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ISSN: 2056-9890

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

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

(Received 9 July 2010; accepted 19 July 2010; online 24 July 2010)

In the title compound, [Pt(C30H31NP2)2](PF6)2·2CH2Cl2, the four-coordinated PtII atom, situated on an inversion centre, exhibits a highly distorted square-planar geometry illustrated by the P—Pt—P bite angle of 70.76 (3)°. The cyclo­hexyl ring and one of the phenyl rings display 0.630 (7):0.37 (7) and 0.60 (2):0.40 (2) positional disorder, respectively. The dichloro­methane solvent mol­ecule displays 0.526 (4):0.474 (4) positional disorder. C—H⋯F hydrogen bonds stabilize the crystal packing.

Related literature

For applications of Pt(II) diphosphinoamine complexes in homogeneous catalysis, see: Brink et al. (2010[Brink, A., Visser, H. G., Steyl, G. & Roodt, A. (2010). Dalton Trans. pp. 5572-5578.]); 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.]); 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.], 2008[Steyn, M., Roodt, A. & Steyl, G. (2008). Acta Cryst. E64, m827.]); 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, m1367-m1368.],b[Viljoen, J. A., Visser, H. G., Roodt, A. & Steyn, M. (2009b). Acta Cryst. E65, m1514-m1515.], 2010[Viljoen, J. A., Visser, H. G. & Roodt, A. (2010). Acta Cryst. E66, m603-m604.]). For related platinum(II) complexes, see: Cloete et al. (2010[Cloete, N., Visser, H. G. & Roodt, A. (2010). Acta Cryst. E66, m51-m52.]); Dyson et al. (2004[Dyson, P. J., Fei, Z. & Scopelliti, R. (2004). Eur. J. Inorg. Chem. pp. 530-537.]); Engelbrecht et al. (2010[Engelbrecht, I., Visser, H. G. & Roodt, A. (2010). Acta Cryst. E66, m922-m923.]); Farrar & Browning (1995[Farrar, D. G. & Browning, C. S. (1995). J. Chem. Soc. Dalton Trans. pp. 521-530.]). For related diphenyl­phosphino ligands, see: 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.]); Keat et al. (1981[Keat, R., Manojlovic-Muir, L., Muir, K. W. & Rycroft, D. S. (1981). J. Chem. Soc. Dalton Trans. pp. 2192-2198.]).

[Scheme 1]

Experimental

Crystal data
  • [Pt(C30H31NP2)2](PF6)2·2CH2Cl2

  • Mr = 1588.38

  • Monoclinic, P 21 /c

  • a = 13.350 (5) Å

  • b = 18.764 (4) Å

  • c = 15.248 (5) Å

  • β = 123.333 (5)°

  • V = 3191.3 (17) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 2.59 mm−1

  • T = 100 K

  • 0.32 × 0.29 × 0.14 mm

Data collection
  • Bruker X8 APEXII KappaCCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2001[Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.491, Tmax = 0.713

  • 57085 measured reflections

  • 7899 independent reflections

  • 6367 reflections with I > 2σ(I)

  • Rint = 0.042

Refinement
  • R[F2 > 2σ(F2)] = 0.027

  • wR(F2) = 0.070

  • S = 1.03

  • 7899 reflections

  • 503 parameters

  • 18 restraints

  • H-atom parameters constrained

  • Δρmax = 0.72 e Å−3

  • Δρmin = −0.99 e Å−3

Table 1
Selected bond lengths (Å)

Pt1—P1 2.2918 (9)
Pt1—P2 2.2999 (9)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
C12A—H12A⋯F2 0.95 2.45 3.186 (11) 134
C32—H32⋯F2 0.95 2.47 3.138 (4) 127

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2 and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2007[Bruker (2007). APEX2 and SAINT-Plus. 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, 1999[Brandenburg, K. & Putz, H. (1999). 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


Comment top

The synthesis of Pt(II) diphosphinoamine complexes forms part of ongoing research in our group in the field of homogeneous catalysis (Brink et al., 2010; Otto et al., 1998; Roodt & Steyn, 2000; Steyn et al., 1992, 1997, 2008; Viljoen et al., 2008, 2009a,b, 2010). In the title compound (Fig. 1, Table 1), the PtII atom is situated on an inversion centre. The strain in the complex is illustrated by the distorted square-planar geometry around the Pt atom, with a P—Pt—P bite angle of 70.76 (3)°, forcing the P1–N1–P2 angle to 102.58 (12)° and demonstrating the deviation from the ideal tetrahedral geometry of the N atom. The N atom is displaced by 0.166 (3) and -0.081 (3) Å from the C1A, P1, P2 and C1B, P1, P2 planes respectively, showing that the N atom adopts an almost planar geometry with the two P atoms and the C atom attached to it to accomodate the steric bulk of the phenyl groups and the cyclohexyl ring of the ligand. The P atoms are also severely distorted from the expected tetrahedral configuration with Pt1—P1—N1 and Pt1—P2—N1 angles being 93.47 (8) and 93.08 (9)°, respectively. The cyclohexyl ring, bonded to the N atom, and the C11-phenyl ring, bonded to P1, display 0.63:0.37 and 0.60:0.40 positional disorder, respectively. The dichloromethane molecules display 0.53:0.47 positional disorder (Fig. 2). Molecules of the title compound pack in horizontal rows across the bc plane in the unit cell (Fig. 3). Intermolecular hydrogen bonds exist between C12A—H12A and F2 and C32—H32 and F2 (Table 2).

