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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 8| August 2010| Pages m922-m923
https://doi.org/10.1107/S1600536810025560

Bis[N,N-bis­­(di­phenyl­phosphan­yl)pentyl­amine-κ2P,P′]platinum(II) bis­­(hexa­fluoridophosphate) di­chloro­methane disolvate

Ilana Engelbrecht,a* Hendrik G. Vissera and Andreas Roodta

aDepartment of Chemistry, University of the Free State, PO Box 339, Bloemfontein 9300, South Africa
*Correspondence e-mail: engelbrechti@ufs.ac.za

(Received 24 June 2010; accepted 29 June 2010; online 14 July 2010)

The PtII atom in the title compound, [Pt(C29H31NP2)2](PF6)2·2CH2Cl2, is coordinated by four P atoms from two bis­(di­phenyl­phosphan­yl)pentyl­amine ligands with an average Pt—P distance of 2.300 (1) Å. The coordination around the PtII atom shows a highly distorted square-planar geometry, as evidenced by the P—Pt—P bite angles of 70.45 (3) and 70.64 (3)°. The asymmetric unit contains two hexa­fluoridophosphate ions, the metal complex and two dichloro­methane solvent mol­ecules. One of the chloride atoms of one of the dichloro­methane mol­ecules is disordered over two sites in a 0.515 (3):0.485 (3) ratio. C—H⋯F hydrogen bonds stabilize the crystal packing.

Related literature

For related platinum(II) complexes, see: Farrar & Browning (1995[Farrar, D. G. & Browning, C. S. (1995). J. Chem. Soc. Dalton Trans. pp. 521-530.]); Dyson et al. (2004[Dyson, P. J., Fei, Z. & Scopelliti, R. (2004). Eur. J. Inorg. Chem. pp. 530-537.]); Cloete et al. (2010[Cloete, N., Visser, H. G. & Roodt, A. (2010). Acta Cryst. E66, m51-m52.]). For related diphenyl­phosphanyl ligands, see: Keat et al. (1981[Keat, R., Manojlovic-Muir, L., Muir, K. W. & Rycroft, D. S. (1981). J. Chem. Soc. Dalton Trans. pp. 2192-2198.]); Cloete et al. (2008[Cloete, N., Visser, H. G., Roodt, A., Dixon, J. T. & Blann, K. (2008). Acta Cryst. E64, o480.], 2009[Cloete, N., Visser, H. G., Roodt, A. & Gabrielli, W. F. (2009). Acta Cryst. E65, o3081.]); Cotton et al. (1996[Cotton, F. A., Kuhn, F. E. & Yokochi, A. (1996). Inorg. Chim. Acta, 252, 251-256.]); Fei et al. (2003[Fei, Z., Scopeleti, R. & Dyson, P. J. (2003). Dalton Trans. pp. 2772-2779.]). For applications of diphenyl­phosphanyl ligands and their metal complexes in homogeneous catalysis, see: Steyn et al. (1992[Steyn, G. J. J., Roodt, A. & Leipoldt, J. G. (1992). Inorg. Chem. 31, 3477-3481.], 1997[Steyn, G. J. J., Roodt, A., Poletaeva, I. A. & Varshavsky, Y. S. (1997). J. Organomet. Chem. 536-537, 197-205.]); Otto et al. (1998[Otto, S., Roodt, A., Swarts, J. C. & Erasmus, J. C. (1998). Polyhedron, 17, 2447-2453.]); Roodt & Steyn (2000[Roodt, A. & Steyn, G. J. J. (2000). Recent Research Developments in Inorganic Chemistry, Vol. 2, pp. 1-23. Trivandrum, India: Transworld Research Network.]); Brink et al. (2010[Brink, A., Visser, H. G., Steyl, G. & Roodt, A. (2010). Dalton Trans. pp. 5572-5578.]); Viljoen et al. (2008[Viljoen, J. A., Muller, A. & Roodt, A. (2008). Acta Cryst. E64, m838-m839.], 2009a[Viljoen, J. A., Visser, H. G., Roodt, A. & Steyn, M. (2009a). Acta Cryst. E65, m1514-m1515.],b[Viljoen, J. A., Visser, H. G., Roodt, A. & Steyn, M. (2009b). Acta Cryst. E65, m1367-m1368.], 2010[Viljoen, J. A., Visser, H. G. & Roodt, A. (2010). Acta Cryst. E66, m603-m604.]); Steyn et al. (2008[Steyn, M., Roodt, A. & Steyl, G. (2008). Acta Cryst. E64, m827.]).

[Scheme 1]

Experimental

Crystal data

  • [Pt(C29H31NP2)2](PF6)2·2CH2Cl2

  • Mr = 1565.85

  • Monoclinic, C c

  • a = 11.3876 (10) Å

  • b = 24.283 (3) Å

  • c = 23.102 (2) Å

  • β = 97.669 (4)°

  • V = 6331.1 (11) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 2.61 mm−1

  • T = 100 K

  • 0.26 × 0.19 × 0.13 mm
Data collection

  • Bruker X8 APEXII 4K Kappa CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2004[Bruker (2004). SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.550, Tmax = 0.728

  • 47664 measured reflections

  • 14210 independent reflections

  • 13180 reflections with I > 2σ(I)

  • Rint = 0.03
Refinement

  • R[F2 > 2σ(F2)] = 0.024

  • wR(F2) = 0.047

  • S = 0.89

  • 14210 reflections

  • 767 parameters

  • 2 restraints

  • H-atom parameters constrained

  • Δρmax = 1.08 e Å−3

  • Δρmin = −1.13 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 6561 Friedel pairs

  • Flack parameter: 0.014 (2)

Table 1
Selected geometric parameters (Å, °)

P1—Pt1 2.3063 (8)
P2—Pt1 2.2965 (8)
P3—Pt1 2.2994 (8)
P4—Pt1 2.2995 (8)
P2—N1—P1 103.40 (13)
P4—N2—P3 103.15 (13)
N1—P1—Pt1 92.81 (9)
C41—P2—Pt1 118.82 (11)
C51—P3—Pt1 122.28 (11)
N2—P4—Pt1 93.11 (9)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
C25—H25⋯F8 0.95 2.53 3.437 (4) 160
C55—H55⋯F2 0.95 2.49 3.079 (4) 120
C65—H65⋯F10 0.95 2.47 3.297 (4) 145
C83—H83⋯F11 0.95 2.37 3.267 (4) 158
C01—H01B⋯F2i 0.99 2.29 3.244 (5) 161
C01—H01B⋯F6i 0.99 2.4 3.150 (5) 132
C5—H5C⋯F11ii 0.98 2.51 3.196 (4) 127
C8—H8A⋯F3iii 0.99 2.54 3.450 (4) 153
C53—H53⋯F7iv 0.95 2.51 3.273 (4) 137
C63—H63⋯F4v 0.95 2.51 3.373 (4) 151
C73—H73⋯F9vi 0.95 2.53 3.426 (4) 156
Symmetry codes: (i) [x+{\script{1\over 2}}, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]; (ii) x-1, y, z; (iii) x+1, y, z; (iv) [x, -y+1, z+{\script{1\over 2}}]; (v) [x+{\script{1\over 2}}, y-{\script{1\over 2}}, z]; (vi) [x-{\script{1\over 2}}, y+{\script{1\over 2}}, z].

