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Acta Crystallographica Section E: Structure Reports Online logoLink to Acta Crystallographica Section E: Structure Reports Online
. 2009 Jun 20;65(Pt 7):m793. doi: 10.1107/S1600536809022405

{Bis[2-(diphenyl­phosphino)eth­yl]phenyl­phosphine-κ3 P,P′,P′′}chloridoplatinium(II) hexa­fluoridophosphate

Scott A Heston a, Bruce C Noll b, Monte L Helm a,*
PMCID: PMC2969258  PMID: 21582720

Abstract

In the title compound, [PtCl(C34H33P3)]PF6, the PtII cation adopts a distorted square-planar PtClP3 geometry, arising from the P,P′,P′′-tridentate triphos ligand and a chloride ion. Four of the F atoms of the PF6 anion are disordered over two sets of positions in a 0.614 (17):0.386 (17) ratio.

Related literature

The corresponding complex with a PdII metal center is published concurently (Vorce et al., 2009). The corresponding PtII complex has been previously reported as a CuCl2 salt (Fernadez et al., 2005). The corresponding complexes with both PtII and PdII have been previously reported as chloride and diphenyl­tetra­chlorido­stannate(IV) salts (Sevillano et al., 1999a ; Garcia-Seijo et al., 2001; Housecroft et al., 1990). For other group 10–triphos complexes, see: Sevillano et al. (1999b ); Müller et al. (2000); Aizawa et al. (2002); Bertinsson et al. (1983); Autissier et al. (2005); Fernandez et al. (2005); King et al. (1971).graphic file with name e-65-0m793-scheme1.jpg

Experimental

Crystal data

  • [PtCl(C34H33P3)]PF6

  • M r = 910.02

  • Monoclinic, Inline graphic

  • a = 11.3870 (11) Å

  • b = 19.6221 (18) Å

  • c = 16.4439 (16) Å

  • β = 107.528 (3)°

  • V = 3503.6 (6) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 4.32 mm−1

  • T = 298 K

  • 0.50 × 0.30 × 0.10 mm

Data collection

  • Bruker SMART X2S diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2008a ) T min = 0.21, T max = 0.65

  • 21968 measured reflections

  • 6155 independent reflections

  • 5269 reflections with I > 2σ(I)

  • R int = 0.025

Refinement

  • R[F 2 > 2σ(F 2)] = 0.020

  • wR(F 2) = 0.049

  • S = 1.03

  • 6155 reflections

  • 452 parameters

  • 204 restraints

  • H-atom parameters constrained

  • Δρmax = 0.58 e Å−3

  • Δρmin = −0.41 e Å−3

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT and XPREP (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008b ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008b ); molecular graphics: SHELXTL (Sheldrick, 2008b ); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809022405/hb2993sup1.cif

e-65-0m793-sup1.cif (25.6KB, cif)

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809022405/hb2993Isup2.hkl

e-65-0m793-Isup2.hkl (301.3KB, hkl)

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Selected bond lengths (Å).

Pt1—P2 2.2095 (8)
Pt1—P3 2.3007 (8)
Pt1—P1 2.3185 (8)
Pt1—Cl1 2.3434 (8)

Acknowledgments

We thank Research Corporation Cottrell Science Award (No. 7293) for funding supporting this study.

supplementary crystallographic information

Comment

The crystal structure of the title compound, (I), consists of a [Pt(triphos)Cl]+ cation and disordered PF6- anion (Fig. 1). The cation shows a distorted square planar geometry (Table 1) around the metal center with a non-coordinating PF6- anion.

Experimental

The synthesis of (I) by a previously reported proceedure (King, et al., 1971). Crystals where grown by slow solvent evaporation of a saturated dichloromethane solution of (I).

Figures

Fig. 1.

Fig. 1.

The molecular structure of (I), with 50% probability displacement ellipsoids.

Fig. 2.

Fig. 2.

The molecular structure of (I), with atom labels and 50% probability displacement ellipsoids. Hydrogen atoms are omitted for clarity.

