Literature DB >> 22807752

Bis[N,N-bis-(diphenyl-phosphan-yl)cyclo-penta-namine-κ²P,P']platinum(II) bis-(trifluoro-methane-sulfonate).

Ilana Engelbrecht1, Hendrik G Visser, Andreas Roodt.   

Abstract

The title compound, [Pt(C₂₉H₂₉NP₂)₂](CF₃SO₃)₂, consists of a Pt(II) atom, situated on an inversion centre, coordinated by two diphosphinoamine bidentate ligands and charge-balanced by two trifluoro-methane-sulfonate anions. The Pt(II) atom has a distorted square-planar geometry defined by the four P atoms. The distortion is illustrated by the P-Pt-P bite angle of 70.31 (4)°. The geometry around the N atom deviates from a trigonal-planar geometry, evidenced by the P-N-P bite angle of 102.3 (2) °. The N atom is displaced by 0.114 (4) Å from the C/P/P plane. In order to coordinate, the orientation of the phenyl rings alters from a C(s) conformation to a C(2v) conformation. The cyclo-pentane ring is slightly twisted: the puckering parameters are q(2) = 0.420 (5) Å and ϕ = 26.5 (8) °. The trifluoro-methane-sulfonate anion displays a 0.511 (11):0.489 (11) positional disorder. Weak inter- and intra-molecular C-H⋯O hydrogen bonds influence the crystal packing.

Entities:  

Year:  2012        PMID： 22807752      PMCID： PMC3393184          DOI： 10.1107/S1600536812026359

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For related platinum(II) complexes, see: Farrar & Browning (1995 ▶); Dyson et al. (2004 ▶); Cloete et al. (2010 ▶); Engelbrecht et al. (2010 ▶). For diphosphinoamine (PNP) and other P-donor ligands, see: Keat et al. (1981 ▶); Purcell et al. (1995 ▶); Cotton et al. (1996 ▶); Otto & Roodt (2001 ▶); Fei et al. (2003 ▶); Otto et al. (2005 ▶); Muller et al. (2008 ▶); Engelbrecht et al. (2010 ▶, 2011 ▶). For their use in catalytic olefin transformation reactions, see: Haumann et al. (2004 ▶); Crous et al. (2005 ▶); Booyens et al. (2007 ▶); Ferreira et al. (2007 ▶). For puckering parameters, see: Cremer & Pople (1975 ▶).

Experimental

Crystal data

[Pt(C29H29NP2)2](CF3SO3)2 M = 1400.18 Monoclinic, a = 10.041 (5) Å b = 13.662 (4) Å c = 20.928 (5) Å β = 93.916 (5)° V = 2864.2 (19) Å3 Z = 2 Mo Kα radiation μ = 2.71 mm−1 T = 100 K 0.19 × 0.18 × 0.16 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2008 ▶) T min = 0.627, T max = 0.671 44370 measured reflections 6894 independent reflections 4869 reflections with I > 2σ(I) R int = 0.101