Data collection: APEX2 (Bruker, 2010[Bruker (2010). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2004[Bruker (2004). SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg & Putz, 2005[Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: WinGX (Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536810025560/bt5278sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810025560/bt5278Isup2.hkl

checkCIF report


Comment top

The synthesis of diphenylphosphanyl ligands and metal complexes thereof, forms part of ongoing research in the field of homogeneous catalysis (Steyn et al., 1992, 1997; Otto et al., 1998; Roodt & Steyn, 2000; Brink et al., 2010; Viljoen et al., 2008, 2009a,b, 2010; Steyn et al., 2008). Colourless crystals of the title compound crystallize with two hexafluoridophosphate anions and two dichloromethane solvent molecules, of which one displays a 51% possitional disorder on one chloride atom. In the title compound, all bond distances and angles are considered to be normal and fall within the range reported for similar complexes (Farrar et al., 1995; Dyson et al., 2004; Cloete et al., 2010). The square-planar geometry around the PtII metal centre is highly distorted with P1—Pt—P2 and P3—Pt—P4 bite angles of 70.45 (3) and 70.64 (3) °, respectively. The distorted tetrahedral angles of the P atoms, which range between 92.81 (9) and 122.28 (11) ° further illustrate the strain in the complex. The N atoms also deviate from the ideal tetrahedral configuration with P1—N1—P2 and P3—N2—P4 angles being 103.40 (13) and 103.15 (13) °, respectively. The distance between the N1 atom and the plane created by C1, P1 and P2 is -0.021 (2) ° whereas the distance of N2 and the plane created by C6, P3 and P4 shows a slightly bigger deviation of -0.122 (2) °. This shows that the N atom adopts an almost planar geometry with the two P atoms and the C atom attached to it in each case to accomodate the steric bulk of the phenyl groups and the alkyl group of the ligand. The intermolecular hydrogen bonds lead to a three-dimensional polymetric network obtained through C—H···F interactions.

Related literature top

For related platinum(II) complexes, see: Farrar et al. (1995); Dyson et al. (2004); Cloete et al. (2010). For related diphenylphosphanyl ligands, see: Keat et al. (1981); Cloete et al. (2008, 2009); Cotton et al. (1996); Fei et al. (2003). For applications of diphenylphosphanyl ligands and their metal complexes in homogeneous catalysis, see: Steyn et al. (1992, 1997); Otto et al. (1998); Roodt & Steyn (2000); Brink et al. (2010); Viljoen et al. (2008, 2009a,b, 2010); Steyn et al. (2008).

Experimental top

[Pt(cod)Cl2] (20 mg, 0.0535 mmol) (cod = 1,5-cyclooctadiene) dissolved in the minimum amount of dichloromethane was added in a rapid dropwise manner to a solution of bis(diphenylphosphanyl)pentylamine (51.9 mg, 0.114 mmol) and NaPF6 (20 mg, 0.119 mmol) dissolved in the minimum volume of dichloromethane-methanol (1:1). After stirring for 20 min, the solvent was removed completely under reduced pressure. Dichloromethane was added until no further dissolution of solid was evident. The resulting heterogeneous mixture was filtered to remove the insoluble NaCl by-product. The colourless solid product was precipitated upon addition of methanol followed by a reduction in solvent volume under reduced pressure. The compound was isolated by filtration and washed with diethyl ether (10 cm3). Colourless crystals suitable for X-ray crystallography were obtained by the slow diffusion of diethyl ether into a solution of the product in dichloromethane at room temperature. (Crude yield: 39 mg, 66%) Spectroscopy data: 1H NMR (600 MHz, CD2Cl2): δ = 0.6 (t, 6H, CH3), 0.7 to 1.1 (m, 12H, 6 x CH2), 2.9 (t, 4H, N—CH2), 7.3 to 7.8 (m, 40H, Ar); 31P NMR (243 MHz, CD2Cl2): δ = 40.6 (t, 1JPt—P = 1063.0 Hz), -134.69 to -153.74 (m, PF6).

Refinement top

The methyl, methylene and aromatic H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms, with C—H = 0.95, 0.99 and 0.98Å and Uĩso~(H) = 1.5U~eq~(C) and 1.2U~eq~(C), respectively.The methyl groups were generated to fit the difference electron density and the groups were then refined as rigid rotors. The highest peak is located 0.06Å from C1 and the deepest hole is situated 0.06Å from C02B.

Structure description top

The synthesis of diphenylphosphanyl ligands and metal complexes thereof, forms part of ongoing research in the field of homogeneous catalysis (Steyn et al., 1992, 1997; Otto et al., 1998; Roodt & Steyn, 2000; Brink et al., 2010; Viljoen et al., 2008, 2009a,b, 2010; Steyn et al., 2008). Colourless crystals of the title compound crystallize with two hexafluoridophosphate anions and two dichloromethane solvent molecules, of which one displays a 51% possitional disorder on one chloride atom. In the title compound, all bond distances and angles are considered to be normal and fall within the range reported for similar complexes (Farrar et al., 1995; Dyson et al., 2004; Cloete et al., 2010). The square-planar geometry around the PtII metal centre is highly distorted with P1—Pt—P2 and P3—Pt—P4 bite angles of 70.45 (3) and 70.64 (3) °, respectively. The distorted tetrahedral angles of the P atoms, which range between 92.81 (9) and 122.28 (11) ° further illustrate the strain in the complex. The N atoms also deviate from the ideal tetrahedral configuration with P1—N1—P2 and P3—N2—P4 angles being 103.40 (13) and 103.15 (13) °, respectively. The distance between the N1 atom and the plane created by C1, P1 and P2 is -0.021 (2) ° whereas the distance of N2 and the plane created by C6, P3 and P4 shows a slightly bigger deviation of -0.122 (2) °. This shows that the N atom adopts an almost planar geometry with the two P atoms and the C atom attached to it in each case to accomodate the steric bulk of the phenyl groups and the alkyl group of the ligand. The intermolecular hydrogen bonds lead to a three-dimensional polymetric network obtained through C—H···F interactions.

For related platinum(II) complexes, see: Farrar et al. (1995); Dyson et al. (2004); Cloete et al. (2010). For related diphenylphosphanyl ligands, see: Keat et al. (1981); Cloete et al. (2008, 2009); Cotton et al. (1996); Fei et al. (2003). For applications of diphenylphosphanyl ligands and their metal complexes in homogeneous catalysis, see: Steyn et al. (1992, 1997); Otto et al. (1998); Roodt & Steyn (2000); Brink et al. (2010); Viljoen et al. (2008, 2009a,b, 2010); Steyn et al. (2008).

Computing details top

Data collection: APEX2 (Bruker, 2010); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus (Bruker, 2004); 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).

Figures top
[Figure 1] Fig. 1. Molecular structure of the title compound. Displacement ellipsoids are drawn at the 50% probability level. Hydrogen atoms, solvent molecules and hexafluoridophosphate ions have been omitted for clarity and are displayed in Figure 2.
[Figure 2] Fig. 2. Numbering scheme of solvent molecules and hexafluoridophosphate ions. Displacement ellipsoids are drawn at the 50% probability level. Hydrogen atoms have been omitted for clarity.
Bis[N,N-bis(diphenylphosphanyl)pentylamine-κ2P,P']platinum(II) bis(hexafluoridophosphate) dichloromethane disolvate top
Crystal data top
[Pt(C29H31NP2)2](PF6)2·2CH2Cl2F(000) = 3136
Mr = 1565.85Dx = 1.643 Mg m−3
Monoclinic, CcMo Kα radiation, λ = 0.71073 Å
Hall symbol: C -2ycCell parameters from 9893 reflections
a = 11.3876 (10) Åθ = 2.8–28.2°
b = 24.283 (3) ŵ = 2.61 mm−1
c = 23.102 (2) ÅT = 100 K
β = 97.669 (4)°Cuboid, colourless
V = 6331.1 (11) Å30.26 × 0.19 × 0.13 mm
Z = 4
Data collection top
Bruker X8 APEXII 4K Kappa CCD
diffractometer		14210 independent reflections
Radiation source: fine-focus sealed tube13180 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.03
ω and φ scansθmax = 28°, θmin = 4.2°
Absorption correction: multi-scan
(SADABS; Bruker, 2004)		h = −13→15
Tmin = 0.550, Tmax = 0.728k = −32→32
47664 measured reflectionsl = −30→30
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.024H-atom parameters constrained
wR(F2) = 0.047 w = 1/[σ2(Fo2) + (0.P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.89(Δ/σ)max = 0.045
14210 reflectionsΔρmax = 1.08 e Å−3
767 parametersΔρmin = −1.13 e Å−3
2 restraintsAbsolute structure: Flack (1983), 6561 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.014 (2)
Crystal data top
[Pt(C29H31NP2)2](PF6)2·2CH2Cl2V = 6331.1 (11) Å3
Mr = 1565.85Z = 4
Monoclinic, CcMo Kα radiation
a = 11.3876 (10) ŵ = 2.61 mm−1
b = 24.283 (3) ÅT = 100 K
c = 23.102 (2) Å0.26 × 0.19 × 0.13 mm
β = 97.669 (4)°
Data collection top
Bruker X8 APEXII 4K Kappa CCD
diffractometer		14210 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2004)		13180 reflections with I > 2σ(I)
Tmin = 0.550, Tmax = 0.728Rint = 0.03
47664 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.024H-atom parameters constrained
wR(F2) = 0.047Δρmax = 1.08 e Å−3
S = 0.89Δρmin = −1.13 e Å−3
14210 reflectionsAbsolute structure: Flack (1983), 6561 Friedel pairs
767 parametersAbsolute structure parameter: 0.014 (2)
2 restraints
Special details top