Related literature top

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

Experimental top

Pt(cod)Cl2 (20 mg, 0.054 mmol) (cod = 1,5-cyclooctadiene) dissolved in a minimum amount of dichloromethane was added in a rapid dropwise manner to a solution of bis(diphenylphosphino)cyclohexylamine (52.5 mg, 0.112 mmol) and NaPF6 (19.8 mg, 0.118 mmol) dissolved in a 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). Layering of a dichloromethane solution of the product with methanol gave colourless crystals, suitable for X-ray diffraction (crude yield: 44 mg, 73%). Spectroscopy data: 1H NMR (600 MHz, CD2Cl2): δ = 0.6 to 1.4 (m, 18H), 3.1 (m, 2H), 3.6 (m, 2H), 7.4 to 7.7 (m, 20H). 31P NMR (243 MHz, CD2Cl2): δ = 39.9 (t, 1JPt—P = 1062.0 Hz), -135.2 to -152.7 (m, PF6).

Refinement top

H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.95 (aromatic), 1.00 (CH) and 0.99 (CH2) Å and Uiso(H) = 1.2Ueq(C). The highest residual peak is located 0.15 Å from CL1A and the deepest hole is situated 0.56 Å from CL1B.

Structure description top

The synthesis of Pt(II) diphosphinoamine complexes forms part of ongoing research in our group in the field of homogeneous catalysis (Brink et al., 2010; Otto et al., 1998; Roodt & Steyn, 2000; Steyn et al., 1992, 1997, 2008; Viljoen et al., 2008, 2009a,b, 2010). In the title compound (Fig. 1, Table 1), the PtII atom is situated on an inversion centre. The strain in the complex is illustrated by the distorted square-planar geometry around the Pt atom, with a P—Pt—P bite angle of 70.76 (3)°, forcing the P1–N1–P2 angle to 102.58 (12)° and demonstrating the deviation from the ideal tetrahedral geometry of the N atom. The N atom is displaced by 0.166 (3) and -0.081 (3) Å from the C1A, P1, P2 and C1B, P1, P2 planes respectively, showing that the N atom adopts an almost planar geometry with the two P atoms and the C atom attached to it to accomodate the steric bulk of the phenyl groups and the cyclohexyl ring of the ligand. The P atoms are also severely distorted from the expected tetrahedral configuration with Pt1—P1—N1 and Pt1—P2—N1 angles being 93.47 (8) and 93.08 (9)°, respectively. The cyclohexyl ring, bonded to the N atom, and the C11-phenyl ring, bonded to P1, display 0.63:0.37 and 0.60:0.40 positional disorder, respectively. The dichloromethane molecules display 0.53:0.47 positional disorder (Fig. 2). Molecules of the title compound pack in horizontal rows across the bc plane in the unit cell (Fig. 3). Intermolecular hydrogen bonds exist between C12A—H12A and F2 and C32—H32 and F2 (Table 2).

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

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 1999); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. Molecular structure of the complex cation in the title compound. Displacement ellipsoids are drawn at the 50% probability level. Dashed lines denote the bonds between the minor disordered atoms. H atoms, solvent molecules and hexafluorophosphate anions have been omitted for clarity. [Symmetry code: (i) 1-x, 1-y, 1-z.]
[Figure 2] Fig. 2. A view of the solvent molecules and hexafluorophosphate anions. Displacement ellipsoids are drawn at the 50% probability level. H atoms have been omitted for clarity. [Symmetry code: (i) 1-x, 1-y, 1-z.]
[Figure 3] Fig. 3. Perspective view of the unit cell of the title compound along the a axis. H atoms, solvent molecules and hexafluorophosphate anions have been omitted for clarity.
Bis[N,N-bis(diphenylphosphanyl)cyclohexylamine- κ2P,P']platinum(II) bis(hexafluoridophosphate) dichloromethane disolvate top
Crystal data top
[Pt(C30H31NP2)2](PF6)2·2CH2Cl2F(000) = 1589
Mr = 1588.38Dx = 1.653 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ybcCell parameters from 9230 reflections
a = 13.350 (5) Åθ = 2.8–28.2°
b = 18.764 (4) ŵ = 2.59 mm1
c = 15.248 (5) ÅT = 100 K
β = 123.333 (5)°Cuboid, colourless
V = 3191.3 (17) Å30.32 × 0.29 × 0.14 mm
Z = 2
Data collection top
Bruker X8 APEXII KappaCCD
diffractometer
7899 independent reflections
Radiation source: fine-focus sealed tube6367 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
ω and φ scansθmax = 28.4°, θmin = 4.2°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 1317
Tmin = 0.491, Tmax = 0.713k = 2524
57085 measured reflectionsl = 2020
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.070H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0297P)2 + 4.9393P]
where P = (Fo2 + 2Fc2)/3
7899 reflections(Δ/σ)max = 0.003
503 parametersΔρmax = 0.72 e Å3
18 restraintsΔρmin = 0.99 e Å3
Crystal data top
[Pt(C30H31NP2)2](PF6)2·2CH2Cl2V = 3191.3 (17) Å3
Mr = 1588.38Z = 2
Monoclinic, P21/cMo Kα radiation
a = 13.350 (5) ŵ = 2.59 mm1
b = 18.764 (4) ÅT = 100 K
c = 15.248 (5) Å0.32 × 0.29 × 0.14 mm
β = 123.333 (5)°
Data collection top
Bruker X8 APEXII KappaCCD
diffractometer
7899 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
6367 reflections with I > 2σ(I)
Tmin = 0.491, Tmax = 0.713Rint = 0.042
57085 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02718 restraints
wR(F2) = 0.070H-atom parameters constrained
S = 1.03Δρmax = 0.72 e Å3
7899 reflectionsΔρmin = 0.99 e Å3
503 parameters
Special details top

