, θmin = 2.4° |
0.75° wide ω scans | h = −11→12 |
10351 measured reflections | k = −14→13 |
5474 independent reflections | l = −15→14 |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.106 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0689P)2] where P = (Fo2 + 2Fc2)/3 |
5474 reflections | (Δ/σ)max < 0.001 |
331 parameters | Δρmax = 0.45 e Å−3 |
0 restraints | Δρmin = −0.30 e Å−3 |
C32H38P4 | γ = 90.900 (5)° |
Mr = 546.5 | V = 1473.79 (15) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.0161 (6) Å | Mo Kα radiation |
b = 11.9258 (7) Å | µ = 0.28 mm−1 |
c = 12.9951 (7) Å | T = 120 K |
α = 104.831 (5)° | 0.32 × 0.15 × 0.13 mm |
β = 100.201 (5)° |
Oxford DiffractionKM-4-CCD diffractometer | 4356 reflections with I > 2σ(I) |
10351 measured reflections | Rint = 0.023 |
5474 independent reflections |
R[F2 > 2σ(F2)] = 0.038 | 0 restraints |
wR(F2) = 0.106 | H-atom parameters constrained |
S = 1.07 | Δρmax = 0.45 e Å−3 |
5474 reflections | Δρmin = −0.30 e Å−3 |
331 parameters |
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 > σ(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 | ||
C1 | −0.05525 (19) | 0.27686 (16) | 0.36738 (15) | 0.0197 (4) | |
C2 | −0.10603 (19) | 0.16151 (17) | 0.33015 (16) | 0.0223 (4) | |
H2 | −0.0706 | 0.11 | 0.2741 | 0.027* | |
C3 | −0.2075 (2) | 0.12062 (18) | 0.37356 (17) | 0.0267 (5) | |
H3 | −0.2412 | 0.0416 | 0.347 | 0.032* | |
C4 | −0.2601 (2) | 0.19420 (19) | 0.45549 (17) | 0.0299 (5) | |
H4 | −0.3292 | 0.1659 | 0.4857 | 0.036* | |
C5 | −0.2118 (2) | 0.3082 (2) | 0.49266 (18) | 0.0354 (5) | |
H5 | −0.2479 | 0.3592 | 0.5486 | 0.042* | |
C6 | −0.1106 (2) | 0.34949 (18) | 0.44923 (17) | 0.0288 (5) | |
H6 | −0.0783 | 0.4288 | 0.4757 | 0.035* | |
C7 | −0.03069 (19) | 0.37273 (17) | 0.19424 (16) | 0.0222 (4) | |
C8 | −0.0180 (2) | 0.48242 (19) | 0.17833 (18) | 0.0325 (5) | |
H8 | 0.0439 | 0.5402 | 0.2289 | 0.039* | |
C9 | −0.0951 (3) | 0.5082 (2) | 0.0890 (2) | 0.0446 (7) | |
H9 | −0.0871 | 0.5841 | 0.0792 | 0.054* | |
C10 | −0.1834 (3) | 0.4244 (2) | 0.0143 (2) | 0.0431 (6) | |
H10 | −0.2353 | 0.4423 | −0.0474 | 0.052* | |
C11 | −0.1966 (2) | 0.3146 (2) | 0.02890 (18) | 0.0368 (6) | |
H11 | −0.2575 | 0.2569 | −0.0227 | 0.044* | |
C12 | −0.1212 (2) | 0.28863 (19) | 0.11857 (17) | 0.0278 (5) | |
H12 | −0.1309 | 0.2131 | 0.1288 | 0.033* | |
C13 | 0.24915 (19) | 0.19694 (17) | 0.47598 (16) | 0.0214 (4) | |
C14 | 0.2700 (2) | 0.31269 (17) | 0.53800 (16) | 0.0258 (5) | |