Experimental. The intensity data was collected on a Bruker X8 ApexII 4 K Kappa CCD diffractometer using an exposure time of 30 s/frame. A total of 1757 frames were collected with a frame width of 0.5° covering up to θ = 28.32° with 99.1% completeness accomplished.

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C10.1482 (3)0.56240 (17)0.77193 (14)0.0287 (6)
H1A0.10640.59650.75750.034*
H1B0.09270.54020.79190.034*
C010.8626 (5)0.75498 (18)0.64979 (17)0.0559 (14)
H01A0.91860.78330.63930.067*
H01B0.790.75690.6210.067*
C20.1807 (3)0.52966 (14)0.71951 (14)0.0255 (7)
H2A0.22320.55410.6950.031*
H2B0.23490.49920.73380.031*
C30.0724 (3)0.50600 (16)0.68260 (15)0.0308 (8)
H3A0.03230.48040.7070.037*
H3B0.09860.48430.65040.037*
C4−0.0175 (3)0.54921 (16)0.65640 (14)0.0289 (9)
H4A0.02070.57370.63020.035*
H4B−0.04170.57210.68830.035*
C5−0.1280 (3)0.52310 (16)0.62195 (15)0.0287 (6)
H5A−0.10460.50040.59040.043*
H5B−0.1820.55220.60540.043*
H5C−0.16810.50010.64810.043*
C60.7473 (3)0.65347 (13)1.03600 (13)0.0153 (7)
H6A0.80680.66931.01320.018*
H6B0.77770.61741.05140.018*
C70.7345 (3)0.69112 (14)1.08671 (14)0.0229 (8)
H7A0.67860.67451.1110.027*
H7B0.70080.72671.07170.027*
C80.8540 (3)0.70150 (14)1.12475 (14)0.0210 (7)
H8A0.90920.71811.10.025*
H8B0.84180.72861.15540.025*
C90.9120 (3)0.65016 (16)1.15412 (16)0.0335 (9)
H9A0.93340.62461.12380.04*
H9B0.85470.63121.17590.04*
C101.0234 (3)0.66455 (16)1.19610 (15)0.0301 (9)
H10A1.07940.68431.17480.045*
H10B1.06040.63061.21280.045*
H10C1.00180.68791.22760.045*
C110.1754 (3)0.54547 (12)0.92209 (13)0.0124 (6)
C120.1015 (3)0.59109 (13)0.92072 (14)0.0173 (7)
H120.10630.61930.89260.021*
C130.0210 (3)0.59546 (14)0.96012 (14)0.0214 (7)
H13−0.02990.62660.95910.026*
C140.0144 (3)0.55456 (14)1.00112 (14)0.0223 (8)
H14−0.04040.55791.02850.027*
C150.0874 (3)0.50870 (14)1.00257 (14)0.0219 (7)
H150.08210.48071.03080.026*
C160.1678 (3)0.50367 (14)0.96310 (14)0.0181 (8)
H160.21740.47210.96380.022*
C210.3353 (3)0.47632 (12)0.86595 (12)0.0124 (6)
C220.2482 (3)0.43718 (13)0.84764 (13)0.0158 (7)
H220.16670.44620.8460.019*
C230.2824 (3)0.38498 (13)0.83188 (14)0.0201 (7)
H230.22380.35810.81940.024*
C240.4007 (3)0.37181 (13)0.83429 (14)0.0202 (7)
H240.4230.33590.82350.024*
C250.4881 (3)0.41069 (13)0.85241 (14)0.0198 (7)
H250.56950.40150.8540.024*
C260.4549 (3)0.46288 (13)0.86811 (12)0.0159 (7)
H260.51380.48960.88040.019*
C310.4393 (3)0.62230 (14)0.75582 (14)0.0138 (7)
C320.4829 (3)0.57081 (13)0.74347 (13)0.0179 (7)
H320.45640.53890.76170.021*
C330.5654 (3)0.56589 (15)0.70451 (14)0.0237 (8)
H330.59440.53060.69570.028*
C340.6049 (3)0.61239 (15)0.67874 (16)0.0231 (9)
H340.6610.60890.6520.028*
C350.5639 (3)0.66405 (14)0.69120 (13)0.0199 (7)
H350.59190.69570.67320.024*
C360.4817 (3)0.66947 (13)0.73026 (13)0.0162 (6)
H360.45430.70490.73960.019*
C410.2697 (3)0.69369 (13)0.80151 (13)0.0139 (6)
C420.2631 (3)0.72902 (13)0.84867 (14)0.0170 (7)
H420.29640.71820.88690.02*
C430.2080 (3)0.77987 (14)0.83976 (15)0.0238 (8)
H430.20290.80370.87190.029*
C440.1608 (3)0.79582 (14)0.78425 (15)0.0245 (8)
H440.12620.83130.77790.029*
C450.1638 (3)0.76030 (14)0.73776 (15)0.0236 (8)
H450.12780.77080.69990.028*
C460.2187 (3)0.70949 (14)0.74582 (14)0.0206 (7)
H460.22160.68550.71350.025*
C510.4639 (3)0.59396 (14)1.06229 (14)0.0128 (7)
C520.5255 (3)0.58111 (13)1.11684 (13)0.0175 (7)
H520.60680.5711.12020.021*
C530.4689 (3)0.58301 (14)1.16598 (13)0.0210 (7)
H530.51160.57561.20340.025*
C540.3483 (3)0.59587 (13)1.16053 (15)0.0215 (7)
H540.30830.59581.19410.026*
C550.2871 (3)0.60865 (13)1.10647 (15)0.0201 (8)
H550.20540.61781.1030.024*
C560.3451 (3)0.60810 (12)1.05696 (14)0.0164 (7)
H560.30340.61741.01980.02*
C610.6169 (2)0.52730 (12)1.00093 (12)0.0113 (6)
C620.5670 (3)0.48035 (13)1.02358 (13)0.0168 (7)
H620.50110.48391.04460.02*
C630.6140 (3)0.42899 (13)1.01521 (14)0.0194 (7)
H630.580.39721.03020.023*
C640.7105 (3)0.42374 (14)0.98505 (14)0.0206 (7)
H640.74230.38830.97930.025*
C650.7610 (3)0.46978 (13)0.96313 (13)0.0189 (7)
H650.82810.46590.94310.023*
C660.7136 (3)0.52137 (13)0.97039 (13)0.0159 (7)
H660.74720.55280.95450.019*
C710.5542 (3)0.74473 (12)0.93612 (13)0.0132 (6)
C720.5523 (3)0.77807 (13)0.88622 (14)0.0176 (7)
H720.57830.76360.85190.021*
C730.5127 (3)0.83181 (13)0.88716 (15)0.0217 (7)
H730.50890.8540.85310.026*
C740.4788 (3)0.85312 (14)0.93750 (16)0.0257 (8)
H740.45590.89070.93880.031*
C750.4779 (3)0.81994 (14)0.98661 (15)0.0257 (8)
H750.45260.83461.0210.031*
C760.5137 (3)0.76581 (13)0.98528 (14)0.0197 (7)
H760.51060.74291.01840.024*
C810.7146 (3)0.67248 (13)0.88803 (13)0.0142 (6)
C820.7258 (3)0.63027 (13)0.84829 (13)0.0167 (7)
H820.66770.6020.84290.02*
C830.8203 (3)0.62906 (14)0.81665 (14)0.0225 (7)
H830.82760.60.78980.027*
C840.9043 (3)0.67045 (14)0.82435 (14)0.0200 (7)
H840.96850.67010.8020.024*
C850.8958 (3)0.71218 (13)0.86402 (13)0.0192 (7)
H850.9550.73990.86960.023*