Refinement

R[F 2 > 2σ(F 2)] = 0.040 wR(F 2) = 0.093 S = 1.02 6894 reflections 398 parameters 7 restraints H-atom parameters constrained Δρmax = 1.39 e Å−3 Δρmin = −1.42 e Å−3 Data collection: APEX2 (Bruker, 2011 ▶); cell refinement: SAINT-Plus (Bruker, 2008 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg & Putz, 2005 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶). Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812026359/zb2023sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812026359/zb2023Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Pt(C29H29NP2)2](CF3SO3)2F(000) = 1408
Mr = 1400.18Dx = 1.624 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9870 reflections
a = 10.041 (5) Åθ = 2.8–28.1°
b = 13.662 (4) ŵ = 2.71 mm−1
c = 20.928 (5) ÅT = 100 K
β = 93.916 (5)°Cuboid, colourless
V = 2864.2 (19) Å30.19 × 0.18 × 0.16 mm
Z = 2
Bruker APEXII CCD diffractometer4869 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.101
φ and ω scansθmax = 28°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2008)h = −12→13
Tmin = 0.627, Tmax = 0.671k = −18→18
44370 measured reflectionsl = −27→27
6894 independent reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.093H-atom parameters constrained
S = 1.02w = 1/[σ2(Fo2) + (0.0387P)2 + 0.8274P] where P = (Fo2 + 2Fc2)/3
6894 reflections(Δ/σ)max = 0.001
398 parametersΔρmax = 1.39 e Å−3
7 restraintsΔρmin = −1.42 e Å−3
Experimental. The intensity data were collected on a Bruker X8 ApexII 4 K Kappa CCD diffractometer using an exposure time of 20 s/frame. A total of 1880 frames were collected with a frame width of 0.5° covering up to θ = 28.0° with 99.8% completeness accomplished.Spectroscopy data: 1H NMR (600 MHz, CD2Cl2): δ = 1.0 (m, 4H), 1.1 (m, 4H), 1.2 (m, 4H), 1.4 (m, 4H), 3.5 (m, 2H), 7.4 – 7.8 (m, 40H). 31P NMR (243 MHz, CD2Cl2): δ = 39.7 (t, 1JPt—P = 1063.0 Hz).
Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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.
xyzUiso*/UeqOcc. (<1)
C11.0762 (4)0.3164 (3)0.9779 (2)0.0230 (10)
H11.01690.34871.00810.028*
C21.2188 (5)0.3463 (3)0.9988 (2)0.0306 (11)
H2A1.28460.3090.97540.037*
H2B1.2380.33711.04550.037*
C31.2184 (6)0.4555 (4)0.9805 (2)0.0382 (12)
H3A1.17920.49571.01380.046*
H3B1.31020.47890.97480.046*
C41.1334 (6)0.4606 (4)0.9179 (3)0.0395 (13)
H4A1.19090.46540.88140.047*
H4B1.07480.51890.91740.047*
C51.0489 (5)0.3669 (3)0.9123 (2)0.0261 (10)
H5A1.07690.32470.87720.031*
H5B0.9530.38270.90440.031*
C111.2563 (4)0.1091 (3)0.91477 (19)0.0207 (9)
C121.3335 (5)0.0312 (3)0.9382 (2)0.0264 (10)
H121.2961−0.0170.96440.032*