Experimental. The intensity data was collected on a Bruker X8 ApexII 4 K Kappa CCD diffractometer using an exposure time of 5 s/frame. A total of 1847 frames were collected with a frame width of 0.5° covering up to θ = 28.36° with 99.1% completeness accomplished.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C1A0.7123 (8)0.5220 (6)0.8424 (9)0.0219 (18)0.630 (7)
H1A0.66990.55990.85620.026*0.630 (7)
C2A0.8441 (5)0.5445 (3)0.8991 (3)0.0299 (14)0.630 (7)
H2A10.88890.5090.88560.036*0.630 (7)
H2A20.84970.59110.87150.036*0.630 (7)
C3A0.8998 (7)0.5504 (4)1.0172 (5)0.0391 (16)0.630 (7)
H3A10.8610.591.03080.047*0.630 (7)
H3A20.98610.56181.05290.047*0.630 (7)
C4A0.8855 (6)0.4809 (3)1.0631 (4)0.0405 (17)0.630 (7)
H4A10.93240.44261.05720.049*0.630 (7)
H4A20.91780.48791.13850.049*0.630 (7)
C5A0.7558 (9)0.4589 (5)1.0064 (8)0.036 (2)0.630 (7)
H5A10.71050.4941.020.043*0.630 (7)
H5A20.74960.41191.03270.043*0.630 (7)
C6A0.7028 (19)0.4544 (9)0.8898 (17)0.0228 (17)0.630 (7)
H6A10.74390.41590.8770.027*0.630 (7)
H6A20.61720.44120.85360.027*0.630 (7)
C1B0.7520 (13)0.5190 (12)0.8490 (17)0.024 (3)0.370 (7)
H1B0.8310.50480.86150.029*0.370 (7)
C2B0.7677 (8)0.5875 (5)0.9006 (6)0.028 (2)0.370 (7)
H2B10.68970.60440.88620.034*0.370 (7)
H2B20.7980.62340.8730.034*0.370 (7)
C3B0.8569 (9)0.5787 (6)1.0188 (7)0.029 (2)0.370 (7)
H3B10.93670.56731.03250.035*0.370 (7)
H3B20.86370.62451.05390.035*0.370 (7)
C4B0.8217 (10)0.5209 (6)1.0662 (7)0.040 (3)0.370 (7)
C5B0.7999 (16)0.4511 (10)1.0077 (15)0.038 (4)0.370 (7)
H5B10.7730.41511.03790.045*0.370 (7)
H5B20.87710.43441.02020.045*0.370 (7)
C6B0.705 (4)0.455 (2)0.886 (3)0.040 (3)0.370 (7)
H6B10.6240.46430.86990.048*0.370 (7)
H6B20.70370.40940.85150.048*0.370 (7)
C11A0.509 (3)0.6467 (9)0.648 (2)0.0207 (12)0.60 (2)
C16A0.3952 (15)0.6778 (12)0.594 (2)0.0273 (8)0.60 (2)
H16A0.32610.64840.56540.033*0.60 (2)
C15A0.3821 (12)0.7511 (12)0.5829 (14)0.030 (3)0.60 (2)
H15A0.30450.77190.54430.035*0.60 (2)
C14A0.4835 (9)0.7935 (5)0.6283 (11)0.040 (2)0.60 (2)
H14A0.47570.84390.62310.048*0.60 (2)
C13A0.5958 (7)0.7629 (4)0.6811 (13)0.048 (4)0.60 (2)
H13A0.66490.79250.71210.058*0.60 (2)
C12A0.6090 (9)0.6895 (5)0.6894 (11)0.036 (2)0.60 (2)
H12A0.68660.66870.72330.044*0.60 (2)
C11B0.506 (5)0.6450 (13)0.655 (3)0.0207 (12)0.40 (2)
C12B0.6086 (14)0.6845 (7)0.7260 (12)0.022 (2)0.40 (2)
H12B0.68370.66110.76820.027*0.40 (2)
C13B0.6009 (9)0.7572 (5)0.7357 (13)0.030 (3)0.40 (2)
H13B0.670.78390.78490.036*0.40 (2)
C14B0.4914 (12)0.7906 (6)0.6727 (14)0.028 (3)0.40 (2)
H14B0.48610.84080.67660.034*0.40 (2)
C15B0.390 (2)0.7519 (18)0.604 (2)0.030 (3)0.40 (2)
H15B0.31420.77510.56470.035*0.40 (2)
C16B0.398 (2)0.6792 (19)0.594 (3)0.0273 (8)0.40 (2)
H16B0.32870.6530.54450.033*0.40 (2)
C210.4170 (3)0.51739 (15)0.6806 (2)0.0222 (6)
C220.4104 (3)0.55086 (17)0.7594 (2)0.0279 (7)
H220.45580.59270.79230.034*
C230.3373 (3)0.52266 (19)0.7891 (3)0.0335 (7)
H230.33360.54490.84320.04*
C240.2697 (3)0.46216 (18)0.7400 (2)0.0312 (7)
H240.21990.4430.76080.037*
C250.2743 (3)0.42946 (17)0.6607 (2)0.0276 (7)
H250.22650.38860.62630.033*
C260.3486 (3)0.45657 (16)0.6320 (2)0.0241 (6)
H260.35320.43350.57880.029*
C310.8129 (3)0.50637 (15)0.6510 (2)0.0208 (6)
C320.8465 (3)0.57719 (16)0.6751 (2)0.0286 (7)
H320.80870.60670.69930.034*
C330.9353 (3)0.60518 (18)0.6641 (3)0.0377 (8)
H330.95930.65350.68210.045*
C340.9887 (3)0.56276 (18)0.6270 (3)0.0333 (7)
H341.04860.58210.61840.04*
C350.9553 (3)0.49219 (17)0.6021 (3)0.0300 (7)
H350.99190.46330.57620.036*
C360.8685 (3)0.46348 (16)0.6149 (2)0.0234 (6)
H360.84690.41470.59920.028*