H14 | 0.3222 | 0.3667 | 0.5163 | 0.031* | |
C15 | 0.2149 (2) | 0.34903 (18) | 0.63082 (18) | 0.0297 (5) | |
H15 | 0.2286 | 0.428 | 0.6719 | 0.036* | |
C16 | 0.1403 (2) | 0.27079 (19) | 0.66379 (17) | 0.0313 (5) | |
H16 | 0.1035 | 0.2958 | 0.7278 | 0.038* | |
C17 | 0.1193 (2) | 0.15651 (19) | 0.60370 (18) | 0.0313 (5) | |
H17 | 0.0675 | 0.103 | 0.6263 | 0.038* | |
C18 | 0.1735 (2) | 0.11927 (18) | 0.51040 (17) | 0.0260 (5) | |
H18 | 0.1588 | 0.0402 | 0.4697 | 0.031* | |
C19 | 0.3207 (2) | −0.00176 (16) | 0.32067 (15) | 0.0206 (4) | |
C20 | 0.2027 (2) | −0.07357 (17) | 0.27282 (16) | 0.0253 (4) | |
H20 | 0.1186 | −0.0399 | 0.2577 | 0.03* | |
C21 | 0.2071 (2) | −0.19302 (18) | 0.24733 (17) | 0.0291 (5) | |
H21 | 0.126 | −0.2409 | 0.2153 | 0.035* | |
C22 | 0.3292 (2) | −0.24324 (19) | 0.26830 (17) | 0.0317 (5) | |
H22 | 0.3317 | −0.3255 | 0.251 | 0.038* | |
C23 | 0.4468 (2) | −0.17404 (19) | 0.31416 (18) | 0.0334 (5) | |
H23 | 0.5308 | −0.2084 | 0.3279 | 0.04* | |
C24 | 0.4427 (2) | −0.05407 (18) | 0.34036 (16) | 0.0269 (5) | |
H24 | 0.5242 | −0.0068 | 0.3722 | 0.032* | |
C25 | 0.4464 (2) | 0.34098 (17) | 0.19073 (17) | 0.0241 (4) | |
C26 | 0.4359 (2) | 0.42053 (18) | 0.30219 (18) | 0.0300 (5) | |
H26A | 0.5207 | 0.469 | 0.3328 | 0.045* | |
H26B | 0.4204 | 0.3729 | 0.3508 | 0.045* | |
H26C | 0.36 | 0.4703 | 0.2941 | 0.045* | |
C27 | 0.5567 (2) | 0.25572 (19) | 0.20422 (18) | 0.0280 (5) | |
H27A | 0.5694 | 0.2103 | 0.1327 | 0.042* | |
H27B | 0.529 | 0.2032 | 0.2447 | 0.042* | |
H27C | 0.6423 | 0.299 | 0.2439 | 0.042* | |
C28 | 0.4878 (2) | 0.41895 (19) | 0.1227 (2) | 0.0334 (5) | |
H28A | 0.4212 | 0.4777 | 0.1184 | 0.05* | |
H28B | 0.4908 | 0.3714 | 0.0496 | 0.05* | |
H28C | 0.5778 | 0.4575 | 0.1567 | 0.05* | |
C29 | 0.2723 (2) | 0.14372 (18) | 0.00756 (16) | 0.0277 (5) | |
C30 | 0.3239 (2) | 0.03535 (18) | 0.04003 (18) | 0.0333 (5) | |
H30A | 0.267 | 0.014 | 0.087 | 0.05* | |
H30B | 0.4181 | 0.0515 | 0.0791 | 0.05* | |
H30C | 0.3196 | −0.0289 | −0.0251 | 0.05* | |
C31 | 0.3551 (2) | 0.1739 (2) | −0.07156 (18) | 0.0383 (6) | |
H31A | 0.3423 | 0.1103 | −0.138 | 0.058* | |
H31B | 0.4516 | 0.1854 | −0.0379 | 0.058* | |
H31C | 0.3242 | 0.2455 | −0.0893 | 0.058* | |
C32 | 0.1237 (2) | 0.1177 (2) | −0.05120 (19) | 0.0367 (5) | |
H32A | 0.1174 | 0.0502 | −0.1139 | 0.055* | |
H32B | 0.091 | 0.1852 | −0.0757 | 0.055* | |
H32C | 0.0678 | 0.1009 | −0.0015 | 0.055* | |
P1 | 0.07579 (5) | 0.34576 (4) | 0.31567 (4) | 0.01952 (13) | |