Crystal data

[PtCl(C34H33P3)]PF6 F(000) = 1784
Mr = 910.02 Dx = 1.725 Mg m3
Monoclinic, P21/c Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc Cell parameters from 9957 reflections
a = 11.3870 (11) Å θ = 2.5–25.1°
b = 19.6221 (18) Å µ = 4.32 mm1
c = 16.4439 (16) Å T = 298 K
β = 107.528 (3)° Plate, colorless
V = 3503.6 (6) Å3 0.50 × 0.30 × 0.10 mm
Z = 4

Data collection

Bruker SMART X2S diffractometer 6155 independent reflections
Radiation source: microfocus sealed tube, Bruker 5269 reflections with I > 2σ(I)
graphite Rint = 0.025
Detector resolution: 8.33 pixels mm-1 θmax = 25.1°, θmin = 2.8°
ω scans h = −13→13
Absorption correction: multi-scan (SADABS; Sheldrick, 2008a) k = −18→23
Tmin = 0.21, Tmax = 0.65 l = −19→19
21968 measured reflections

Refinement

Refinement on F2 Primary atom site location: structure-invariant direct methods
Least-squares matrix: full Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.020 Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.049 H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0227P)2 + 1.641P] where P = (Fo2 + 2Fc2)/3
6155 reflections (Δ/σ)max = 0.002
452 parameters Δρmax = 0.58 e Å3
204 restraints Δρmin = −0.41 e Å3

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.
Refinement. The PF6 anion is disordered, showing alternate positions of the 4 F atoms F3—F6 when rotated about the axis F1—P4—F2. A second orientation for these equatorial positions was located. Based on the thermal parameters, additional positions are indicated, but were not modeled. To improve the quality of the fit for this anion, distance restraints (SHELX SADI) were added for the P–F bonds, as well as for the FF interatomic distances. These account for 156 of the 204 restraints applied. The remaining restraints (ISOR) were applied to the anisotropic displacement parameters for the fluorine atoms.Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