C131.4666 (5)0.0238 (4)0.9232 (2)0.0330 (12)
H131.5186−0.03110.93740.04*
C141.5222 (5)0.0964 (4)0.8878 (2)0.0297 (11)
H141.61390.09250.87950.036*
C151.4480 (5)0.1736 (4)0.8645 (2)0.0316 (11)
H151.48760.22290.84010.038*
C161.3142 (5)0.1796 (3)0.8768 (2)0.0264 (10)
H161.26130.2320.85930.032*
C210.9925 (4)0.1201 (3)0.85355 (19)0.0201 (9)
C221.0380 (4)0.0582 (3)0.8056 (2)0.0236 (10)
H221.11940.02320.81270.028*
C230.9622 (5)0.0492 (4)0.7479 (2)0.0272 (10)
H230.99110.00730.71530.033*
C240.8444 (5)0.1013 (3)0.7378 (2)0.0265 (10)
H240.79260.09460.69830.032*
C250.8016 (5)0.1625 (3)0.7842 (2)0.0263 (10)
H250.72150.19890.77630.032*
C260.8746 (4)0.1713 (3)0.8424 (2)0.0222 (10)
H260.84360.21270.87470.027*
C311.1077 (4)0.1741 (3)1.11284 (19)0.0208 (9)
C321.2084 (5)0.1038 (3)1.1270 (2)0.0263 (10)
H321.20980.04521.10260.032*
C331.3044 (5)0.1194 (4)1.1758 (2)0.0317 (11)
H331.37130.07161.18570.038*
C341.3027 (5)0.2060 (4)1.2107 (2)0.0346 (12)
H341.370.21731.2440.042*
C351.2052 (5)0.2756 (4)1.1978 (2)0.0364 (12)
H351.20530.33441.22210.044*
C361.1069 (5)0.2591 (4)1.1491 (2)0.0302 (11)
H361.03860.30631.14050.036*
C410.8337 (4)0.2049 (3)1.0621 (2)0.0209 (9)
C420.7533 (5)0.2500 (3)1.0139 (2)0.0267 (10)
H420.78720.26250.97340.032*
C430.6244 (5)0.2764 (4)1.0250 (2)0.0324 (11)
H430.570.30770.99220.039*
C440.5735 (5)0.2576 (4)1.0840 (2)0.0326 (12)
H440.48370.27421.09090.039*
C450.6538 (5)0.2148 (4)1.1327 (2)0.0306 (11)
H450.61980.20391.17330.037*
C460.7842 (5)0.1876 (3)1.1222 (2)0.0262 (10)
H460.83920.15771.15540.031*
N11.0451 (3)0.2102 (3)0.97884 (16)0.0190 (8)
P11.08226 (11)0.11427 (8)0.93121 (5)0.01603 (7)
P20.99258 (11)0.15296 (8)1.04487 (5)0.01603 (7)
Pt11010.01603 (7)
O1A0.6874 (3)0.3547 (3)0.87585 (18)0.0410 (9)0.511 (11)
S1A0.6839 (7)0.4342 (5)0.8293 (4)0.0353 (13)0.511 (11)
O2A0.7720 (9)0.4555 (9)0.7931 (7)0.080 (5)0.511 (11)
O3A0.5823 (9)0.3523 (6)0.7743 (3)0.045 (3)0.511 (11)
C01A0.5385 (9)0.4916 (7)0.8440 (3)0.0353 (13)0.511 (11)
F3A0.5273 (8)0.5233 (6)0.9030 (4)0.048 (2)0.511 (11)
F2A0.4267 (8)0.4383 (6)0.8272 (6)0.070 (3)0.511 (11)
F1A0.5064 (7)0.5707 (5)0.8087 (4)0.042 (2)*0.511 (11)
O1B0.6874 (3)0.3547 (3)0.87585 (18)0.0410 (9)0.489 (11)
F3B0.6075 (16)0.5606 (9)0.8840 (7)0.129 (7)0.489 (11)
O2B0.7866 (7)0.5037 (6)0.8490 (5)0.047 (3)0.489 (11)
C01B0.5446 (10)0.5042 (8)0.8351 (5)0.0308 (12)0.489 (11)
O3B0.6795 (15)0.4142 (10)0.7618 (4)0.082 (5)0.489 (11)
S1B0.6660 (6)0.4067 (5)0.8193 (4)0.0308 (12)0.489 (11)
F2B0.4419 (11)0.4684 (10)0.8634 (6)0.100 (5)0.489 (11)
F1B0.5215 (9)0.5642 (6)0.7862 (5)0.058 (3)*0.489 (11)
U11U22U33U12U13U23