C410.7127 (3)0.38095 (14)0.6872 (2)0.0215 (6)
C420.8280 (3)0.35531 (16)0.7592 (2)0.0255 (6)
H420.89520.38590.78470.031*
C430.8445 (3)0.28564 (17)0.7933 (2)0.0317 (7)
H430.9230.26830.84240.038*
C440.7477 (4)0.24134 (18)0.7563 (3)0.0406 (9)
H440.75930.19350.78050.049*
C450.6336 (4)0.26580 (19)0.6842 (3)0.0455 (9)
H450.5670.23460.65850.055*
C460.6156 (3)0.33545 (16)0.6491 (3)0.0321 (7)
H460.53690.35210.5990.039*
N10.6583 (2)0.52112 (12)0.72778 (17)0.0206 (5)
F11.0498 (2)0.69802 (10)0.96793 (16)0.0490 (6)
F20.8895 (2)0.71702 (11)0.80417 (17)0.0544 (6)
F30.9056 (2)0.77212 (16)0.9418 (2)0.0720 (8)
F40.9237 (2)0.83448 (11)0.82524 (17)0.0555 (6)
F51.0843 (2)0.81596 (12)0.98976 (18)0.0632 (7)
F61.0704 (2)0.76089 (16)0.8535 (2)0.0741 (8)
P10.51549 (7)0.55043 (4)0.64387 (5)0.01807 (14)
P20.68416 (6)0.47263 (4)0.64749 (5)0.01702 (14)
P30.98835 (7)0.76603 (4)0.89695 (6)0.02531 (17)
Pt10.50.50.50.01390 (5)
Cl1A0.2941 (3)0.24968 (16)1.0253 (3)0.0898 (11)0.526 (4)
Cl2A0.4137 (3)0.36092 (12)0.98377 (18)0.0645 (8)0.526 (4)
C01A0.3384 (12)0.2783 (6)0.9426 (8)0.088 (4)0.526 (4)
H01A0.26690.2830.87010.105*0.526 (4)
H01B0.39210.24220.94190.105*0.526 (4)
Cl1B0.3117 (2)0.20374 (13)1.00257 (18)0.0514 (8)*0.474 (4)
Cl2B0.3439 (3)0.35456 (12)0.9852 (2)0.0534 (7)0.474 (4)
C01B0.2399 (8)0.2844 (4)0.9415 (7)0.049 (2)0.474 (4)
H01C0.19820.27940.86440.058*0.474 (4)
H01D0.1790.29560.95740.058*0.474 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C1A0.023 (5)0.024 (3)0.010 (3)0.008 (4)0.004 (4)0.001 (2)
C2A0.028 (3)0.033 (3)0.014 (2)0.007 (2)0.002 (2)0.0017 (19)
C3A0.040 (4)0.041 (4)0.020 (3)0.004 (3)0.006 (3)0.005 (3)
C4A0.054 (4)0.040 (3)0.015 (2)0.007 (3)0.011 (3)0.005 (2)
C5A0.065 (7)0.030 (4)0.024 (3)0.000 (4)0.032 (5)0.002 (2)
C6A0.036 (4)0.021 (3)0.019 (4)0.001 (3)0.019 (3)0.003 (2)
C1B0.012 (8)0.039 (6)0.012 (5)0.002 (7)0.000 (7)0.003 (4)
C2B0.031 (5)0.035 (5)0.014 (4)0.005 (4)0.010 (4)0.003 (3)
C3B0.027 (5)0.044 (6)0.008 (4)0.002 (4)0.005 (4)0.004 (4)
C4B0.043 (6)0.056 (6)0.017 (4)0.002 (5)0.014 (4)0.004 (4)
C5B0.057 (11)0.042 (7)0.033 (6)0.008 (7)0.037 (8)0.008 (5)
C6B0.043 (6)0.056 (6)0.017 (4)0.002 (5)0.014 (4)0.004 (4)
C11A0.027 (2)0.0199 (15)0.019 (3)0.0022 (14)0.0149 (19)0.0038 (15)
C16A0.0252 (17)0.0286 (17)0.0296 (16)0.0017 (14)0.0161 (15)0.0051 (14)
C15A0.031 (2)0.0288 (18)0.030 (7)0.0092 (19)0.018 (3)0.002 (4)
C14A0.049 (4)0.022 (3)0.052 (6)0.007 (3)0.029 (5)0.001 (4)
C13A0.034 (4)0.025 (3)0.070 (9)0.006 (3)0.018 (4)0.012 (4)
C12A0.025 (3)0.025 (3)0.046 (6)0.000 (3)0.011 (4)0.010 (4)
C11B0.027 (2)0.0199 (15)0.019 (3)0.0022 (14)0.0149 (19)0.0038 (15)
C12B0.032 (5)0.017 (4)0.024 (6)0.001 (3)0.019 (5)0.003 (4)
C13B0.035 (5)0.023 (4)0.030 (7)0.006 (4)0.017 (5)0.012 (4)
C14B0.038 (6)0.016 (4)0.039 (8)0.001 (4)0.027 (6)0.006 (5)
C15B0.031 (2)0.0288 (18)0.030 (7)0.0092 (19)0.018 (3)0.002 (4)
C16B0.0252 (17)0.0286 (17)0.0296 (16)0.0017 (14)0.0161 (15)0.0051 (14)
C210.0253 (15)0.0255 (14)0.0212 (14)0.0019 (12)0.0163 (13)0.0016 (11)
C220.0345 (18)0.0308 (16)0.0248 (15)0.0004 (14)0.0203 (14)0.0038 (12)
C230.039 (2)0.0436 (18)0.0295 (17)0.0050 (16)0.0266 (16)0.0002 (14)
C240.0257 (17)0.042 (2)0.0318 (17)0.0063 (14)0.0198 (15)0.0111 (14)
C250.0208 (15)0.0318 (16)0.0275 (15)0.0008 (13)0.0116 (13)0.0047 (13)
C260.0255 (16)0.0252 (15)0.0227 (14)0.0006 (12)0.0140 (13)0.0008 (11)
C310.0173 (13)0.0249 (14)0.0163 (12)0.0023 (11)0.0067 (11)0.0010 (11)
C320.0370 (18)0.0249 (15)0.0320 (16)0.0060 (13)0.0241 (15)0.0056 (13)
C330.044 (2)0.0319 (17)0.045 (2)0.0157 (16)0.0294 (18)0.0077 (15)