C860.8009 (3)0.71373 (13)0.89587 (13)0.0149 (6)
H860.79450.74270.92290.018*
N10.2516 (2)0.57749 (10)0.81489 (10)0.0128 (5)
N20.6347 (2)0.64435 (10)0.99603 (10)0.0132 (5)
F10.1335 (2)0.71148 (9)0.96105 (10)0.0424 (6)
F20.13372 (19)0.70746 (9)1.05954 (9)0.0404 (6)
F3−0.02480 (17)0.74020 (9)1.00181 (8)0.0330 (5)
F40.0917 (2)0.79785 (8)1.06069 (8)0.0385 (5)
F50.0903 (2)0.80160 (8)0.96277 (8)0.0345 (5)
F60.24994 (19)0.76911 (11)1.02022 (10)0.0551 (7)
F70.72443 (19)0.43486 (9)0.74705 (9)0.0375 (5)
F80.78582 (17)0.40997 (8)0.84068 (8)0.0255 (4)
F90.91953 (17)0.42305 (8)0.77746 (8)0.0314 (5)
F100.90878 (19)0.48342 (9)0.85057 (8)0.0385 (6)
F110.84607 (19)0.50836 (8)0.75712 (9)0.0349 (5)
F120.71315 (19)0.49579 (9)0.82069 (10)0.0341 (6)
P10.29586 (7)0.54624 (3)0.87958 (3)0.01116 (16)
P20.34891 (7)0.62997 (4)0.81388 (3)0.01159 (16)
P30.53802 (7)0.59136 (4)0.99775 (3)0.01165 (16)
P40.59236 (7)0.67322 (3)0.92964 (3)0.01178 (16)
P50.11328 (8)0.75458 (4)1.01089 (4)0.02094 (19)
P60.81623 (8)0.45921 (4)0.79889 (4)0.02016 (19)
Pt10.441743 (9)0.610768 (4)0.906107 (7)0.01061 (3)
Cl10.82677 (9)0.76853 (4)0.71916 (4)0.0404 (2)
Cl20.92773 (14)0.68887 (6)0.64686 (5)0.0751 (5)
Cl30.30911 (8)0.36043 (4)0.97952 (4)0.0320 (2)
Cl4A0.2246 (2)0.36509 (14)1.09592 (9)0.0580 (9)0.515 (3)
C02A0.3267 (3)0.34492 (15)1.05375 (14)0.0255 (7)0.515 (3)
H02A0.33390.30441.05740.031*0.515 (3)
H02B0.40370.36061.07110.031*0.515 (3)
Cl4B0.2955 (3)0.40266 (14)1.09242 (10)0.0612 (9)0.485 (3)
C02B0.3267 (3)0.34492 (15)1.05375 (14)0.0308 (8)0.485 (3)
H02C0.27270.31461.06120.037*0.485 (3)
H02D0.40910.33281.06660.037*0.485 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0226 (13)0.0425 (18)0.0194 (12)0.0050 (12)−0.0034 (10)−0.0088 (12)
C010.083 (4)0.041 (3)0.039 (3)0.039 (3)−0.010 (2)0.001 (2)
C20.0335 (18)0.0216 (18)0.0222 (17)0.0036 (14)0.0069 (14)0.0032 (14)
C30.041 (2)0.031 (2)0.0215 (17)0.0028 (16)0.0065 (15)−0.0015 (15)
C40.0239 (19)0.047 (3)0.0160 (17)0.0091 (17)0.0024 (14)−0.0047 (17)
C50.0226 (13)0.0425 (18)0.0194 (12)0.0050 (12)−0.0034 (10)−0.0088 (12)
C60.0166 (16)0.0123 (17)0.0160 (16)−0.0026 (12)−0.0009 (13)0.0025 (13)
C70.0225 (18)0.0202 (19)0.0250 (18)0.0007 (14)−0.0004 (15)−0.0077 (15)
C80.0233 (18)0.0207 (19)0.0187 (17)−0.0071 (14)0.0020 (14)−0.0071 (14)
C90.036 (2)0.032 (2)0.029 (2)−0.0150 (17)−0.0076 (17)0.0064 (17)
C100.030 (2)0.030 (2)0.027 (2)−0.0086 (16)−0.0071 (16)0.0046 (16)
C110.0101 (15)0.0113 (16)0.0160 (15)−0.0021 (12)0.0021 (12)−0.0013 (12)
C120.0203 (17)0.0128 (17)0.0194 (17)−0.0017 (13)0.0050 (13)0.0029 (13)
C130.0177 (17)0.0214 (19)0.0263 (19)0.0037 (14)0.0071 (14)−0.0001 (15)
C140.0195 (18)0.026 (2)0.0230 (18)−0.0019 (14)0.0086 (14)−0.0017 (15)
C150.0249 (19)0.0208 (19)0.0206 (17)−0.0027 (14)0.0051 (14)0.0042 (14)
C160.0216 (18)0.0113 (18)0.0225 (19)0.0015 (13)0.0065 (15)0.0006 (14)
C210.0153 (15)0.0094 (16)0.0124 (15)−0.0020 (12)0.0015 (12)0.0025 (12)
C220.0170 (16)0.0139 (17)0.0170 (16)−0.0016 (13)0.0046 (13)0.0000 (13)
C230.0229 (18)0.0137 (17)0.0240 (17)−0.0065 (13)0.0044 (14)−0.0036 (14)
C240.0291 (19)0.0087 (16)0.0236 (18)0.0034 (13)0.0063 (14)−0.0029 (13)
C250.0186 (17)0.0160 (18)0.0251 (18)0.0054 (13)0.0041 (14)0.0001 (14)
C260.0176 (16)0.0142 (17)0.0163 (16)−0.0019 (12)0.0035 (12)−0.0013 (13)
C310.0136 (16)0.0159 (18)0.0120 (16)−0.0004 (13)0.0020 (12)0.0019 (14)
C320.0178 (17)0.0132 (18)0.0225 (17)−0.0013 (13)0.0026 (13)0.0010 (14)
C330.0227 (18)0.021 (2)0.0282 (19)0.0029 (14)0.0056 (15)−0.0078 (15)
C340.022 (2)0.032 (2)0.0168 (19)−0.0028 (15)0.0097 (16)−0.0019 (16)
C350.0210 (17)0.0212 (19)0.0178 (16)−0.0026 (14)0.0034 (13)0.0030 (14)
C360.0185 (16)0.0130 (17)0.0171 (16)0.0027 (12)0.0026 (13)0.0009 (13)
C410.0145 (16)0.0100 (16)0.0179 (16)0.0015 (12)0.0049 (12)0.0002 (13)
C420.0159 (16)0.0156 (17)0.0192 (16)0.0038 (13)0.0021 (13)0.0019 (13)
C430.0237 (19)0.020 (2)0.030 (2)0.0013 (14)0.0115 (15)−0.0041 (16)
C440.0227 (18)0.0142 (18)0.039 (2)0.0065 (14)0.0132 (16)0.0079 (16)
C450.0247 (19)0.022 (2)0.0245 (18)0.0082 (14)0.0063 (14)0.0113 (15)
C460.0222 (18)0.0205 (19)0.0191 (17)0.0032 (14)0.0021 (14)0.0008 (14)
C510.0165 (17)0.0075 (16)0.0142 (16)−0.0015 (14)0.0009 (13)−0.0018 (14)
C520.0168 (16)0.0193 (18)0.0165 (16)0.0005 (13)0.0030 (13)0.0021 (14)
C530.0293 (19)0.0210 (19)0.0129 (16)−0.0001 (15)0.0033 (14)0.0010 (14)
C540.031 (2)0.0150 (18)0.0218 (18)−0.0013 (14)0.0158 (15)−0.0012 (14)
C550.0204 (19)0.019 (2)0.022 (2)0.0018 (14)0.0081 (16)0.0014 (15)
C560.0178 (16)0.0128 (17)0.0184 (16)−0.0006 (13)0.0017 (13)−0.0007 (13)
C610.0085 (14)0.0116 (16)0.0126 (15)−0.0005 (11)−0.0028 (11)0.0004 (12)
C620.0182 (16)0.0150 (17)0.0174 (16)0.0001 (13)0.0030 (13)0.0017 (13)
C630.0212 (17)0.0093 (16)0.0263 (18)−0.0027 (13)−0.0019 (14)0.0015 (14)
C640.0247 (18)0.0141 (18)0.0215 (17)0.0031 (14)−0.0028 (14)−0.0048 (14)
C650.0151 (16)0.0218 (19)0.0197 (17)0.0032 (13)0.0016 (13)−0.0033 (14)