C10.027 (2)0.019 (2)0.023 (2)0.0027 (19)0.0023 (19)0.0019 (19)
C20.034 (3)0.028 (3)0.029 (2)−0.005 (2)−0.002 (2)−0.002 (2)
C30.047 (3)0.032 (3)0.036 (3)−0.013 (3)0.000 (2)0.003 (2)
C40.050 (3)0.028 (3)0.039 (3)−0.006 (3)0.001 (3)0.008 (2)
C50.031 (3)0.023 (3)0.024 (2)0.003 (2)0.000 (2)0.0031 (19)
C110.024 (2)0.021 (2)0.017 (2)0.0018 (18)0.0011 (18)−0.0008 (18)
C120.024 (2)0.028 (3)0.028 (2)−0.0023 (19)−0.001 (2)0.000 (2)
C130.022 (2)0.038 (3)0.038 (3)0.008 (2)−0.003 (2)0.002 (2)
C140.016 (2)0.039 (3)0.034 (3)−0.002 (2)0.004 (2)−0.003 (2)
C150.027 (3)0.038 (3)0.029 (3)0.000 (2)0.004 (2)0.002 (2)
C160.027 (3)0.026 (3)0.026 (2)0.006 (2)0.002 (2)−0.001 (2)
C210.025 (2)0.019 (2)0.016 (2)−0.0026 (18)0.0029 (18)0.0013 (17)
C220.024 (2)0.024 (3)0.023 (2)0.0024 (19)0.0018 (19)−0.0010 (19)
C230.032 (3)0.028 (3)0.022 (2)−0.002 (2)0.002 (2)−0.003 (2)
C240.028 (3)0.030 (3)0.021 (2)−0.002 (2)−0.0043 (19)0.001 (2)
C250.023 (2)0.026 (3)0.030 (2)0.003 (2)0.001 (2)0.002 (2)
C260.024 (2)0.019 (2)0.023 (2)0.0034 (19)0.0017 (19)−0.0007 (18)
C310.026 (2)0.019 (2)0.017 (2)0.0012 (18)0.0005 (18)0.0003 (18)
C320.029 (3)0.025 (3)0.024 (2)0.000 (2)0.000 (2)−0.006 (2)
C330.027 (3)0.041 (3)0.026 (2)0.005 (2)−0.003 (2)−0.002 (2)
C340.036 (3)0.038 (3)0.029 (3)−0.001 (2)−0.007 (2)−0.007 (2)
C350.047 (3)0.034 (3)0.027 (3)−0.004 (3)−0.003 (2)−0.012 (2)
C360.038 (3)0.028 (3)0.025 (2)0.003 (2)−0.001 (2)−0.003 (2)
C410.023 (2)0.019 (2)0.021 (2)0.0018 (18)0.0023 (18)−0.0035 (18)
C420.030 (3)0.026 (3)0.025 (2)0.004 (2)0.006 (2)0.000 (2)
C430.033 (3)0.032 (3)0.032 (3)0.009 (2)0.001 (2)0.004 (2)
C440.025 (3)0.034 (3)0.039 (3)0.007 (2)0.008 (2)−0.005 (2)
C450.034 (3)0.029 (3)0.029 (2)0.001 (2)0.008 (2)−0.004 (2)
C460.032 (3)0.022 (2)0.025 (2)0.007 (2)0.006 (2)−0.001 (2)
N10.0225 (19)0.020 (2)0.0147 (16)0.0061 (15)0.0041 (15)0.0005 (15)
P10.01943 (12)0.01522 (12)0.01339 (11)0.00270 (10)0.00077 (7)0.00016 (10)
P20.01943 (12)0.01522 (12)0.01339 (11)0.00270 (10)0.00077 (7)0.00016 (10)
Pt10.01943 (12)0.01522 (12)0.01339 (11)0.00270 (10)0.00077 (7)0.00016 (10)
O1A0.037 (2)0.035 (2)0.051 (2)0.0101 (17)0.0047 (18)0.0085 (18)
S1A0.049 (3)0.025 (3)0.032 (2)0.023 (2)0.0062 (19)0.0012 (18)
O2A0.039 (5)0.096 (9)0.106 (12)−0.009 (6)0.023 (6)0.052 (8)
O3A0.060 (6)0.042 (5)0.032 (4)0.011 (4)−0.010 (4)−0.024 (4)
C01A0.049 (3)0.025 (3)0.032 (2)0.023 (2)0.0062 (19)0.0012 (18)
F3A0.044 (5)0.051 (5)0.050 (4)0.015 (3)0.018 (4)−0.008 (4)
F2A0.028 (4)0.051 (5)0.127 (9)−0.004 (3)−0.032 (5)−0.003 (6)
O1B0.037 (2)0.035 (2)0.051 (2)0.0101 (17)0.0047 (18)0.0085 (18)
F3B0.169 (15)0.075 (9)0.129 (11)0.060 (9)−0.091 (11)−0.077 (8)