x y z Uiso*/Ueq Occ. (<1)
Pt1 0.139852 (10) 0.364806 (6) 0.374003 (7) 0.03173 (5)
Cl1 0.31867 (8) 0.35123 (5) 0.48942 (5) 0.0498 (2)
P1 0.22200 (7) 0.43573 (4) 0.29227 (5) 0.03695 (19)
P2 −0.03648 (7) 0.37743 (4) 0.27189 (5) 0.03518 (19)
P3 0.03774 (7) 0.28264 (4) 0.42630 (5) 0.03706 (19)
C1 0.3286 (3) 0.39017 (18) 0.2487 (2) 0.0417 (8)
C2 0.3950 (4) 0.3357 (2) 0.2925 (3) 0.0696 (12)
H2 0.3851 0.3227 0.3444 0.084*
C3 0.4758 (5) 0.3003 (3) 0.2602 (4) 0.0929 (17)
H3 0.5209 0.2641 0.2909 0.111*
C4 0.4896 (4) 0.3182 (3) 0.1838 (3) 0.0811 (14)
H4 0.5422 0.2933 0.1614 0.097*
C5 0.4268 (4) 0.3724 (3) 0.1397 (3) 0.0809 (15)
H5 0.4382 0.3850 0.0881 0.097*
C6 0.3458 (4) 0.4088 (2) 0.1716 (2) 0.0662 (12)
H6 0.3030 0.4457 0.1413 0.079*
C7 0.2923 (3) 0.51580 (17) 0.3367 (2) 0.0448 (8)
C8 0.3091 (4) 0.5681 (2) 0.2843 (3) 0.0690 (12)
H8 0.2889 0.5616 0.2257 0.083*
C9 0.3563 (5) 0.6303 (2) 0.3202 (4) 0.0815 (15)
H9 0.3673 0.6653 0.2852 0.098*
C10 0.3863 (4) 0.6405 (2) 0.4054 (4) 0.0774 (15)
H10 0.4162 0.6827 0.4283 0.093*
C11 0.3726 (4) 0.5886 (2) 0.4579 (3) 0.0774 (14)
H11 0.3950 0.5954 0.5166 0.093*
C12 0.3255 (3) 0.5262 (2) 0.4237 (3) 0.0587 (10)
H12 0.3162 0.4913 0.4595 0.070*
C13 0.0924 (3) 0.46082 (19) 0.2000 (2) 0.0480 (9)
H13A 0.0534 0.5012 0.2141 0.058*
H13B 0.1226 0.4718 0.1524 0.058*
C14 −0.0024 (3) 0.40301 (19) 0.1745 (2) 0.0459 (8)
H14A 0.0311 0.3649 0.1510 0.055*
H14B −0.0766 0.4188 0.1320 0.055*
C15 −0.1372 (3) 0.44123 (17) 0.2947 (2) 0.0392 (8)
C16 −0.2526 (3) 0.4525 (2) 0.2376 (2) 0.0612 (11)
H16 −0.2769 0.4292 0.1860 0.073*
C17 −0.3320 (4) 0.4987 (2) 0.2575 (3) 0.0777 (13)
H17 −0.4097 0.5061 0.2192 0.093*
C18 −0.2964 (4) 0.5334 (2) 0.3334 (3) 0.0718 (12)
H18 −0.3501 0.5642 0.3462 0.086*
C19 −0.1830 (4) 0.5230 (2) 0.3901 (3) 0.0655 (11)
H19 −0.1593 0.5468 0.4413 0.079*
C20 −0.1031 (3) 0.47681 (18) 0.3711 (2) 0.0512 (9)