C660.0166 (16)0.0131 (17)0.0178 (16)−0.0017 (12)0.0013 (13)0.0036 (13)
C710.0098 (15)0.0085 (16)0.0213 (17)−0.0018 (11)0.0025 (13)−0.0012 (13)
C720.0159 (16)0.0160 (18)0.0214 (17)0.0020 (13)0.0043 (13)0.0001 (14)
C730.0171 (17)0.0118 (17)0.036 (2)0.0005 (13)0.0035 (14)0.0096 (15)
C740.0180 (17)0.0115 (18)0.047 (2)0.0050 (13)0.0043 (16)−0.0001 (16)
C750.0254 (19)0.020 (2)0.032 (2)0.0046 (14)0.0049 (15)−0.0057 (16)
C760.0208 (18)0.0157 (18)0.0228 (18)0.0010 (13)0.0033 (14)0.0007 (14)
C810.0172 (16)0.0126 (16)0.0128 (15)0.0037 (12)0.0016 (12)0.0057 (13)
C820.0206 (17)0.0123 (16)0.0163 (16)−0.0002 (13)0.0000 (13)−0.0009 (13)
C830.0265 (19)0.0193 (18)0.0219 (18)0.0061 (14)0.0043 (15)−0.0014 (14)
C840.0128 (15)0.0237 (19)0.0251 (18)0.0083 (14)0.0086 (13)0.0070 (15)
C850.0169 (16)0.0152 (18)0.0254 (18)−0.0008 (13)0.0018 (13)0.0081 (14)
C860.0161 (16)0.0113 (17)0.0172 (16)0.0009 (12)0.0012 (13)0.0000 (13)
N10.0164 (14)0.0105 (14)0.0117 (13)−0.0018 (10)0.0029 (10)0.0025 (11)
N20.0155 (14)0.0094 (14)0.0144 (13)−0.0031 (10)0.0008 (11)0.0002 (11)
F10.0632 (16)0.0221 (13)0.0480 (14)0.0013 (11)0.0298 (12)−0.0063 (11)
F20.0393 (14)0.0381 (14)0.0445 (14)0.0116 (10)0.0078 (11)0.0248 (11)
F30.0222 (11)0.0453 (14)0.0309 (11)−0.0060 (9)0.0019 (9)−0.0027 (10)
F40.0682 (16)0.0261 (13)0.0226 (11)−0.0068 (11)0.0115 (10)−0.0082 (9)
F50.0593 (15)0.0232 (12)0.0223 (11)−0.0004 (10)0.0107 (10)0.0041 (9)
F60.0236 (13)0.089 (2)0.0527 (15)−0.0191 (12)0.0053 (11)0.0092 (14)
F70.0388 (13)0.0365 (14)0.0330 (12)−0.0031 (10)−0.0100 (10)−0.0004 (10)
F80.0283 (11)0.0167 (10)0.0319 (11)0.0016 (8)0.0058 (9)0.0050 (9)
F90.0334 (12)0.0306 (12)0.0323 (12)0.0132 (9)0.0122 (9)0.0028 (9)
F100.0381 (13)0.0467 (15)0.0308 (12)−0.0201 (11)0.0048 (10)−0.0113 (11)
F110.0504 (14)0.0223 (12)0.0369 (12)0.0045 (10)0.0239 (10)0.0066 (10)
F120.0343 (13)0.0212 (12)0.0514 (15)0.0085 (9)0.0224 (11)0.0054 (11)
P10.0111 (4)0.0094 (4)0.0131 (4)−0.0002 (3)0.0021 (3)0.0003 (3)
P20.0131 (4)0.0091 (4)0.0128 (4)−0.0005 (3)0.0024 (3)0.0003 (3)
P30.0139 (4)0.0082 (4)0.0131 (4)0.0003 (3)0.0030 (3)0.0008 (3)
P40.0139 (4)0.0084 (4)0.0130 (4)−0.0007 (3)0.0016 (3)0.0009 (3)
P50.0224 (5)0.0167 (5)0.0244 (5)−0.0013 (3)0.0057 (4)0.0022 (4)
P60.0210 (5)0.0155 (5)0.0243 (5)0.0015 (3)0.0045 (4)−0.0012 (4)
Pt10.01167 (5)0.00794 (5)0.01223 (5)−0.00055 (6)0.00167 (3)0.00060 (6)
Cl10.0451 (6)0.0342 (6)0.0393 (5)0.0035 (5)−0.0036 (5)0.0046 (5)
Cl20.1083 (12)0.0499 (8)0.0559 (8)0.0418 (8)−0.0303 (7)−0.0227 (6)
Cl30.0380 (5)0.0263 (5)0.0310 (5)0.0089 (4)0.0017 (4)0.0022 (4)
Cl4A0.0499 (15)0.098 (2)0.0262 (11)0.0341 (15)0.0077 (10)−0.0048 (12)
C02A0.0335 (18)0.0216 (18)0.0222 (17)0.0036 (14)0.0069 (14)0.0032 (14)
Cl4B0.072 (2)0.081 (2)0.0297 (12)0.0381 (17)0.0039 (12)−0.0141 (13)
C02B0.041 (2)0.031 (2)0.0215 (17)0.0028 (16)0.0065 (15)−0.0015 (15)
Geometric parameters (Å, º) top
C1—N11.481 (4)C43—H430.95
C1—C21.535 (5)C44—C451.381 (5)
C1—H1A0.99C44—H440.95
C1—H1B0.99C45—C461.385 (4)
C01—Cl11.737 (4)C45—H450.95
C01—Cl21.774 (4)C46—H460.95
C01—H01A0.99C51—C561.386 (4)
C01—H01B0.99C51—C521.394 (4)
C2—C31.516 (5)C51—P31.810 (3)
C2—H2A0.99C52—C531.380 (4)
C2—H2B0.99C52—H520.95
C3—C41.533 (5)C53—C541.397 (5)
C3—H3A0.99C53—H530.95
C3—H3B0.99C54—C551.382 (5)
C4—C51.534 (5)C54—H540.95
C4—H4A0.99C55—C561.395 (5)
C4—H4B0.99C55—H550.95
C5—H5A0.98C56—H560.95
C5—H5B0.98C61—C661.393 (4)
C5—H5C0.98C61—C621.405 (4)
C6—N21.493 (4)C61—P31.793 (3)
C6—C71.508 (4)C62—C631.381 (4)
C6—H6A0.99C62—H620.95
C6—H6B0.99C63—C641.383 (5)
C7—C81.539 (4)C63—H630.95
C7—H7A0.99C64—C651.384 (4)
C7—H7B0.99C64—H640.95
C8—C91.527 (5)C65—C661.383 (4)
C8—H8A0.99C65—H650.95
C8—H8B0.99C66—H660.95
C9—C101.531 (5)C71—C761.380 (4)
C9—H9A0.99C71—C721.406 (4)
C9—H9B0.99C71—P41.801 (3)
C10—H10A0.98C72—C731.382 (4)
C10—H10B0.98C72—H720.95
C10—H10C0.98C73—C741.375 (5)
C11—C121.389 (4)C73—H730.95
C11—C161.399 (4)C74—C751.393 (5)
C11—P11.791 (3)C74—H740.95
C12—C131.379 (4)C75—C761.378 (4)
C12—H120.95C75—H750.95
C13—C141.381 (4)C76—H760.95
C13—H130.95C81—C821.393 (4)
C14—C151.387 (5)C81—C861.397 (4)
C14—H140.95C81—P41.794 (3)
C15—C161.381 (4)C82—C831.379 (4)
C15—H150.95C82—H820.95
C16—H160.95C83—C841.382 (5)
C21—C261.395 (4)C83—H830.95
C21—C221.397 (4)C84—C851.378 (4)
C21—P11.795 (3)C84—H840.95
C22—C231.389 (4)C85—C861.387 (4)
C22—H220.95C85—H850.95
C23—C241.378 (5)C86—H860.95
C23—H230.95N1—P21.691 (3)
C24—C251.394 (5)N1—P11.692 (3)
C24—H240.95N2—P41.697 (3)
C25—C261.385 (4)N2—P31.697 (3)
C25—H250.95F1—P51.595 (2)
C26—H260.95F2—P51.599 (2)
C31—C321.389 (4)F3—P51.597 (2)
C31—C361.403 (4)F4—P51.601 (2)
C31—P21.806 (3)F5—P51.591 (2)
C32—C331.390 (4)F6—P51.582 (2)
C32—H320.95F7—P61.595 (2)
C33—C341.380 (5)F8—P61.603 (2)
C33—H330.95F9—P61.598 (2)
C34—C351.382 (5)F10—P61.596 (2)
C34—H340.95F11—P61.599 (2)
C35—C361.391 (4)F12—P61.606 (2)
C35—H350.95P1—Pt12.3063 (8)
C36—H360.95P2—Pt12.2965 (8)