O2B0.020 (4)0.042 (5)0.080 (7)0.001 (4)0.011 (4)0.018 (5)
C01B0.0310 (18)0.029 (3)0.033 (3)0.0079 (18)0.0072 (15)0.0028 (19)
O3B0.115 (13)0.099 (10)0.031 (5)0.050 (10)−0.002 (6)−0.028 (6)
S1B0.0310 (18)0.029 (3)0.033 (3)0.0079 (18)0.0072 (15)0.0028 (19)
F2B0.077 (9)0.161 (14)0.064 (7)0.058 (9)0.026 (7)0.002 (7)
C1—N11.484 (6)C32—C331.372 (6)
C1—C21.524 (6)C32—H320.95
C1—C51.543 (6)C33—C341.390 (7)
C1—H11C33—H330.95
C2—C31.540 (7)C34—C351.378 (7)
C2—H2A0.99C34—H340.95
C2—H2B0.99C35—C361.389 (6)
C3—C41.516 (7)C35—H350.95
C3—H3A0.99C36—H360.95
C3—H3B0.99C41—C421.391 (6)
C4—C51.535 (7)C41—C461.403 (6)
C4—H4A0.99C41—P21.805 (4)
C4—H4B0.99C42—C431.379 (6)
C5—H5A0.99C42—H420.95
C5—H5B0.99C43—C441.391 (7)
C11—C121.387 (6)C43—H430.95
C11—C161.400 (6)C44—C451.385 (7)
C11—P11.805 (4)C44—H440.95
C12—C131.397 (7)C45—C461.393 (6)
C12—H120.95C45—H450.95
C13—C141.379 (7)C46—H460.95
C13—H130.95N1—P21.703 (4)
C14—C151.362 (7)N1—P11.704 (4)
C14—H140.95P1—Pt12.3139 (12)
C15—C161.388 (6)P1—P22.6534 (15)
C15—H150.95P2—Pt12.2943 (13)
C16—H160.95Pt1—P2i2.2943 (13)
C21—C261.381 (6)Pt1—P1i2.3139 (12)
C21—C221.413 (6)O1A—S1A1.458 (9)
C21—P11.806 (4)S1A—O2A1.237 (12)
C22—C231.388 (6)S1A—C01A1.704 (2)
C22—H220.95S1A—O3A1.859 (11)
C23—C241.384 (6)C01A—F3A1.320 (2)
C23—H230.95C01A—F1A1.336 (5)
C24—C251.373 (6)C01A—F2A1.364 (13)
C24—H240.95F3B—C01B1.398 (15)
C25—C261.384 (6)O2B—S1B1.873 (12)
C25—H250.95C01B—F2B1.318 (2)
C26—H260.95C01B—F1B1.320 (5)
C31—C361.387 (6)C01B—S1B1.850 (12)
C31—C321.412 (6)O3B—S1B1.226 (12)
C31—P21.794 (4)
N1—C1—C2116.9 (4)C35—C34—C33121.2 (5)
N1—C1—C5115.1 (3)C35—C34—H34119.4
C2—C1—C5104.0 (4)C33—C34—H34119.4
N1—C1—H1106.7C34—C35—C36119.4 (5)
C2—C1—H1106.7C34—C35—H35120.3
C5—C1—H1106.7C36—C35—H35120.3
C1—C2—C3101.6 (4)C31—C36—C35120.5 (5)
C1—C2—H2A111.4C31—C36—H36119.8
C3—C2—H2A111.4C35—C36—H36119.8
C1—C2—H2B111.4C42—C41—C46120.0 (4)
C3—C2—H2B111.4C42—C41—P2120.4 (3)
H2A—C2—H2B109.3C46—C41—P2119.0 (3)
C4—C3—C2104.6 (4)C43—C42—C41119.9 (4)
C4—C3—H3A110.8C43—C42—H42120
C2—C3—H3A110.8C41—C42—H42120
C4—C3—H3B110.8C42—C43—C44120.5 (4)
C2—C3—H3B110.8C42—C43—H43119.8
H3A—C3—H3B108.9C44—C43—H43119.8
C3—C4—C5107.6 (4)C45—C44—C43120.0 (4)
C3—C4—H4A110.2C45—C44—H44120
C5—C4—H4A110.2C43—C44—H44120
C3—C4—H4B110.2C44—C45—C46120.2 (5)
C5—C4—H4B110.2C44—C45—H45119.9
H4A—C4—H4B108.5C46—C45—H45119.9
C4—C5—C1104.0 (4)C45—C46—C41119.4 (4)
C4—C5—H5A111C45—C46—H46120.3
C1—C5—H5A111C41—C46—H46120.3
C4—C5—H5B111C1—N1—P2122.5 (3)
C1—C5—H5B111C1—N1—P1133.6 (3)
H5A—C5—H5B109P2—N1—P1102.32 (19)
C12—C11—C16119.0 (4)N1—P1—C11113.27 (19)