C340.0286 (17)0.0397 (19)0.0355 (18)0.0063 (14)0.0201 (15)0.0035 (14)
C350.0228 (15)0.0404 (19)0.0280 (16)0.0037 (14)0.0147 (14)0.0039 (13)
C360.0191 (14)0.0239 (15)0.0234 (14)0.0027 (12)0.0092 (12)0.0015 (12)
C410.0284 (15)0.0186 (13)0.0186 (13)0.0023 (12)0.0137 (12)0.0007 (10)
C420.0322 (17)0.0258 (15)0.0198 (14)0.0026 (13)0.0152 (13)0.0017 (11)
C430.0397 (19)0.0331 (17)0.0240 (15)0.0123 (15)0.0186 (15)0.0094 (13)
C440.055 (2)0.0254 (17)0.045 (2)0.0091 (16)0.0297 (19)0.0127 (15)
C450.047 (2)0.0271 (18)0.056 (2)0.0065 (16)0.024 (2)0.0057 (16)
C460.0327 (18)0.0223 (15)0.0345 (17)0.0024 (13)0.0142 (15)0.0014 (13)
N10.0277 (13)0.0195 (11)0.0122 (11)0.0019 (10)0.0094 (10)0.0025 (9)
F10.0658 (15)0.0295 (10)0.0423 (12)0.0081 (10)0.0237 (11)0.0069 (9)
F20.0586 (15)0.0359 (11)0.0416 (12)0.0169 (10)0.0104 (11)0.0100 (9)
F30.0660 (17)0.098 (2)0.0795 (18)0.0130 (15)0.0571 (16)0.0007 (16)
F40.0587 (15)0.0308 (11)0.0434 (12)0.0029 (10)0.0068 (11)0.0053 (9)
F50.0654 (16)0.0408 (13)0.0424 (13)0.0176 (11)0.0036 (12)0.0055 (10)
F60.0680 (17)0.105 (2)0.0836 (19)0.0132 (16)0.0631 (16)0.0188 (16)
P10.0247 (4)0.0178 (3)0.0151 (3)0.0015 (3)0.0131 (3)0.0026 (3)
P20.0191 (4)0.0164 (3)0.0139 (3)0.0011 (3)0.0079 (3)0.0012 (3)
P30.0242 (4)0.0221 (4)0.0284 (4)0.0023 (3)0.0136 (3)0.0016 (3)
Pt10.01666 (8)0.01500 (7)0.01119 (7)0.00172 (6)0.00838 (6)0.00207 (5)
Cl1A0.129 (3)0.0727 (19)0.105 (2)0.0276 (17)0.087 (2)0.0308 (16)
Cl2A0.087 (2)0.0546 (13)0.0543 (13)0.0015 (13)0.0400 (14)0.0013 (10)
C01A0.122 (10)0.081 (7)0.066 (6)0.027 (7)0.055 (7)0.025 (5)
Cl2B0.0664 (18)0.0422 (12)0.0650 (15)0.0022 (11)0.0447 (14)0.0095 (10)
C01B0.048 (5)0.041 (5)0.041 (5)0.007 (4)0.014 (4)0.010 (4)
Geometric parameters (Å, º) top
C1A—N11.480 (12)C15B—H15B0.95
C1A—C6A1.50 (2)C16B—H16B0.95
C1A—C2A1.533 (10)C21—C261.393 (4)
C1A—H1A1.00C21—C221.400 (4)
C2A—C3A1.529 (7)C21—P11.799 (3)
C2A—H2A10.99C22—C231.387 (4)
C2A—H2A20.99C22—H220.95
C3A—C4A1.540 (9)C23—C241.386 (5)
C3A—H3A10.99C23—H230.95
C3A—H3A20.99C24—C251.386 (4)
C4A—C5A1.508 (12)C24—H240.95
C4A—H4A10.99C25—C261.384 (4)
C4A—H4A20.99C25—H250.95
C5A—C6A1.51 (2)C26—H260.95
C5A—H5A10.99C31—C321.386 (4)
C5A—H5A20.99C31—C361.398 (4)
C6A—H6A10.99C31—P21.804 (3)
C6A—H6A20.99C32—C331.389 (4)
C1B—C2B1.46 (2)C32—H320.95
C1B—N11.56 (2)C33—C341.381 (5)
C1B—C6B1.60 (5)C33—H330.95
C1B—H1B1.00C34—C351.382 (4)
C2B—C3B1.528 (11)C34—H340.95
C2B—H2B10.99C35—C361.385 (4)
C2B—H2B20.99C35—H350.95
C3B—C4B1.514 (15)C36—H360.95
C3B—H3B10.99C41—C461.385 (4)
C3B—H3B20.99C41—C421.396 (4)
C4B—C5B1.52 (2)C41—P21.794 (3)
C5B—C6B1.57 (5)C42—C431.379 (4)
C5B—H5B10.99C42—H420.95
C5B—H5B20.99C43—C441.370 (5)
C6B—H6B10.99C43—H430.95
C6B—H6B20.99C44—C451.378 (5)
C11A—C12A1.38 (3)C44—H440.95
C11A—C16A1.40 (3)C45—C461.382 (5)
C11A—P11.811 (16)C45—H450.95
C16A—C15A1.385 (15)C46—H460.95
C16A—H16A0.95N1—P11.701 (3)
C15A—C14A1.384 (15)N1—P21.706 (2)
C15A—H15A0.95F1—P31.580 (2)
C14A—C13A1.378 (12)F2—P31.593 (2)
C14A—H14A0.95F3—P31.591 (2)
C13A—C12A1.387 (12)F4—P31.598 (2)
C13A—H13A0.95F5—P31.590 (2)
C12A—H12A0.95F6—P31.564 (2)
C11B—C16B1.37 (4)Pt1—P12.2918 (9)
C11B—C12B1.40 (4)Pt1—P22.2999 (9)
C11B—P11.79 (3)Cl1A—C01A1.747 (11)
C12B—C13B1.383 (15)Cl2A—C01A1.765 (11)
C12B—H12B0.95C01A—H01A0.99
C13B—C14B1.381 (15)C01A—H01B0.99
C13B—H13B0.95Cl1B—C01B1.760 (8)
C14B—C15B1.38 (2)Cl2B—C01B1.757 (9)
C14B—H14B0.95C01B—H01C0.99
C15B—C16B1.39 (2)C01B—H01D0.99
N1—C1A—C6A116.4 (11)C22—C21—P1120.9 (2)
N1—C1A—C2A109.4 (7)C23—C22—C21119.7 (3)
C6A—C1A—C2A109.6 (11)C23—C22—H22120.1
N1—C1A—H1A107C21—C22—H22120.1
C6A—C1A—H1A107C24—C23—C22120.2 (3)