P2 | 0.33268 (5) | 0.15796 (4) | 0.35823 (4) | 0.02017 (14) | |
P3 | 0.17163 (5) | 0.19161 (4) | 0.22775 (4) | 0.01832 (13) | |
P4 | 0.26732 (5) | 0.27752 (4) | 0.12351 (4) | 0.02045 (14) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0156 (9) | 0.0236 (10) | 0.0209 (10) | 0.0015 (8) | 0.0024 (8) | 0.0079 (8) |
C2 | 0.0207 (10) | 0.0228 (10) | 0.0249 (10) | 0.0040 (8) | 0.0074 (8) | 0.0069 (8) |
C3 | 0.0237 (11) | 0.0252 (11) | 0.0326 (12) | −0.0018 (9) | 0.0030 (9) | 0.0117 (9) |
C4 | 0.0218 (11) | 0.0421 (13) | 0.0278 (11) | −0.0058 (10) | 0.0057 (9) | 0.0126 (10) |
C5 | 0.0308 (12) | 0.0417 (13) | 0.0296 (12) | −0.0043 (10) | 0.0124 (10) | −0.0021 (10) |
C6 | 0.0249 (11) | 0.0296 (12) | 0.0279 (11) | −0.0054 (9) | 0.0081 (9) | −0.0011 (9) |
C7 | 0.0197 (10) | 0.0263 (11) | 0.0252 (11) | 0.0094 (8) | 0.0118 (8) | 0.0093 (8) |
C8 | 0.0415 (13) | 0.0272 (12) | 0.0341 (12) | 0.0122 (10) | 0.0153 (10) | 0.0115 (10) |
C9 | 0.0699 (19) | 0.0379 (14) | 0.0377 (14) | 0.0269 (13) | 0.0232 (14) | 0.0204 (11) |
C10 | 0.0430 (14) | 0.0630 (17) | 0.0331 (13) | 0.0277 (13) | 0.0118 (11) | 0.0257 (13) |
C11 | 0.0233 (11) | 0.0606 (16) | 0.0294 (12) | 0.0093 (11) | 0.0081 (10) | 0.0145 (11) |
C12 | 0.0197 (10) | 0.0381 (12) | 0.0294 (11) | 0.0035 (9) | 0.0071 (9) | 0.0140 (9) |
C13 | 0.0172 (9) | 0.0241 (10) | 0.0224 (10) | 0.0036 (8) | 0.0008 (8) | 0.0068 (8) |
C14 | 0.0235 (10) | 0.0244 (11) | 0.0268 (11) | −0.0003 (9) | −0.0014 (9) | 0.0062 (9) |
C15 | 0.0304 (11) | 0.0241 (11) | 0.0299 (11) | 0.0056 (9) | 0.0012 (9) | 0.0013 (9) |
C16 | 0.0343 (12) | 0.0359 (13) | 0.0251 (11) | 0.0107 (10) | 0.0097 (10) | 0.0072 (9) |
C17 | 0.0331 (12) | 0.0313 (12) | 0.0337 (12) | 0.0045 (10) | 0.0128 (10) | 0.0115 (10) |
C18 | 0.0285 (11) | 0.0234 (10) | 0.0255 (11) | 0.0018 (9) | 0.0046 (9) | 0.0057 (8) |
C19 | 0.0219 (10) | 0.0215 (10) | 0.0206 (10) | 0.0048 (8) | 0.0062 (8) | 0.0080 (8) |
C20 | 0.0234 (10) | 0.0248 (11) | 0.0294 (11) | 0.0037 (8) | 0.0063 (9) | 0.0087 (9) |
C21 | 0.0339 (12) | 0.0244 (11) | 0.0293 (11) | −0.0002 (9) | 0.0068 (10) | 0.0072 (9) |
C22 | 0.0490 (14) | 0.0218 (11) | 0.0259 (11) | 0.0116 (10) | 0.0095 (10) | 0.0070 (9) |
C23 | 0.0366 (13) | 0.0332 (12) | 0.0315 (12) | 0.0180 (10) | 0.0062 (10) | 0.0100 (10) |
C24 | 0.0245 (11) | 0.0298 (11) | 0.0260 (11) | 0.0054 (9) | 0.0039 (9) | 0.0070 (9) |
C25 | 0.0176 (10) | 0.0260 (11) | 0.0313 (11) | 0.0001 (8) | 0.0060 (8) | 0.0112 (9) |