C12—C11—P1119.2 (3)N1—P1—C21112.14 (19)
C16—C11—P1121.7 (3)C11—P1—C21105.09 (19)
C11—C12—C13119.7 (5)N1—P1—Pt193.07 (13)
C11—C12—H12120.1C11—P1—Pt1118.91 (14)
C13—C12—H12120.1C21—P1—Pt1114.36 (14)
C14—C13—C12119.9 (5)C11—P1—P2124.81 (14)
C14—C13—H13120.1C21—P1—P2128.24 (15)
C12—C13—H13120.1Pt1—P1—P254.50 (4)
C15—C14—C13121.1 (4)N1—P2—C31110.5 (2)
C15—C14—H14119.4N1—P2—C41107.96 (19)
C13—C14—H14119.4C31—P2—C41108.0 (2)
C14—C15—C16119.5 (5)N1—P2—Pt193.78 (13)
C14—C15—H15120.2C31—P2—Pt1115.73 (15)
C16—C15—H15120.2C41—P2—Pt1119.61 (15)
C15—C16—C11120.6 (4)C31—P2—P1120.20 (15)
C15—C16—H16119.7C41—P2—P1128.04 (14)
C11—C16—H16119.7Pt1—P2—P155.19 (3)
C26—C21—C22119.9 (4)P2i—Pt1—P2180.0000 (10)
C26—C21—P1123.0 (3)P2i—Pt1—P1i70.31 (4)
C22—C21—P1116.6 (3)P2—Pt1—P1i109.69 (4)
C23—C22—C21119.2 (4)P2i—Pt1—P1109.69 (4)
C23—C22—H22120.4P2—Pt1—P170.31 (4)
C21—C22—H22120.4P1i—Pt1—P1180.0000 (10)
C24—C23—C22119.9 (4)O2A—S1A—O1A126.8 (7)
C24—C23—H23120O2A—S1A—C01A131.2 (9)
C22—C23—H23120O1A—S1A—C01A101.7 (5)
C25—C24—C23120.7 (4)O2A—S1A—O3A98.5 (9)
C25—C24—H24119.6O1A—S1A—O3A87.3 (5)
C23—C24—H24119.6C01A—S1A—O3A87.0 (5)
C24—C25—C26120.2 (4)F3A—C01A—F1A102.7 (8)
C24—C25—H25119.9F3A—C01A—F2A107.2 (8)
C26—C25—H25119.9F1A—C01A—F2A97.2 (7)
C21—C26—C25120.1 (4)F3A—C01A—S1A116.7 (6)
C21—C26—H26120F1A—C01A—S1A116.7 (7)
C25—C26—H26120F2A—C01A—S1A114.1 (7)
C36—C31—C32119.1 (4)F2B—C01B—F1B118.6 (10)
C36—C31—P2122.7 (3)F2B—C01B—F3B101.7 (10)
C32—C31—P2118.1 (3)F1B—C01B—F3B105.8 (11)
C33—C32—C31120.5 (4)F2B—C01B—S1B111.0 (9)
C33—C32—H32119.8F1B—C01B—S1B113.1 (7)
C31—C32—H32119.8F3B—C01B—S1B104.9 (7)
C32—C33—C34119.4 (5)O3B—S1B—C01B103.5 (7)
C32—C33—H33120.3O3B—S1B—O2B98.8 (9)
C34—C33—H33120.3C01B—S1B—O2B81.4 (6)
N1—C1—C2—C3170.6 (4)C1—N1—P2—C31−54.4 (4)
C5—C1—C2—C342.5 (4)P1—N1—P2—C31113.0 (2)
C1—C2—C3—C4−37.7 (5)C1—N1—P2—C4163.5 (4)
C2—C3—C4—C518.9 (6)P1—N1—P2—C41−129.1 (2)
C3—C4—C5—C17.2 (6)C1—N1—P2—Pt1−173.7 (3)
N1—C1—C5—C4−160.2 (4)P1—N1—P2—Pt1−6.25 (16)
C2—C1—C5—C4−31.0 (5)C1—N1—P2—P1−167.5 (4)
C16—C11—C12—C13−0.6 (7)C36—C31—P2—N181.5 (4)
P1—C11—C12—C13176.9 (4)C32—C31—P2—N1−94.2 (4)
C11—C12—C13—C143.1 (7)C36—C31—P2—C41−36.4 (4)
C12—C13—C14—C15−3.0 (8)C32—C31—P2—C41147.9 (3)
C13—C14—C15—C160.2 (7)C36—C31—P2—Pt1−173.6 (3)
C14—C15—C16—C112.4 (7)C32—C31—P2—Pt110.8 (4)
C12—C11—C16—C15−2.2 (7)C36—C31—P2—P1123.4 (4)
P1—C11—C16—C15−179.6 (4)C32—C31—P2—P1−52.3 (4)
C26—C21—C22—C23−0.6 (6)C42—C41—P2—N123.8 (4)
P1—C21—C22—C23171.0 (3)C46—C41—P2—N1−164.9 (4)
C21—C22—C23—C240.6 (7)C42—C41—P2—C31143.3 (4)
C22—C23—C24—C250.3 (7)C46—C41—P2—C31−45.4 (4)
C23—C24—C25—C26−1.3 (7)C42—C41—P2—Pt1−81.5 (4)