C2A—C1A—H1A107C24—C23—H23119.9
C3A—C2A—C1A110.4 (6)C22—C23—H23119.9
C3A—C2A—H2A1109.6C23—C24—C25120.4 (3)
C1A—C2A—H2A1109.6C23—C24—H24119.8
C3A—C2A—H2A2109.6C25—C24—H24119.8
C1A—C2A—H2A2109.6C26—C25—C24119.8 (3)
H2A1—C2A—H2A2108.1C26—C25—H25120.1
C2A—C3A—C4A111.9 (5)C24—C25—H25120.1
C2A—C3A—H3A1109.2C25—C26—C21120.5 (3)
C4A—C3A—H3A1109.2C25—C26—H26119.8
C2A—C3A—H3A2109.2C21—C26—H26119.8
C4A—C3A—H3A2109.2C32—C31—C36119.4 (3)
H3A1—C3A—H3A2107.9C32—C31—P2120.6 (2)
C5A—C4A—C3A111.2 (6)C36—C31—P2119.4 (2)
C5A—C4A—H4A1109.4C31—C32—C33120.3 (3)
C3A—C4A—H4A1109.4C31—C32—H32119.8
C5A—C4A—H4A2109.4C33—C32—H32119.8
C3A—C4A—H4A2109.4C34—C33—C32119.9 (3)
H4A1—C4A—H4A2108C34—C33—H33120
C4A—C5A—C6A109.7 (9)C32—C33—H33120
C4A—C5A—H5A1109.7C33—C34—C35120.2 (3)
C6A—C5A—H5A1109.7C33—C34—H34119.9
C4A—C5A—H5A2109.7C35—C34—H34119.9
C6A—C5A—H5A2109.7C34—C35—C36120.2 (3)
H5A1—C5A—H5A2108.2C34—C35—H35119.9
C1A—C6A—C5A114.3 (14)C36—C35—H35119.9
C1A—C6A—H6A1108.7C35—C36—C31119.9 (3)
C5A—C6A—H6A1108.7C35—C36—H36120
C1A—C6A—H6A2108.7C31—C36—H36120
C5A—C6A—H6A2108.7C46—C41—C42119.4 (3)
H6A1—C6A—H6A2107.6C46—C41—P2118.3 (2)
C2B—C1B—N1113.5 (14)C42—C41—P2122.2 (2)
C2B—C1B—C6B116 (2)C43—C42—C41120.1 (3)
N1—C1B—C6B103 (2)C43—C42—H42119.9
C2B—C1B—H1B107.9C41—C42—H42119.9
N1—C1B—H1B107.9C44—C43—C42120.0 (3)
C6B—C1B—H1B107.9C44—C43—H43120
C1B—C2B—C3B109.1 (11)C42—C43—H43120
C1B—C2B—H2B1109.9C43—C44—C45120.3 (3)
C3B—C2B—H2B1109.9C43—C44—H44119.8
C1B—C2B—H2B2109.9C45—C44—H44119.8
C3B—C2B—H2B2109.9C44—C45—C46120.3 (3)
H2B1—C2B—H2B2108.3C44—C45—H45119.8
C4B—C3B—C2B113.4 (8)C46—C45—H45119.8
C4B—C3B—H3B1108.9C45—C46—C41119.8 (3)
C2B—C3B—H3B1108.9C45—C46—H46120.1
C4B—C3B—H3B2108.9C41—C46—H46120.1
C2B—C3B—H3B2108.9C1A—N1—P1120.1 (4)
H3B1—C3B—H3B2107.7C1B—N1—P1137.3 (6)
C3B—C4B—C5B110.2 (9)C1A—N1—P2134.0 (4)
C4B—C5B—C6B115.4 (19)C1B—N1—P2119.3 (7)
C4B—C5B—H5B1108.4P1—N1—P2102.58 (12)
C6B—C5B—H5B1108.4N1—P1—C11B110.8 (17)
C4B—C5B—H5B2108.4N1—P1—C21111.32 (13)
C6B—C5B—H5B2108.4C11B—P1—C21102.4 (13)
H5B1—C5B—H5B2107.5N1—P1—C11A110.5 (11)
C5B—C6B—C1B103 (3)C21—P1—C11A106.0 (9)
C5B—C6B—H6B1111.1N1—P1—Pt193.47 (8)
C1B—C6B—H6B1111.1C11B—P1—Pt1121.4 (10)
C5B—C6B—H6B2111.1C21—P1—Pt1117.31 (10)
C1B—C6B—H6B2111.1C11A—P1—Pt1117.7 (6)
H6B1—C6B—H6B2109N1—P2—C41110.98 (12)
C12A—C11A—C16A119.5 (11)N1—P2—C31110.86 (13)
C12A—C11A—P1123 (2)C41—P2—C31107.74 (14)
C16A—C11A—P1116.8 (19)N1—P2—Pt193.08 (9)
C15A—C16A—C11A120.6 (15)C41—P2—Pt1117.31 (10)
C15A—C16A—H16A119.7C31—P2—Pt1116.09 (10)
C11A—C16A—H16A119.7F6—P3—F191.14 (14)
C14A—C15A—C16A119.1 (13)F6—P3—F590.24 (16)
C14A—C15A—H15A120.4F1—P3—F590.30 (12)
C16A—C15A—H15A120.4F6—P3—F3179.34 (18)
C13A—C14A—C15A120.3 (9)F1—P3—F389.15 (14)
C13A—C14A—H14A119.9F5—P3—F389.16 (16)
C15A—C14A—H14A119.9F6—P3—F291.09 (16)
C14A—C13A—C12A120.7 (8)F1—P3—F290.39 (12)
C14A—C13A—H13A119.7F5—P3—F2178.49 (15)
C12A—C13A—H13A119.7F3—P3—F289.51 (15)
C11A—C12A—C13A119.7 (12)F6—P3—F490.00 (15)
C11A—C12A—H12A120.2F1—P3—F4178.76 (14)
C13A—C12A—H12A120.2F5—P3—F490.20 (12)
C16B—C11B—C12B119.3 (16)F3—P3—F489.72 (15)
C16B—C11B—P1120 (3)F2—P3—F489.08 (12)
C12B—C11B—P1121 (3)P1i—Pt1—P1180.0000 (10)
C13B—C12B—C11B120.5 (18)P1i—Pt1—P2i70.76 (3)
C13B—C12B—H12B119.7P1—Pt1—P2i109.24 (3)
C11B—C12B—H12B119.7P1i—Pt1—P2109.24 (3)
C14B—C13B—C12B119.0 (10)P1—Pt1—P270.76 (3)
C14B—C13B—H13B120.5P2i—Pt1—P2180
C12B—C13B—H13B120.5Cl1A—C01A—Cl2A111.5 (5)
C15B—C14B—C13B120.9 (14)Cl1A—C01A—H01A109.3
C15B—C14B—H14B119.5Cl2A—C01A—H01A109.3
C13B—C14B—H14B119.5Cl1A—C01A—H01B109.3
C14B—C15B—C16B120 (2)Cl2A—C01A—H01B109.3