C26 | 0.0274 (11) | 0.0248 (11) | 0.0360 (12) | −0.0062 (9) | 0.0071 (10) | 0.0046 (9) |
C27 | 0.0171 (10) | 0.0351 (12) | 0.0346 (12) | 0.0035 (9) | 0.0054 (9) | 0.0138 (9) |
C28 | 0.0248 (11) | 0.0353 (13) | 0.0473 (14) | 0.0004 (9) | 0.0126 (10) | 0.0196 (11) |
C29 | 0.0271 (11) | 0.0330 (12) | 0.0227 (11) | 0.0047 (9) | 0.0073 (9) | 0.0048 (9) |
C30 | 0.0362 (13) | 0.0275 (11) | 0.0338 (12) | 0.0067 (10) | 0.0133 (10) | −0.0010 (9) |
C31 | 0.0382 (13) | 0.0515 (15) | 0.0263 (12) | 0.0066 (11) | 0.0125 (10) | 0.0074 (10) |
C32 | 0.0332 (12) | 0.0413 (14) | 0.0287 (12) | −0.0010 (11) | 0.0000 (10) | 0.0009 (10) |
P1 | 0.0169 (3) | 0.0182 (3) | 0.0239 (3) | 0.00124 (19) | 0.0052 (2) | 0.0054 (2) |
P2 | 0.0165 (3) | 0.0201 (3) | 0.0244 (3) | 0.0010 (2) | 0.0029 (2) | 0.0074 (2) |
P3 | 0.0153 (2) | 0.0183 (3) | 0.0219 (3) | 0.00182 (19) | 0.0037 (2) | 0.0060 (2) |
P4 | 0.0165 (3) | 0.0232 (3) | 0.0239 (3) | 0.0039 (2) | 0.0057 (2) | 0.0088 (2) |
C1—C2 | 1.391 (3) | C20—C21 | 1.381 (3) |
C1—C6 | 1.393 (3) | C20—H20 | 0.95 |
C1—P1 | 1.847 (2) | C21—C22 | 1.385 (3) |
C2—C3 | 1.385 (3) | C21—H21 | 0.95 |
C2—H2 | 0.95 | C22—C23 | 1.376 (3) |
C3—C4 | 1.384 (3) | C22—H22 | 0.95 |
C3—H3 | 0.95 | C23—C24 | 1.386 (3) |
C4—C5 | 1.369 (3) | C23—H23 | 0.95 |
C4—H4 | 0.95 | C24—H24 | 0.95 |
C5—C6 | 1.385 (3) | C25—C27 | 1.530 (3) |
C5—H5 | 0.95 | C25—C26 | 1.537 (3) |
C6—H6 | 0.95 | C25—C28 | 1.535 (3) |
C7—C8 | 1.383 (3) | C25—P4 | 1.902 (2) |
C7—C12 | 1.395 (3) | C26—H26A | 0.98 |
C7—P1 | 1.845 (2) | C26—H26B | 0.98 |
C8—C9 | 1.382 (3) | C26—H26C | 0.98 |
C8—H8 | 0.95 | C27—H27A | 0.98 |
C9—C10 | 1.376 (4) | C27—H27B | 0.98 |
C9—H9 | 0.95 | C27—H27C | 0.98 |
C10—C11 | 1.378 (4) | C28—H28A | 0.98 |
C10—H10 | 0.95 | C28—H28B | 0.98 |
C11—C12 | 1.380 (3) | C28—H28C | 0.98 |
C11—H11 | 0.95 | C29—C30 | 1.529 (3) |
C12—H12 | 0.95 | C29—C31 | 1.535 (3) |
C13—C18 | 1.394 (3) | C29—C32 | 1.535 (3) |
C13—C14 | 1.400 (3) | C29—P4 | 1.902 (2) |
C13—P2 | 1.833 (2) | C30—H30A | 0.98 |
C14—C15 | 1.387 (3) | C30—H30B | 0.98 |
C14—H14 | 0.95 | C30—H30C | 0.98 |
C15—C16 | 1.382 (3) | C31—H31A | 0.98 |
C15—H15 | 0.95 | C31—H31B | 0.98 |
C16—C17 | 1.378 (3) | C31—H31C | 0.98 |
C16—H16 | 0.95 | C32—H32A | 0.98 |
C17—C18 | 1.388 (3) | C32—H32B | 0.98 |
C17—H17 | 0.95 | C32—H32C | 0.98 |
C18—H18 | 0.95 | P1—P3 | 2.2305 (7) |
C19—C24 | 1.394 (3) | P2—P3 | 2.2446 (7) |
C19—C20 | 1.397 (3) | P3—P4 | 2.2231 (7) |
C19—P2 | 1.838 (2) | ||
C2—C1—C6 | 117.64 (18) | C22—C23—C24 | 119.9 (2) |