C41—C461.393 (4)P3—Pt12.2994 (8)
C41—C421.397 (4)P4—Pt12.2995 (8)
C41—P21.795 (3)Cl3—C02A1.741 (3)
C42—C431.388 (4)Cl4A—C02A1.687 (4)
C42—H420.95C02A—H02A0.99
C43—C441.378 (5)C02A—H02B0.99
N1—C1—C2113.8 (3)C53—C52—C51120.1 (3)
N1—C1—H1A108.8C53—C52—H52119.9
C2—C1—H1A108.8C51—C52—H52119.9
N1—C1—H1B108.8C52—C53—C54119.7 (3)
C2—C1—H1B108.8C52—C53—H53120.2
H1A—C1—H1B107.7C54—C53—H53120.2
Cl1—C01—Cl2111.0 (2)C55—C54—C53120.2 (3)
Cl1—C01—H01A109.4C55—C54—H54119.9
Cl2—C01—H01A109.4C53—C54—H54119.9
Cl1—C01—H01B109.4C54—C55—C56120.1 (3)
Cl2—C01—H01B109.4C54—C55—H55119.9
H01A—C01—H01B108C56—C55—H55119.9
C3—C2—C1112.1 (3)C51—C56—C55119.5 (3)
C3—C2—H2A109.2C51—C56—H56120.2
C1—C2—H2A109.2C55—C56—H56120.2
C3—C2—H2B109.2C66—C61—C62119.4 (3)
C1—C2—H2B109.2C66—C61—P3119.6 (2)
H2A—C2—H2B107.9C62—C61—P3119.6 (2)
C2—C3—C4114.4 (3)C63—C62—C61119.8 (3)
C2—C3—H3A108.7C63—C62—H62120.1
C4—C3—H3A108.7C61—C62—H62120.1
C2—C3—H3B108.7C62—C63—C64120.2 (3)
C4—C3—H3B108.7C62—C63—H63119.9
H3A—C3—H3B107.6C64—C63—H63119.9
C3—C4—C5112.4 (3)C63—C64—C65120.5 (3)
C3—C4—H4A109.1C63—C64—H64119.8
C5—C4—H4A109.1C65—C64—H64119.8
C3—C4—H4B109.1C66—C65—C64120.0 (3)
C5—C4—H4B109.1C66—C65—H65120
H4A—C4—H4B107.9C64—C65—H65120
C4—C5—H5A109.5C65—C66—C61120.2 (3)
C4—C5—H5B109.5C65—C66—H66119.9
H5A—C5—H5B109.5C61—C66—H66119.9
C4—C5—H5C109.5C76—C71—C72119.4 (3)
H5A—C5—H5C109.5C76—C71—P4122.5 (2)
H5B—C5—H5C109.5C72—C71—P4117.7 (2)
N2—C6—C7114.0 (3)C73—C72—C71120.0 (3)
N2—C6—H6A108.8C73—C72—H72120
C7—C6—H6A108.8C71—C72—H72120
N2—C6—H6B108.8C74—C73—C72119.9 (3)
C7—C6—H6B108.8C74—C73—H73120.1
H6A—C6—H6B107.7C72—C73—H73120.1
C6—C7—C8111.9 (3)C73—C74—C75120.3 (3)
C6—C7—H7A109.2C73—C74—H74119.8
C8—C7—H7A109.2C75—C74—H74119.8
C6—C7—H7B109.2C76—C75—C74120.0 (3)
C8—C7—H7B109.2C76—C75—H75120
H7A—C7—H7B107.9C74—C75—H75120
C9—C8—C7114.7 (3)C75—C76—C71120.3 (3)
C9—C8—H8A108.6C75—C76—H76119.8
C7—C8—H8A108.6C71—C76—H76119.8
C9—C8—H8B108.6C82—C81—C86119.2 (3)
C7—C8—H8B108.6C82—C81—P4120.4 (2)
H8A—C8—H8B107.6C86—C81—P4120.4 (2)
C8—C9—C10111.6 (3)C83—C82—C81120.8 (3)
C8—C9—H9A109.3C83—C82—H82119.6
C10—C9—H9A109.3C81—C82—H82119.6
C8—C9—H9B109.3C82—C83—C84119.4 (3)
C10—C9—H9B109.3C82—C83—H83120.3
H9A—C9—H9B108C84—C83—H83120.3
C9—C10—H10A109.5C85—C84—C83120.8 (3)
C9—C10—H10B109.5C85—C84—H84119.6
H10A—C10—H10B109.5C83—C84—H84119.6
C9—C10—H10C109.5C84—C85—C86120.1 (3)
H10A—C10—H10C109.5C84—C85—H85120
H10B—C10—H10C109.5C86—C85—H85120
C12—C11—C16120.1 (3)C85—C86—C81119.7 (3)
C12—C11—P1119.0 (2)C85—C86—H86120.1
C16—C11—P1120.0 (2)C81—C86—H86120.1
C13—C12—C11120.0 (3)C1—N1—P2129.9 (2)
C13—C12—H12120C1—N1—P1126.7 (2)
C11—C12—H12120P2—N1—P1103.40 (13)
C12—C13—C14119.9 (3)C6—N2—P4127.9 (2)
C12—C13—H13120C6—N2—P3127.2 (2)
C14—C13—H13120P4—N2—P3103.15 (13)
C13—C14—C15120.4 (3)N1—P1—C11109.23 (13)
C13—C14—H14119.8N1—P1—C21108.74 (13)
C15—C14—H14119.8C11—P1—C21108.33 (14)
C16—C15—C14120.2 (3)N1—P1—Pt192.81 (9)
C16—C15—H15119.9C11—P1—Pt1116.03 (10)
C14—C15—H15119.9C21—P1—Pt1120.08 (10)
C15—C16—C11119.3 (3)N1—P2—C41109.61 (14)
C15—C16—H16120.3N1—P2—C31111.84 (15)
C11—C16—H16120.3C41—P2—C31107.14 (15)
C26—C21—C22120.1 (3)N1—P2—Pt193.19 (9)
C26—C21—P1118.8 (2)C41—P2—Pt1118.82 (11)
C22—C21—P1120.8 (2)C31—P2—Pt1115.52 (11)
C23—C22—C21119.2 (3)N2—P3—C61109.63 (14)
C23—C22—H22120.4N2—P3—C51111.60 (14)
C21—C22—H22120.4C61—P3—C51106.41 (15)
C24—C23—C22120.5 (3)N2—P3—Pt193.10 (9)
C24—C23—H23119.7C61—P3—Pt1112.97 (10)
C22—C23—H23119.7C51—P3—Pt1122.28 (11)
C23—C24—C25120.6 (3)N2—P4—C81109.44 (13)
C23—C24—H24119.7N2—P4—C71111.45 (13)
C25—C24—H24119.7C81—P4—C71105.50 (14)
C26—C25—C24119.3 (3)N2—P4—Pt193.11 (9)
C26—C25—H25120.3C81—P4—Pt1118.32 (11)
C24—C25—H25120.3C71—P4—Pt1118.34 (10)
C25—C26—C21120.3 (3)F6—P5—F590.13 (13)
C25—C26—H26119.9F6—P5—F190.59 (14)
C21—C26—H26119.9F5—P5—F189.57 (12)
C32—C31—C36119.7 (3)F6—P5—F3179.62 (16)
C32—C31—P2120.0 (3)F5—P5—F389.88 (12)
C36—C31—P2119.4 (3)F1—P5—F389.79 (12)
C31—C32—C33120.1 (3)F6—P5—F290.89 (13)
C31—C32—H32120F5—P5—F2178.86 (13)
C33—C32—H32120F1—P5—F290.94 (12)
C34—C33—C32119.8 (3)F3—P5—F289.10 (12)
C34—C33—H33120.1F6—P5—F489.92 (14)
C32—C33—H33120.1F5—P5—F490.26 (11)
C33—C34—C35121.0 (3)F1—P5—F4179.46 (15)
C33—C34—H34119.5F3—P5—F489.70 (12)
C35—C34—H34119.5F2—P5—F489.22 (12)
C34—C35—C36119.8 (3)F7—P6—F10179.64 (15)
C34—C35—H35120.1F7—P6—F989.97 (12)
C36—C35—H35120.1F10—P6—F989.67 (12)
C35—C36—C31119.7 (3)F7—P6—F1189.68 (12)
C35—C36—H36120.2F10—P6—F1190.24 (12)
C31—C36—H36120.2F9—P6—F1189.93 (11)
C46—C41—C42119.5 (3)F7—P6—F890.17 (12)
C46—C41—P2121.6 (2)F10—P6—F889.90 (11)
C42—C41—P2118.9 (2)F9—P6—F890.23 (11)
C43—C42—C41120.1 (3)F11—P6—F8179.79 (14)
C43—C42—H42120F7—P6—F1290.42 (13)
C41—C42—H42120F10—P6—F1289.94 (12)
C44—C43—C42120.0 (3)F9—P6—F12179.60 (14)
C44—C43—H43120F11—P6—F1289.97 (11)
C42—C43—H43120F8—P6—F1289.87 (11)
C43—C44—C45120.1 (3)P2—Pt1—P3178.92 (3)
C43—C44—H44120P2—Pt1—P4108.78 (3)