C14B—C15B—H15B120.1H01A—C01A—H01B108
C16B—C15B—H15B120.1Cl2B—C01B—Cl1B110.9 (5)
C11B—C16B—C15B120 (2)Cl2B—C01B—H01C109.5
C11B—C16B—H16B119.8Cl1B—C01B—H01C109.5
C15B—C16B—H16B119.8Cl2B—C01B—H01D109.5
C26—C21—C22119.5 (3)Cl1B—C01B—H01D109.5
C26—C21—P1119.6 (2)H01C—C01B—H01D108.1
N1—C1A—C2A—C3A176.4 (6)C1A—N1—P1—C11B69.5 (12)
C6A—C1A—C2A—C3A54.8 (12)C1B—N1—P1—C11B62.4 (16)
C1A—C2A—C3A—C4A55.2 (8)P2—N1—P1—C11B128.4 (11)
C2A—C3A—C4A—C5A55.4 (8)C1A—N1—P1—C2143.8 (5)
C3A—C4A—C5A—C6A54.1 (10)C1B—N1—P1—C2150.9 (12)
N1—C1A—C6A—C5A178.1 (9)P2—N1—P1—C21118.30 (14)
C2A—C1A—C6A—C5A57.1 (15)C1A—N1—P1—C11A73.7 (9)
C4A—C5A—C6A—C1A56.8 (15)C1B—N1—P1—C11A66.6 (14)
N1—C1B—C2B—C3B177.7 (9)P2—N1—P1—C11A124.2 (7)
C6B—C1B—C2B—C3B59 (2)C1A—N1—P1—Pt1165.0 (5)
C1B—C2B—C3B—C4B55.3 (12)C1B—N1—P1—Pt1172.1 (12)
C2B—C3B—C4B—C5B53.7 (13)P2—N1—P1—Pt12.84 (11)
C3B—C4B—C5B—C6B55 (2)C16B—C11B—P1—N1179.4 (19)
C4B—C5B—C6B—C1B53 (3)C12B—C11B—P1—N11 (2)
C2B—C1B—C6B—C5B56 (3)C16B—C11B—P1—C2161 (2)
N1—C1B—C6B—C5B179.2 (18)C12B—C11B—P1—C21118 (2)
C12A—C11A—C16A—C15A0 (2)C16B—C11B—P1—Pt173 (2)
P1—C11A—C16A—C15A172.2 (17)C12B—C11B—P1—Pt1108.6 (18)
C11A—C16A—C15A—C14A2 (2)C26—C21—P1—N196.5 (3)
C16A—C15A—C14A—C13A2.3 (18)C22—C21—P1—N181.8 (3)
C15A—C14A—C13A—C12A0.1 (16)C26—C21—P1—C11B145.0 (15)
C16A—C11A—C12A—C13A3 (2)C22—C21—P1—C11B36.7 (15)
P1—C11A—C12A—C13A174.0 (9)C26—C21—P1—C11A143.3 (10)
C14A—C13A—C12A—C11A2.6 (18)C22—C21—P1—C11A38.4 (10)
C16B—C11B—C12B—C13B0 (2)C26—C21—P1—Pt19.5 (3)
P1—C11B—C12B—C13B178.7 (16)C22—C21—P1—Pt1172.2 (2)
C11B—C12B—C13B—C14B1.0 (14)C12A—C11A—P1—N117.2 (18)
C12B—C13B—C14B—C15B3 (2)C16A—C11A—P1—N1171.4 (12)
C13B—C14B—C15B—C16B4 (3)C12A—C11A—P1—C21138.0 (15)
C12B—C11B—C16B—C15B1 (3)C16A—C11A—P1—C2150.7 (13)
P1—C11B—C16B—C15B178 (3)C12A—C11A—P1—Pt188.4 (18)
C14B—C15B—C16B—C11B3 (4)C16A—C11A—P1—Pt183.0 (13)
C26—C21—C22—C230.8 (5)C1A—N1—P2—C4140.3 (6)
P1—C21—C22—C23177.4 (3)C1B—N1—P2—C4153.6 (9)
C21—C22—C23—C240.9 (5)P1—N1—P2—C41118.02 (14)
C22—C23—C24—C250.1 (5)C1A—N1—P2—C3179.4 (6)
C23—C24—C25—C261.3 (5)C1B—N1—P2—C3166.1 (9)
C24—C25—C26—C211.4 (5)P1—N1—P2—C31122.29 (14)
C22—C21—C26—C250.3 (5)C1A—N1—P2—Pt1161.2 (6)
P1—C21—C26—C25178.6 (2)C1B—N1—P2—Pt1174.5 (9)
C36—C31—C32—C330.4 (5)P1—N1—P2—Pt12.83 (11)
P2—C31—C32—C33171.3 (3)C46—C41—P2—N186.4 (3)
C31—C32—C33—C341.3 (5)C42—C41—P2—N189.9 (3)
C32—C33—C34—C350.9 (5)C46—C41—P2—C31152.0 (2)
C33—C34—C35—C360.4 (5)C42—C41—P2—C3131.6 (3)
C34—C35—C36—C311.3 (5)C46—C41—P2—Pt118.8 (3)
C32—C31—C36—C350.9 (4)C42—C41—P2—Pt1164.8 (2)
P2—C31—C36—C35170.1 (2)C32—C31—P2—N126.6 (3)
C46—C41—C42—C431.2 (4)C36—C31—P2—N1162.4 (2)
P2—C41—C42—C43175.1 (2)C32—C31—P2—C41148.3 (2)
C41—C42—C43—C440.2 (5)C36—C31—P2—C4140.8 (3)
C42—C43—C44—C450.6 (5)C32—C31—P2—Pt177.9 (3)
C43—C44—C45—C460.5 (6)C36—C31—P2—Pt193.1 (2)
C44—C45—C46—C410.4 (6)N1—P1—Pt1—P2i177.82 (8)
C42—C41—C46—C451.3 (5)C11B—P1—Pt1—P2i60.8 (19)
P2—C41—C46—C45175.2 (3)C21—P1—Pt1—P2i65.99 (12)
C6A—C1A—N1—C1B101 (4)C11A—P1—Pt1—P2i62.5 (12)
C2A—C1A—N1—C1B23 (3)N1—P1—Pt1—P22.18 (8)
C6A—C1A—N1—P194.2 (10)C11B—P1—Pt1—P2119.2 (19)
C2A—C1A—N1—P1140.9 (5)C21—P1—Pt1—P2114.01 (12)
C6A—C1A—N1—P261.2 (11)C11A—P1—Pt1—P2117.5 (12)
C2A—C1A—N1—P263.7 (10)N1—P2—Pt1—P1i177.83 (8)
C2B—C1B—N1—C1A70 (4)C41—P2—Pt1—P1i66.62 (11)
C6B—C1B—N1—C1A57 (4)C31—P2—Pt1—P1i62.78 (11)
C2B—C1B—N1—P149.5 (17)N1—P2—Pt1—P12.17 (8)
C6B—C1B—N1—P177 (2)C41—P2—Pt1—P1113.38 (11)
C2B—C1B—N1—P2142.5 (8)C31—P2—Pt1—P1117.22 (11)
C6B—C1B—N1—P290.8 (17)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C12A—H12A···F20.952.453.186 (11)134
C32—H32···F20.952.473.138 (4)127