H20 −0.0258 0.4696 0.4100 0.061*
C21 −0.1212 (3) 0.29792 (17) 0.2618 (2) 0.0446 (8)
H21A −0.2052 0.3041 0.2255 0.054*
H21B −0.0824 0.2631 0.2368 0.054*
C22 −0.1201 (3) 0.27699 (19) 0.3519 (2) 0.0500 (9)
H22A −0.1502 0.2307 0.3510 0.060*
H22B −0.1743 0.3067 0.3713 0.060*
C23 0.0305 (3) 0.29942 (17) 0.5330 (2) 0.0413 (8)
C24 −0.0603 (3) 0.3399 (2) 0.5480 (2) 0.0529 (9)
H24 −0.1274 0.3533 0.5027 0.063*
C25 −0.0518 (4) 0.3605 (2) 0.6305 (3) 0.0605 (11)
H25 −0.1135 0.3874 0.6402 0.073*
C26 0.0467 (4) 0.3415 (2) 0.6974 (2) 0.0590 (10)
H26 0.0533 0.3564 0.7523 0.071*
C27 0.1362 (4) 0.3003 (2) 0.6833 (2) 0.0614 (11)
H27 0.2024 0.2865 0.7290 0.074*
C28 0.1287 (3) 0.2791 (2) 0.6017 (2) 0.0538 (9)
H28 0.1896 0.2512 0.5929 0.065*
C29 0.1039 (3) 0.19806 (16) 0.42953 (19) 0.0387 (8)
C30 0.0425 (4) 0.14216 (19) 0.4497 (2) 0.0539 (10)
H30 −0.0322 0.1483 0.4609 0.065*
C31 0.0923 (5) 0.0778 (2) 0.4532 (3) 0.0677 (12)
H31 0.0515 0.0407 0.4673 0.081*
C32 0.2015 (4) 0.0680 (2) 0.4359 (3) 0.0675 (12)
H32 0.2343 0.0244 0.4381 0.081*
C33 0.2626 (4) 0.1225 (2) 0.4153 (3) 0.0610 (11)
H33 0.3362 0.1157 0.4029 0.073*
C34 0.2149 (3) 0.18766 (18) 0.4131 (2) 0.0456 (8)
H34 0.2575 0.2246 0.4005 0.055*
P4 0.33951 (10) 0.86107 (6) 0.53542 (7) 0.0655 (3)
F1 0.2344 (3) 0.91309 (17) 0.5407 (2) 0.1331 (13)
F2 0.4424 (3) 0.81198 (16) 0.5283 (2) 0.1263 (12)
F3 0.4311 (7) 0.8949 (6) 0.6137 (6) 0.170 (6) 0.614 (17)
F4 0.2458 (8) 0.8302 (5) 0.4551 (7) 0.181 (7) 0.614 (17)
F5 0.3788 (11) 0.9131 (4) 0.4771 (7) 0.143 (6) 0.614 (17)
F6 0.2992 (7) 0.8122 (5) 0.5916 (7) 0.196 (7) 0.614 (17)
F3' 0.3623 (16) 0.8459 (7) 0.6302 (5) 0.170 (11) 0.386 (17)
F4' 0.3028 (14) 0.8713 (10) 0.4399 (5) 0.184 (10) 0.386 (17)
F5' 0.4294 (9) 0.9199 (4) 0.5545 (15) 0.153 (11) 0.386 (17)
F6' 0.2434 (11) 0.8018 (5) 0.5150 (11) 0.141 (9) 0.386 (17)