C2—C1—P1 | 126.30 (15) | C22—C23—H23 | 120 |
C6—C1—P1 | 116.03 (15) | C24—C23—H23 | 120 |
C3—C2—C1 | 120.96 (18) | C23—C24—C19 | 121.0 (2) |
C3—C2—H2 | 119.5 | C23—C24—H24 | 119.5 |
C1—C2—H2 | 119.5 | C19—C24—H24 | 119.5 |
C2—C3—C4 | 120.36 (19) | C27—C25—C26 | 109.64 (17) |
C2—C3—H3 | 119.8 | C27—C25—C28 | 108.98 (17) |
C4—C3—H3 | 119.8 | C26—C25—C28 | 107.24 (17) |
C5—C4—C3 | 119.4 (2) | C27—C25—P4 | 117.57 (14) |
C5—C4—H4 | 120.3 | C26—C25—P4 | 106.54 (13) |
C3—C4—H4 | 120.3 | C28—C25—P4 | 106.38 (14) |
C4—C5—C6 | 120.4 (2) | C25—C26—H26A | 109.5 |
C4—C5—H5 | 119.8 | C25—C26—H26B | 109.5 |
C6—C5—H5 | 119.8 | H26A—C26—H26B | 109.5 |
C5—C6—C1 | 121.2 (2) | C25—C26—H26C | 109.5 |
C5—C6—H6 | 119.4 | H26A—C26—H26C | 109.5 |
C1—C6—H6 | 119.4 | H26B—C26—H26C | 109.5 |
C8—C7—C12 | 119.11 (19) | C25—C27—H27A | 109.5 |
C8—C7—P1 | 117.40 (16) | C25—C27—H27B | 109.5 |
C12—C7—P1 | 123.49 (15) | H27A—C27—H27B | 109.5 |
C9—C8—C7 | 120.2 (2) | C25—C27—H27C | 109.5 |
C9—C8—H8 | 119.9 | H27A—C27—H27C | 109.5 |
C7—C8—H8 | 119.9 | H27B—C27—H27C | 109.5 |
C10—C9—C8 | 120.3 (2) | C25—C28—H28A | 109.5 |
C10—C9—H9 | 119.8 | C25—C28—H28B | 109.5 |
C8—C9—H9 | 119.8 | H28A—C28—H28B | 109.5 |
C9—C10—C11 | 120.1 (2) | C25—C28—H28C | 109.5 |
C9—C10—H10 | 120 | H28A—C28—H28C | 109.5 |
C11—C10—H10 | 120 | H28B—C28—H28C | 109.5 |
C10—C11—C12 | 120.0 (2) | C30—C29—C31 | 110.04 (18) |
C10—C11—H11 | 120 | C30—C29—C32 | 108.77 (18) |
C12—C11—H11 | 120 | C31—C29—C32 | 107.76 (18) |
C11—C12—C7 | 120.3 (2) | C30—C29—P4 | 115.98 (14) |
C11—C12—H12 | 119.8 | C31—C29—P4 | 109.73 (15) |
C7—C12—H12 | 119.8 | C32—C29—P4 | 104.12 (14) |
C18—C13—C14 | 118.53 (19) | C29—C30—H30A | 109.5 |
C18—C13—P2 | 124.94 (15) | C29—C30—H30B | 109.5 |
C14—C13—P2 | 116.45 (15) | H30A—C30—H30B | 109.5 |
C15—C14—C13 | 120.47 (19) | C29—C30—H30C | 109.5 |
C15—C14—H14 | 119.8 | H30A—C30—H30C | 109.5 |
C13—C14—H14 | 119.8 | H30B—C30—H30C | 109.5 |
C16—C15—C14 | 120.2 (2) | C29—C31—H31A | 109.5 |
C16—C15—H15 | 119.9 | C29—C31—H31B | 109.5 |
C14—C15—H15 | 119.9 | H31A—C31—H31B | 109.5 |
C17—C16—C15 | 120.0 (2) | C29—C31—H31C | 109.5 |
C17—C16—H16 | 120 | H31A—C31—H31C | 109.5 |
C15—C16—H16 | 120 | H31B—C31—H31C | 109.5 |
C16—C17—C18 | 120.3 (2) | C29—C32—H32A | 109.5 |
C16—C17—H17 | 119.8 | C29—C32—H32B | 109.5 |
C18—C17—H17 | 119.8 | H32A—C32—H32B | 109.5 |
C17—C18—C13 | 120.51 (19) | C29—C32—H32C | 109.5 |
C17—C18—H18 | 119.7 | H32A—C32—H32C | 109.5 |
C13—C18—H18 | 119.7 | H32B—C32—H32C | 109.5 |