C45—C44—H44120P3—Pt1—P470.64 (3)
C44—C45—C46120.6 (3)P2—Pt1—P170.45 (3)
C44—C45—H45119.7P3—Pt1—P1110.08 (3)
C46—C45—H45119.7P4—Pt1—P1177.37 (3)
C45—C46—C41119.7 (3)Cl4A—C02A—Cl3120.6 (2)
C45—C46—H46120.2Cl4A—C02A—H02A107.2
C41—C46—H46120.2Cl3—C02A—H02A107.2
C56—C51—C52120.3 (3)Cl4A—C02A—H02B107.2
C56—C51—P3119.5 (2)Cl3—C02A—H02B107.2
C52—C51—P3120.2 (2)H02A—C02A—H02B106.8
N1—C1—C2—C3169.4 (3)C16—C11—P1—Pt1−105.0 (2)
C1—C2—C3—C460.4 (4)C26—C21—P1—N1100.9 (2)
C2—C3—C4—C5−177.3 (3)C22—C21—P1—N1−72.6 (3)
N2—C6—C7—C8−177.1 (3)C26—C21—P1—C11−140.5 (2)
C6—C7—C8—C9−62.8 (4)C22—C21—P1—C1146.0 (3)
C7—C8—C9—C10−174.0 (3)C26—C21—P1—Pt1−4.0 (3)
C16—C11—C12—C130.5 (5)C22—C21—P1—Pt1−177.5 (2)
P1—C11—C12—C13−169.1 (2)C1—N1—P2—C4151.9 (3)
C11—C12—C13—C140.3 (5)P1—N1—P2—C41−125.63 (15)
C12—C13—C14—C15−0.7 (5)C1—N1—P2—C31−66.8 (3)
C13—C14—C15—C160.3 (5)P1—N1—P2—C31115.69 (15)
C14—C15—C16—C110.5 (5)C1—N1—P2—Pt1174.1 (3)
C12—C11—C16—C15−0.9 (5)P1—N1—P2—Pt1−3.46 (12)
P1—C11—C16—C15168.6 (3)C46—C41—P2—N1−79.3 (3)
C26—C21—C22—C230.2 (4)C42—C41—P2—N1103.1 (3)
P1—C21—C22—C23173.6 (2)C46—C41—P2—C3142.2 (3)
C21—C22—C23—C240.1 (5)C42—C41—P2—C31−135.4 (3)
C22—C23—C24—C25−0.2 (5)C46—C41—P2—Pt1175.4 (2)
C23—C24—C25—C260.1 (5)C42—C41—P2—Pt1−2.2 (3)
C24—C25—C26—C210.2 (5)C32—C31—P2—N1−40.8 (3)
C22—C21—C26—C25−0.3 (5)C36—C31—P2—N1150.1 (2)
P1—C21—C26—C25−173.8 (2)C32—C31—P2—C41−160.9 (3)
C36—C31—C32—C33−2.1 (5)C36—C31—P2—C4130.0 (3)
P2—C31—C32—C33−171.2 (2)C32—C31—P2—Pt164.1 (3)
C31—C32—C33—C340.9 (5)C36—C31—P2—Pt1−105.0 (2)
C32—C33—C34—C350.2 (5)C6—N2—P3—C61−49.9 (3)
C33—C34—C35—C360.0 (5)P4—N2—P3—C61115.82 (14)
C34—C35—C36—C31−1.2 (5)C6—N2—P3—C5167.7 (3)
C32—C31—C36—C352.2 (5)P4—N2—P3—C51−126.55 (15)
P2—C31—C36—C35171.4 (2)C6—N2—P3—Pt1−165.6 (2)
C46—C41—C42—C43−1.2 (5)P4—N2—P3—Pt10.08 (12)
P2—C41—C42—C43176.5 (3)C66—C61—P3—N2−36.4 (3)
C41—C42—C43—C44−0.7 (5)C62—C61—P3—N2156.9 (2)
C42—C43—C44—C452.8 (5)C66—C61—P3—C51−157.2 (2)
C43—C44—C45—C46−3.0 (5)C62—C61—P3—C5136.1 (3)
C44—C45—C46—C411.1 (5)C66—C61—P3—Pt166.0 (2)
C42—C41—C46—C451.0 (5)C62—C61—P3—Pt1−100.8 (2)
P2—C41—C46—C45−176.6 (3)C56—C51—P3—N2108.6 (3)
C56—C51—C52—C53−0.7 (5)C52—C51—P3—N2−72.3 (3)
P3—C51—C52—C53−179.9 (3)C56—C51—P3—C61−131.9 (3)
C51—C52—C53—C542.4 (5)C52—C51—P3—C6147.3 (3)
C52—C53—C54—C55−2.4 (5)C56—C51—P3—Pt10.0 (3)
C53—C54—C55—C560.8 (5)C52—C51—P3—Pt1179.1 (2)
C52—C51—C56—C55−0.9 (5)C6—N2—P4—C8143.9 (3)
P3—C51—C56—C55178.3 (2)P3—N2—P4—C81−121.62 (15)
C54—C55—C56—C510.8 (5)C6—N2—P4—C71−72.4 (3)
C66—C61—C62—C63−0.2 (4)P3—N2—P4—C71122.07 (15)
P3—C61—C62—C63166.6 (2)C6—N2—P4—Pt1165.5 (2)
C61—C62—C63—C640.5 (5)P3—N2—P4—Pt1−0.08 (12)
C62—C63—C64—C650.2 (5)C82—C81—P4—N295.9 (3)
C63—C64—C65—C66−1.2 (5)C86—C81—P4—N2−83.0 (3)
C64—C65—C66—C611.5 (4)C82—C81—P4—C71−144.1 (2)
C62—C61—C66—C65−0.8 (4)C86—C81—P4—C7137.0 (3)
P3—C61—C66—C65−167.6 (2)C82—C81—P4—Pt1−8.9 (3)
C76—C71—C72—C731.4 (5)C86—C81—P4—Pt1172.2 (2)
P4—C71—C72—C73173.8 (2)C76—C71—P4—N2−26.7 (3)
C71—C72—C73—C742.1 (5)C72—C71—P4—N2161.2 (2)
C72—C73—C74—C75−3.6 (5)C76—C71—P4—C81−145.4 (3)
C73—C74—C75—C761.5 (5)C72—C71—P4—C8142.5 (3)
C74—C75—C76—C712.1 (5)C76—C71—P4—Pt179.5 (3)
C72—C71—C76—C75−3.5 (5)C72—C71—P4—Pt1−92.7 (2)
P4—C71—C76—C75−175.5 (3)N1—P2—Pt1—P4179.95 (9)
C86—C81—C82—C83−0.3 (4)C41—P2—Pt1—P4−65.57 (12)
P4—C81—C82—C83−179.2 (2)C31—P2—Pt1—P463.88 (13)
C81—C82—C83—C84−0.4 (5)N1—P2—Pt1—P12.62 (9)
C82—C83—C84—C851.3 (5)C41—P2—Pt1—P1117.10 (12)
C83—C84—C85—C86−1.5 (5)C31—P2—Pt1—P1−113.45 (13)
C84—C85—C86—C810.7 (5)N2—P3—Pt1—P4−0.06 (9)
C82—C81—C86—C850.2 (4)C61—P3—Pt1—P4−112.91 (11)
P4—C81—C86—C85179.1 (2)C51—P3—Pt1—P4117.99 (14)
C2—C1—N1—P281.3 (4)N2—P3—Pt1—P1177.25 (9)
C2—C1—N1—P1−101.7 (3)C61—P3—Pt1—P164.40 (11)
C7—C6—N2—P4102.6 (3)C51—P3—Pt1—P1−64.70 (14)
C7—C6—N2—P3−95.2 (3)N2—P4—Pt1—P2−178.97 (9)
C1—N1—P1—C11−55.3 (3)C81—P4—Pt1—P2−64.89 (12)
P2—N1—P1—C11122.28 (14)C71—P4—Pt1—P264.58 (12)
C1—N1—P1—C2162.7 (3)N2—P4—Pt1—P30.06 (9)
P2—N1—P1—C21−119.69 (15)C81—P4—Pt1—P3114.14 (11)
C1—N1—P1—Pt1−174.2 (3)C71—P4—Pt1—P3−116.39 (12)
P2—N1—P1—Pt13.44 (12)N1—P1—Pt1—P2−2.62 (9)
C12—C11—P1—N1−38.5 (3)C11—P1—Pt1—P2−115.62 (12)
C16—C11—P1—N1151.8 (2)C21—P1—Pt1—P2110.97 (11)
C12—C11—P1—C21−156.8 (2)N1—P1—Pt1—P3178.39 (9)
C16—C11—P1—C2133.5 (3)C11—P1—Pt1—P365.38 (12)
C12—C11—P1—Pt164.7 (3)C21—P1—Pt1—P3−68.03 (12)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C25—H25···F80.952.533.437 (4)160
C55—H55···F20.952.493.079 (4)120
C65—H65···F100.952.473.297 (4)145
C83—H83···F110.952.373.267 (4)158
C01—H01B···F2i0.992.293.244 (5)161
C01—H01B···F6i0.992.43.150 (5)132
C5—H5C···F11ii0.982.513.196 (4)127
C8—H8A···F3iii0.992.543.450 (4)153
C53—H53···F7iv0.952.513.273 (4)137
C63—H63···F4v0.952.513.373 (4)151
C73—H73···F9vi0.952.533.426 (4)156
Symmetry codes: (i) x+1/2, −y+3/2, z−1/2; (ii) x−1, y, z; (iii) x+1, y, z; (iv) x, −y+1, z+1/2; (v) x+1/2, y−1/2, z; (vi) x−1/2, y+1/2, z.