C22—C21—C26—C25−0.4 (6)C46—C41—P2—Pt189.8 (4)
P1—C21—C26—C25−171.4 (3)C42—C41—P2—P1−14.4 (5)
C24—C25—C26—C211.3 (7)C46—C41—P2—P1156.9 (3)
C36—C31—C32—C33−0.2 (7)C11—P1—P2—N184.5 (3)
P2—C31—C32—C33175.7 (4)C21—P1—P2—N1−77.7 (3)
C31—C32—C33—C34−1.0 (7)Pt1—P1—P2—N1−172.4 (2)
C32—C33—C34—C351.1 (8)N1—P1—P2—C31−85.7 (3)
C33—C34—C35—C360.0 (8)C11—P1—P2—C31−1.2 (2)
C32—C31—C36—C351.2 (7)C21—P1—P2—C31−163.3 (2)
P2—C31—C36—C35−174.4 (4)Pt1—P1—P2—C31101.95 (17)
C34—C35—C36—C31−1.1 (7)N1—P1—P2—C4169.7 (3)
C46—C41—C42—C43−0.8 (7)C11—P1—P2—C41154.1 (3)
P2—C41—C42—C43170.4 (4)C21—P1—P2—C41−8.0 (3)
C41—C42—C43—C44−0.6 (7)Pt1—P1—P2—C41−102.71 (19)
C42—C43—C44—C452.0 (8)N1—P1—P2—Pt1172.4 (2)
C43—C44—C45—C46−2.0 (8)C11—P1—P2—Pt1−103.14 (18)
C44—C45—C46—C410.6 (7)C21—P1—P2—Pt194.75 (18)
C42—C41—C46—C450.8 (7)N1—P2—Pt1—P1i−175.23 (12)
P2—C41—C46—C45−170.5 (4)C31—P2—Pt1—P1i69.81 (17)
C2—C1—N1—P288.8 (4)C41—P2—Pt1—P1i−62.09 (17)
C5—C1—N1—P2−148.7 (3)P1—P2—Pt1—P1i180
C2—C1—N1—P1−74.2 (5)N1—P2—Pt1—P14.77 (12)
C5—C1—N1—P148.3 (6)C31—P2—Pt1—P1−110.19 (17)
C1—N1—P1—C1148.2 (4)C41—P2—Pt1—P1117.91 (17)
P2—N1—P1—C11−117.2 (2)N1—P1—Pt1—P2i175.24 (12)
C1—N1—P1—C21−70.6 (4)C11—P1—Pt1—P2i−65.98 (16)
P2—N1—P1—C21124.1 (2)C21—P1—Pt1—P2i59.23 (16)
C1—N1—P1—Pt1171.5 (4)P2—P1—Pt1—P2i180
P2—N1—P1—Pt16.19 (16)N1—P1—Pt1—P2−4.76 (12)
C1—N1—P1—P2165.3 (5)C11—P1—Pt1—P2114.02 (16)
C12—C11—P1—N1114.3 (4)C21—P1—Pt1—P2−120.77 (16)
C16—C11—P1—N1−68.3 (4)O2A—S1A—C01A—F3A−117.3 (14)
C12—C11—P1—C21−122.9 (4)O1A—S1A—C01A—F3A57.3 (10)
C16—C11—P1—C2154.5 (4)O3A—S1A—C01A—F3A143.9 (9)
C12—C11—P1—Pt16.6 (4)O2A—S1A—C01A—F1A4.5 (17)
C16—C11—P1—Pt1−176.0 (3)O1A—S1A—C01A—F1A179.1 (8)
C12—C11—P1—P271.5 (4)O3A—S1A—C01A—F1A−94.3 (10)
C16—C11—P1—P2−111.1 (3)O2A—S1A—C01A—F2A116.7 (15)
C26—C21—P1—N1−23.0 (4)O1A—S1A—C01A—F2A−68.6 (7)
C22—C21—P1—N1165.6 (3)O3A—S1A—C01A—F2A18.0 (9)
C26—C21—P1—C11−146.5 (4)F2B—C01B—S1B—O3B126.0 (14)
C22—C21—P1—C1142.2 (4)F1B—C01B—S1B—O3B−10.2 (14)
C26—C21—P1—Pt181.3 (4)F3B—C01B—S1B—O3B−125.0 (13)
C22—C21—P1—Pt1−90.0 (3)F2B—C01B—S1B—O2B−137.0 (12)
C26—C21—P1—P218.4 (5)F1B—C01B—S1B—O2B86.9 (9)
C22—C21—P1—P2−153.0 (3)F3B—C01B—S1B—O2B−27.9 (10)
D—H···AD—HH···AD···AD—H···A
C25—H25···O3A0.952.523.398 (9)154
C26—H26···O1B0.952.53.238 (6)135
C34—H34···O3Aii0.952.383.127 (10)135
C45—H45···O3Aiii0.952.33.229 (9)165
C15—H15···O3Aiv0.952.473.420 (11)178
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
C25—H25⋯O3A 0.952.523.398 (9)154
C26—H26⋯O1B 0.952.53.238 (6)135
C34—H34⋯O3A i 0.952.383.127 (10)135
C45—H45⋯O3A ii 0.952.33.229 (9)165
C15—H15⋯O3A iii 0.952.473.420 (11)178