Experimental details

Crystal data
Chemical formula[Pt(C30H31NP2)2](PF6)2·2CH2Cl2
Mr1588.38
Crystal system, space groupMonoclinic, P21/c
Temperature (K)100
a, b, c (Å)13.350 (5), 18.764 (4), 15.248 (5)
β (°) 123.333 (5)
V3)3191.3 (17)
Z2
Radiation typeMo Kα
µ (mm1)2.59
Crystal size (mm)0.32 × 0.29 × 0.14
Data collection
DiffractometerBruker X8 APEXII KappaCCD
Absorption correctionMulti-scan
(SADABS; Bruker, 2001)
Tmin, Tmax0.491, 0.713
No. of measured, independent and
observed [I > 2σ(I)] reflections
57085, 7899, 6367
Rint0.042
(sin θ/λ)max1)0.668
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.027, 0.070, 1.03
No. of reflections7899
No. of parameters503
No. of restraints18
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.72, 0.99

Computer programs: APEX2 (Bruker, 2007), SAINT-Plus (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg & Putz, 1999), WinGX (Farrugia, 1999).

Selected bond lengths (Å) top
Pt1—P12.2918 (9)Pt1—P22.2999 (9)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C12A—H12A···F20.952.453.186 (11)134
C32—H32···F20.952.473.138 (4)127
 

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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