Experimental details

Crystal data
Chemical formula[Pt(C29H31NP2)2](PF6)2·2CH2Cl2
Mr1565.85
Crystal system, space groupMonoclinic, Cc
Temperature (K)100
a, b, c (Å)11.3876 (10), 24.283 (3), 23.102 (2)
β (°) 97.669 (4)
V (Å3)6331.1 (11)
Z4
Radiation typeMo Kα
µ (mm−1)2.61
Crystal size (mm)0.26 × 0.19 × 0.13
Data collection
DiffractometerBruker X8 APEXII 4K Kappa CCD
Absorption correctionMulti-scan
(SADABS; Bruker, 2004)
Tmin, Tmax0.550, 0.728
No. of measured, independent and
observed [I > 2σ(I)] reflections		47664, 14210, 13180
Rint0.03
(sin θ/λ)max (Å−1)0.661
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.024, 0.047, 0.89
No. of reflections14210
No. of parameters767
No. of restraints2
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)1.08, −1.13
Absolute structureFlack (1983), 6561 Friedel pairs
Absolute structure parameter0.014 (2)

Computer programs: APEX2 (Bruker, 2010), SAINT-Plus (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg & Putz, 2005), WinGX (Farrugia, 1999).

Selected geometric parameters (Å, º) top
P1—Pt12.3063 (8)P3—Pt12.2994 (8)
P2—Pt12.2965 (8)P4—Pt12.2995 (8)
P2—N1—P1103.40 (13)C41—P2—Pt1118.82 (11)
P4—N2—P3103.15 (13)C51—P3—Pt1122.28 (11)
N1—P1—Pt192.81 (9)N2—P4—Pt193.11 (9)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C25—H25···F80.952.533.437 (4)159.6
C55—H55···F20.952.493.079 (4)120.3
C65—H65···F100.952.473.297 (4)145.1
C83—H83···F110.952.373.267 (4)157.6
C01—H01B···F2i0.992.293.244 (5)160.5
C01—H01B···F6i0.992.43.150 (5)132.3
C5—H5C···F11ii0.982.513.196 (4)126.9
C8—H8A···F3iii0.992.543.450 (4)152.5
C53—H53···F7iv0.952.513.273 (4)137.3
C63—H63···F4v0.952.513.373 (4)151
C73—H73···F9vi0.952.533.426 (4)156.3
Symmetry codes: (i) x+1/2, −y+3/2, z−1/2; (ii) x−1, y, z; (iii) x+1, y, z; (iv) x, −y+1, z+1/2; (v) x+1/2, y−1/2, z; (vi) x−1/2, y+1/2, z.
 

Acknowledgements

Financial assistance from the Department of Science and Technology (DST) of South Africa, the South African National Research Foundation (NRF), as well as the DST–NRF centre of excellence (c*change) and the University of the Free State are gratefully acknowledged.

References

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ISSN: 2056-9890
Volume 66| Part 8| August 2010| Pages m922-m923
https://doi.org/10.1107/S1600536810025560
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