C24—C19—C20 | 118.16 (18) | C7—P1—C1 | 99.44 (9) |
C24—C19—P2 | 115.67 (15) | C7—P1—P3 | 96.19 (6) |
C20—C19—P2 | 126.16 (15) | C1—P1—P3 | 101.86 (6) |
C21—C20—C19 | 120.70 (19) | C13—P2—C19 | 103.58 (9) |
C21—C20—H20 | 119.7 | C13—P2—P3 | 101.37 (6) |
C19—C20—H20 | 119.7 | C19—P2—P3 | 100.37 (6) |
C20—C21—C22 | 120.2 (2) | P4—P3—P1 | 97.92 (3) |
C20—C21—H21 | 119.9 | P4—P3—P2 | 109.51 (3) |
C22—C21—H21 | 119.9 | P1—P3—P2 | 102.93 (3) |
C23—C22—C21 | 119.98 (19) | C25—P4—C29 | 110.55 (9) |
C23—C22—H22 | 120 | C25—P4—P3 | 112.04 (7) |
C21—C22—H22 | 120 | C29—P4—P3 | 97.98 (7) |
Experimental details
Crystal data | |
Chemical formula | C32H38P4 |
Mr | 546.5 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 120 |
a, b, c (Å) | 10.0161 (6), 11.9258 (7), 12.9951 (7) |
α, β, γ (°) | 104.831 (5), 100.201 (5), 90.900 (5) |
V (Å3) | 1473.79 (15) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.28 |
Crystal size (mm) | 0.32 × 0.15 × 0.13 |
Data collection | |
Diffractometer | Oxford DiffractionKM-4-CCD diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10351, 5474, 4356 |
Rint | 0.023 |
(sin θ/λ)max (Å−1) | 0.606 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.038, 0.106, 1.07 |
No. of reflections | 5474 |
No. of parameters | 331 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.45, −0.30 |
Computer programs: CrysAlis CCD (Oxford Diffraction, 2006), CrysAlis RED (Oxford Diffraction, 2006), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).
The reaction of Ph2PCl with tBu2P–P(SiMe3)Li 1.5 THF in toluene at -30 °C (Kovacs et al. 1996) yielded unexpectedly (Ph2P)2P(PtBu2) (1) in the place of expected Ph2P–P(SiMe3)–PtBu2.
The molecular structure of (1) is shown in Fig.1. The geometry around P3 atom in (1) is pyramidal, the sum of angles around P3 is 310.26 degrees. The geometry around P1 atom indicates more pyramidal character (the sum of angles is 297.49 degrees) than around P3. The geometry around P4 atom is more planar (the sum of angles is 320.58 degrees) than around P3. The P–P distances (2.2327 Å - mean value) clearly indicate a single bond character of these bonds. The tendency of phosphane to planarity is more visible for compounds with big groups attached to the central P atom. This assumption is strongly supported by the planar geometry around the central P atom in (tBu2P)3P. This planarity is accompanied by a significant shortening of the P–P distances (2.198 Å) (Fritz et al. 1987).