Atomic displacement parameters (Å2)

U11 U22 U33 U12 U13 U23
Pt1 0.02685 (7) 0.03558 (8) 0.03213 (7) −0.00116 (5) 0.00792 (5) 0.00172 (5)
Cl1 0.0352 (4) 0.0585 (6) 0.0467 (5) −0.0016 (4) −0.0013 (4) 0.0038 (4)
P1 0.0324 (4) 0.0385 (5) 0.0422 (5) 0.0009 (4) 0.0147 (4) 0.0056 (4)
P2 0.0290 (4) 0.0438 (5) 0.0311 (4) 0.0000 (4) 0.0066 (3) −0.0002 (3)
P3 0.0322 (4) 0.0416 (5) 0.0385 (4) −0.0023 (4) 0.0124 (4) 0.0045 (4)
C1 0.0343 (17) 0.046 (2) 0.0465 (19) −0.0013 (15) 0.0144 (15) −0.0008 (16)
C2 0.069 (3) 0.069 (3) 0.086 (3) 0.022 (2) 0.047 (3) 0.023 (2)
C3 0.095 (4) 0.080 (4) 0.126 (4) 0.042 (3) 0.067 (4) 0.029 (3)
C4 0.069 (3) 0.085 (4) 0.103 (4) 0.011 (3) 0.046 (3) −0.021 (3)
C5 0.061 (3) 0.134 (5) 0.056 (3) 0.015 (3) 0.029 (2) −0.004 (3)
C6 0.057 (2) 0.095 (3) 0.051 (2) 0.021 (2) 0.023 (2) 0.009 (2)
C7 0.0338 (18) 0.039 (2) 0.064 (2) −0.0003 (15) 0.0188 (17) 0.0049 (17)
C8 0.081 (3) 0.051 (3) 0.087 (3) −0.012 (2) 0.043 (3) 0.004 (2)
C9 0.083 (3) 0.046 (3) 0.122 (5) −0.012 (2) 0.041 (3) 0.014 (3)
C10 0.047 (2) 0.049 (3) 0.122 (4) −0.014 (2) 0.003 (3) −0.006 (3)
C11 0.063 (3) 0.063 (3) 0.084 (3) −0.006 (2) −0.014 (2) −0.005 (3)
C12 0.049 (2) 0.048 (2) 0.068 (3) −0.0065 (18) 0.0007 (19) 0.0046 (19)
C13 0.0418 (19) 0.057 (2) 0.048 (2) 0.0080 (17) 0.0177 (16) 0.0167 (17)
C14 0.0408 (18) 0.063 (2) 0.0335 (17) 0.0071 (18) 0.0111 (14) 0.0050 (16)
C15 0.0340 (17) 0.042 (2) 0.0423 (18) 0.0025 (15) 0.0124 (15) 0.0026 (15)
C16 0.044 (2) 0.074 (3) 0.058 (2) 0.008 (2) 0.0042 (18) −0.010 (2)
C17 0.045 (2) 0.084 (3) 0.094 (3) 0.020 (2) 0.006 (2) −0.006 (3)
C18 0.057 (3) 0.064 (3) 0.098 (3) 0.015 (2) 0.028 (3) −0.015 (3)
C19 0.066 (3) 0.063 (3) 0.067 (3) 0.008 (2) 0.019 (2) −0.017 (2)
C20 0.045 (2) 0.052 (2) 0.053 (2) 0.0059 (17) 0.0090 (17) −0.0046 (18)
C21 0.0377 (18) 0.044 (2) 0.0468 (19) −0.0053 (15) 0.0043 (15) −0.0068 (16)
C22 0.0346 (18) 0.055 (2) 0.058 (2) −0.0089 (16) 0.0104 (16) 0.0066 (18)
C23 0.0398 (18) 0.045 (2) 0.0432 (18) −0.0014 (15) 0.0189 (15) 0.0061 (15)
C24 0.047 (2) 0.063 (2) 0.051 (2) 0.0083 (19) 0.0199 (18) 0.0037 (19)
C25 0.060 (3) 0.069 (3) 0.062 (3) 0.009 (2) 0.032 (2) 0.000 (2)
C26 0.076 (3) 0.062 (3) 0.046 (2) 0.002 (2) 0.027 (2) 0.0018 (19)
C27 0.067 (3) 0.073 (3) 0.042 (2) 0.012 (2) 0.0129 (19) 0.0082 (19)
C28 0.055 (2) 0.062 (3) 0.046 (2) 0.0145 (19) 0.0190 (18) 0.0076 (18)
C29 0.0413 (18) 0.040 (2) 0.0339 (16) −0.0049 (15) 0.0096 (14) 0.0008 (14)
C30 0.060 (2) 0.053 (3) 0.051 (2) −0.0172 (19) 0.0205 (19) −0.0012 (18)
C31 0.096 (4) 0.043 (3) 0.061 (3) −0.020 (2) 0.020 (2) 0.0018 (19)
C32 0.086 (3) 0.042 (2) 0.063 (3) 0.008 (2) 0.005 (2) −0.007 (2)
C33 0.057 (2) 0.053 (3) 0.069 (3) 0.007 (2) 0.012 (2) −0.007 (2)
C34 0.045 (2) 0.043 (2) 0.049 (2) −0.0006 (16) 0.0130 (16) 0.0008 (16)
P4 0.0518 (6) 0.0859 (9) 0.0608 (7) 0.0022 (6) 0.0199 (5) 0.0198 (6)
F1 0.085 (2) 0.135 (3) 0.193 (4) 0.031 (2) 0.062 (2) 0.027 (3)
F2 0.100 (2) 0.108 (3) 0.178 (3) 0.0275 (19) 0.052 (2) −0.005 (2)
F3 0.082 (5) 0.309 (16) 0.115 (7) −0.058 (7) 0.025 (4) −0.069 (8)
F4 0.133 (9) 0.174 (11) 0.166 (11) 0.000 (7) −0.061 (7) −0.044 (8)
F5 0.200 (12) 0.121 (8) 0.155 (10) 0.039 (7) 0.122 (9) 0.062 (7)
F6 0.121 (6) 0.265 (13) 0.210 (13) −0.036 (7) 0.061 (8) 0.170 (11)
F3' 0.27 (3) 0.174 (15) 0.051 (5) 0.124 (16) 0.023 (9) 0.000 (7)
F4' 0.183 (16) 0.31 (3) 0.047 (6) −0.042 (14) 0.010 (8) 0.053 (10)
F5' 0.083 (8) 0.077 (7) 0.31 (3) −0.036 (5) 0.079 (15) −0.040 (13)
F6' 0.163 (15) 0.110 (10) 0.198 (19) −0.074 (10) 0.130 (15) −0.031 (10)