Symmetry codes: (i) ; (ii) ; (iii) .

  11 in total

1.  Borate esters as alternative acid promoters in the palladium-catalyzed methoxycarbonylation of ethylene.

Authors:  Alta C Ferreira; Renier Crous; Linette Bennie; Anna M M Meij; Kevin Blann; Barend C B Bezuidenhoudt; Desmond A Young; Mike J Green; Andreas Roodt
Journal:  Angew Chem Int Ed Engl       Date:  2007       Impact factor: 15.336

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

3.  Rhodium hydride formation in the presence of a bulky monophosphite ligand: a spectroscopic and solid-state investigation.

Authors:  Renier Crous; Michael Datt; Douglas Foster; Linette Bennie; Casper Steenkamp; Johan Huyser; Leo Kirsten; Gideon Steyl; Andreas Roodt
Journal:  Dalton Trans       Date:  2005-02-17       Impact factor: 4.390

4.  Synthesis, crystal structure and hydroformylation activity of triphenylphosphite modified cobalt catalysts.

Authors:  Marco Haumann; Reinout Meijboom; John R Moss; Andreas Roodt
Journal:  Dalton Trans       Date:  2004-05-10       Impact factor: 4.390

5.  Rapid phosphorus(III) ligand evaluation utilising potassium selenocyanate.

Authors:  Alfred Muller; Stefanus Otto; Andreas Roodt
Journal:  Dalton Trans       Date:  2007-11-16       Impact factor: 4.390

6.  Bis[N,N-bis-(diphenyl-phosphan-yl)cyclo-hexyl-amine-κP,P']platinum(II) bis-(hexa-fluorido-phosphate) dichloro-methane disolvate.

Authors:  Ilana Engelbrecht; Hendrik G Visser; Andreas Roodt
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-07-24

7.  N,N-Bis(diphenyl-phosphan-yl)cyclo--penta-namine.

Authors:  Ilana Engelbrecht; Hendrik G Visser; Andreas Roodt
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-11-27

8.  N,N-Bis(diphenyl-phosphanyl)cyclo-propyl-amine.

Authors:  Ilana Engelbrecht; Hendrik G Visser; Andreas Roodt
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-10-23

9.  [N,N-Bis(diphenyl-phosphino)propyl-amine-κP,P']dichloridoplatinum(II).

Authors:  Nicoline Cloete; Hendrik G Visser; Andreas Roodt
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-12-12

10.  Bis[N,N-bis-(diphenyl-phosphan-yl)pentyl-amine-κP,P']platinum(II) bis-(hexa-fluoridophosphate) dichloro-methane disolvate.

Authors:  Ilana Engelbrecht; Hendrik G Visser; Andreas Roodt
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-07-14
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