Geometric parameters (Å, °)

Pt1—P2 2.2095 (8) C17—C18 1.371 (6)
Pt1—P3 2.3007 (8) C17—H17 0.9300
Pt1—P1 2.3185 (8) C18—C19 1.361 (6)
Pt1—Cl1 2.3434 (8) C18—H18 0.9300
P1—C7 1.814 (4) C19—C20 1.384 (5)
P1—C1 1.819 (3) C19—H19 0.9300
P1—C13 1.836 (3) C20—H20 0.9300
P2—C15 1.812 (3) C21—C22 1.535 (5)
P2—C21 1.815 (3) C21—H21A 0.9700
P2—C14 1.828 (3) C21—H21B 0.9700
P3—C23 1.812 (3) C22—H22A 0.9700
P3—C29 1.817 (3) C22—H22B 0.9700
P3—C22 1.848 (3) C23—C24 1.383 (5)
C1—C2 1.380 (5) C23—C28 1.387 (5)
C1—C6 1.389 (5) C24—C25 1.392 (5)
C2—C3 1.381 (6) C24—H24 0.9300
C2—H2 0.9300 C25—C26 1.365 (6)
C3—C4 1.359 (6) C25—H25 0.9300
C3—H3 0.9300 C26—C27 1.375 (5)
C4—C5 1.362 (6) C26—H26 0.9300
C4—H4 0.9300 C27—C28 1.382 (5)
C5—C6 1.388 (6) C27—H27 0.9300
C5—H5 0.9300 C28—H28 0.9300
C6—H6 0.9300 C29—C34 1.385 (4)
C7—C12 1.381 (5) C29—C30 1.393 (5)
C7—C8 1.390 (5) C30—C31 1.379 (5)
C8—C9 1.390 (6) C30—H30 0.9300
C8—H8 0.9300 C31—C32 1.370 (6)
C9—C10 1.352 (7) C31—H31 0.9300
C9—H9 0.9300 C32—C33 1.372 (6)
C10—C11 1.375 (6) C32—H32 0.9300
C10—H10 0.9300 C33—C34 1.385 (5)
C11—C12 1.386 (5) C33—H33 0.9300
C11—H11 0.9300 C34—H34 0.9300
C12—H12 0.9300 P4—F6 1.496 (5)
C13—C14 1.535 (5) P4—F5' 1.512 (8)
C13—H13A 0.9700 P4—F4' 1.512 (8)
C13—H13B 0.9700 P4—F3' 1.530 (8)
C14—H14A 0.9700 P4—F3 1.542 (7)
C14—H14B 0.9700 P4—F2 1.548 (3)
C15—C16 1.383 (5) P4—F4 1.549 (6)
C15—C20 1.387 (5) P4—F5 1.556 (6)
C16—C17 1.387 (5) P4—F6' 1.563 (8)
C16—H16 0.9300 P4—F1 1.595 (3)
P2—Pt1—P3 85.22 (3) C18—C19—C20 119.7 (4)
P2—Pt1—P1 85.71 (3) C18—C19—H19 120.1
P3—Pt1—P1 167.13 (3) C20—C19—H19 120.1
P2—Pt1—Cl1 175.83 (3) C19—C20—C15 120.7 (3)
P3—Pt1—Cl1 91.79 (3) C19—C20—H20 119.7
P1—Pt1—Cl1 97.69 (3) C15—C20—H20 119.7
C7—P1—C1 108.56 (15) C22—C21—P2 107.0 (2)
C7—P1—C13 104.36 (16) C22—C21—H21A 110.3
C1—P1—C13 105.78 (16) P2—C21—H21A 110.3
C7—P1—Pt1 119.51 (12) C22—C21—H21B 110.3
C1—P1—Pt1 111.53 (12) P2—C21—H21B 110.3
C13—P1—Pt1 105.99 (11) H21A—C21—H21B 108.6
C15—P2—C21 105.12 (16) C21—C22—P3 110.3 (2)
C15—P2—C14 107.82 (16) C21—C22—H22A 109.6
C21—P2—C14 113.75 (16) P3—C22—H22A 109.6
C15—P2—Pt1 114.03 (11) C21—C22—H22B 109.6
C21—P2—Pt1 108.04 (11) P3—C22—H22B 109.6
C14—P2—Pt1 108.22 (11) H22A—C22—H22B 108.1
C23—P3—C29 106.08 (15) C24—C23—C28 118.9 (3)
C23—P3—C22 109.46 (16) C24—C23—P3 122.1 (3)
C29—P3—C22 106.05 (16) C28—C23—P3 118.4 (3)
C23—P3—Pt1 114.22 (11) C23—C24—C25 120.3 (4)
C29—P3—Pt1 113.54 (11) C23—C24—H24 119.9
C22—P3—Pt1 107.16 (11) C25—C24—H24 119.9
C2—C1—C6 118.3 (3) C26—C25—C24 120.4 (4)
C2—C1—P1 120.0 (3) C26—C25—H25 119.8
C6—C1—P1 121.6 (3) C24—C25—H25 119.8
C1—C2—C3 120.9 (4) C25—C26—C27 119.7 (4)
C1—C2—H2 119.6 C25—C26—H26 120.1
C3—C2—H2 119.6 C27—C26—H26 120.1
C4—C3—C2 120.1 (4) C26—C27—C28 120.6 (4)
C4—C3—H3 120.0 C26—C27—H27 119.7
C2—C3—H3 120.0 C28—C27—H27 119.7
C3—C4—C5 120.4 (4) C27—C28—C23 120.2 (3)
C3—C4—H4 119.8 C27—C28—H28 119.9
C5—C4—H4 119.8 C23—C28—H28 119.9
C4—C5—C6 120.2 (4) C34—C29—C30 118.9 (3)
C4—C5—H5 119.9 C34—C29—P3 121.6 (3)
C6—C5—H5 119.9 C30—C29—P3 119.5 (3)
C5—C6—C1 120.1 (4) C31—C30—C29 120.1 (4)
C5—C6—H6 119.9 C31—C30—H30 120.0
C1—C6—H6 119.9 C29—C30—H30 120.0
C12—C7—C8 119.1 (4) C32—C31—C30 120.5 (4)
C12—C7—P1 119.7 (3) C32—C31—H31 119.8
C8—C7—P1 121.1 (3) C30—C31—H31 119.8
C7—C8—C9 119.5 (4) C31—C32—C33 120.1 (4)
C7—C8—H8 120.3 C31—C32—H32 119.9
C9—C8—H8 120.3 C33—C32—H32 119.9
C10—C9—C8 121.0 (4) C32—C33—C34 120.1 (4)
C10—C9—H9 119.5 C32—C33—H33 119.9
C8—C9—H9 119.5 C34—C33—H33 119.9
C9—C10—C11 119.9 (4) C29—C34—C33 120.3 (3)
C9—C10—H10 120.0 C29—C34—H34 119.9
C11—C10—H10 120.0 C33—C34—H34 119.9
C10—C11—C12 120.2 (5) F5'—P4—F4' 94.2 (8)
C10—C11—H11 119.9 F5'—P4—F3' 92.3 (7)
C12—C11—H11 119.9 F4'—P4—F3' 173.1 (8)
C7—C12—C11 120.2 (4) F6—P4—F3 90.9 (5)
C7—C12—H12 119.9 F6—P4—F2 91.6 (4)
C11—C12—H12 119.9 F5'—P4—F2 90.6 (4)
C14—C13—P1 110.6 (2) F4'—P4—F2 89.0 (5)
C14—C13—H13A 109.5 F3'—P4—F2 93.2 (4)
P1—C13—H13A 109.5 F3—P4—F2 89.6 (4)
C14—C13—H13B 109.5 F6—P4—F4 90.9 (5)
P1—C13—H13B 109.5 F3—P4—F4 177.5 (5)
H13A—C13—H13B 108.1 F2—P4—F4 92.0 (3)
C13—C14—P2 106.3 (2) F6—P4—F5 178.6 (5)
C13—C14—H14A 110.5 F3—P4—F5 89.1 (4)
P2—C14—H14A 110.5 F2—P4—F5 89.8 (3)
C13—C14—H14B 110.5 F4—P4—F5 89.0 (5)
P2—C14—H14B 110.5 F5'—P4—F6' 178.3 (6)
H14A—C14—H14B 108.7 F4'—P4—F6' 85.3 (8)
C16—C15—C20 118.9 (3) F3'—P4—F6' 88.1 (6)
C16—C15—P2 120.1 (3) F2—P4—F6' 91.0 (4)
C20—C15—P2 120.9 (3) F6—P4—F1 90.1 (4)
C15—C16—C17 119.9 (4) F5'—P4—F1 88.4 (4)
C15—C16—H16 120.1 F4'—P4—F1 89.7 (5)
C17—C16—H16 120.1 F3'—P4—F1 88.2 (4)
C18—C17—C16 120.2 (4) F3—P4—F1 90.5 (4)
C18—C17—H17 119.9 F2—P4—F1 178.3 (2)
C16—C17—H17 119.9 F4—P4—F1 87.8 (3)
C19—C18—C17 120.6 (4) F5—P4—F1 88.5 (3)
C19—C18—H18 119.7 F6'—P4—F1 90.0 (4)
C17—C18—H18 119.7

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HB2993).

References

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Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Supplementary Materials

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809022405/hb2993sup1.cif

e-65-0m793-sup1.cif (25.6KB, cif)

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809022405/hb2993Isup2.hkl

e-65-0m793-Isup2.hkl (301.3KB, hkl)

Additional supplementary materials: crystallographic information; 3D view; checkCIF report


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