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

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ISSN: 2056-9890

(2,2′-Bipyrid­yl)di­carbonyl­bis­(tri­eth­oxy­phosphine-κP)rhenium(I) hexa­fluoro­phosphate

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aSchool of Chemistry, The University of Nottingham, University Park, Nottingham NG7 2RD, England
*Correspondence e-mail: a.j.blake@nottingham.ac.uk

(Received 21 September 2005; accepted 26 September 2005; online 5 October 2005)

In the title compound, [Re(C10H8N2)(C6H15O3P)2(CO)2]PF6, the carbonyl ligands are mutually cis and lie trans to the N donors of the 2,2′-bipyridyl ligand, while the triethoxy­phosphine ligands are mutually trans. The ReI centres exhibit approximate octa­hedral coordination, the major distortions from which arise from the narrow bite angle of the 2,2′-bipyridyl ligand which is expressed in the N—Re—N angles of 74.0 (3) and 74.3 (3)°. There are two cations and two anions in the asymmetric unit. The title compound is of inter­est because it has been shown to be a photocatalyst for CO2 reduction [Ishitani, George, Ibusuki, Johnson, Koike, Nozaki, Pac, Turner & Westwell (1994). Inorg. Chem. 33, 4712–4717].

Comment

The title compound, (I)[link], is of inter­est because it has been shown to be a photocatalyst for CO2 reduction (Ishitani et al., 1994[Ishitani, O., George, M. W., Ibusuki, T., Johnson, F. P. A., Koike, K., Nozaki, K., Pac, C., Turner, J. J. & Westwell, J. R. (1994). Inorg. Chem. 33, 4712-4717.]). A structure determination showed that the carbonyl ligands are mutually cis, while the triethoxy­phosphine ligands are mutually trans. The carbonyl groups are trans to the N-atom donors of the 2,2′-bipyridyl (2,2′-bipy) ligand. The ReI centres occupy approximately octa­hedral coordination environments. The major distortions from ideal octa­hedral geometry arise from the narrow chelate angle of the 2,2′-bipyridyl ligand; the N—Re—N angles are 74.0 (3) and 74.3 (3)°.

[Scheme 1]

Rhenium complexes containing similar arrays of ligands are unusual; the only previous example of the (2,2′-bipy)Re(CO)2P2 fragment which has been structurally characterized is the less symmetrical cis,trans-dicarbon­yl(4,4′-dimethyl-2,2′-bipyrid­yl)(triethoxy­phosphine)(triphenyl­phosphine)rhenium(I) hexa­fluoro­phosphate (Koike et al., 2000[Koike, K., Tanabe, J., Toyama, S., Tsubaki, H., Sakamoto, K., Westwell, J. R., Johnson, F. P. A., Hori, H., Saitoh, H. & Ishitani, O. (2000). Inorg. Chem. 39, 2777-2783.]).

[Figure 1]
Figure 1
A view of the ordered cation–anion pair with the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. Except for the orientations of the ethoxy chain, the geometry of the other cation pair is similar.

Experimental

The title compound was prepared using the method reported previously by Ishitani et al. (1994[Ishitani, O., George, M. W., Ibusuki, T., Johnson, F. P. A., Koike, K., Nozaki, K., Pac, C., Turner, J. J. & Westwell, J. R. (1994). Inorg. Chem. 33, 4712-4717.]) by photolysis (> 360 nm long-pass filter) of (2,2′-bipyrid­yl)tricarbonyl­rhenium trifluoro­methane­sulfonate in MeCN in the presence of P(OEt)3. Reaction with NH4PF6 in MeOH yielded the title salt which was subjected to column chromatography on silica with MeCN/CH2Cl2 (1:5 v/v) as eluant. Crystals were obtained by slow diffusion of diethyl ether into a solution of the product in MeCN.

Crystal data
  • [Re(C10H8N2)(C6H15O3P)2(CO)2]PF6

  • Mr = 875.66

  • Orthorhombic, P c a 21

  • a = 30.821 (6) Å

  • b = 14.136 (3) Å

  • c = 15.571 (3) Å

  • V = 6784 (2) Å3

  • Z = 8

  • Dx = 1.715 Mg m−3

  • Mo Kα radiation

  • Cell parameters from 7686 reflections

  • θ = 2.4–28.8°

  • μ = 3.80 mm−1

  • T = 150 (2) K

  • Cuboid, yellow

  • 0.42 × 0.41 × 0.37 mm

Data collection
  • Bruker SMART APEX CCD area-detector diffractometer

  • ω scans

  • Absorption correction: multi-scan(SADABS; Sheldrick, 2001[Sheldrick, G. M. (2001). SADABS. Version 2.03. University of Göttingen, Germany.])Tmin = 0.114, Tmax = 0.245

  • 42198 measured reflections

  • 12592 independent reflections

  • 11418 reflections with I > 2σ(I)

  • Rint = 0.043

  • θmax = 29.0°

  • h = −41 → 41

  • k = −19 → 19

  • l = −11 → 20

Refinement
  • Refinement on F2

  • R[F2 > 2σ(F2)] = 0.033

  • wR(F2) = 0.074

  • S = 1.15

  • 12592 reflections

  • 790 parameters

  • H-atom parameters constrained

  • w = 1/[σ2(Fo2) + (0.027P)2 + 11.37P] where P = (Fo2 + 2Fc2)/3

  • (Δ/σ)max = 0.003

  • Δρmax = 1.26 e Å−3

  • Δρmin = −1.28 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 3084 Friedel pairs

  • Flack parameter: 0.265 (7)

The asymmetric unit contains two independent cation–anion pairs. In one of the cations there is disorder in the arms of one of the triethoxy­phosphine ligands. A disorder model was developed in which all three O atoms, but only one of the methyl­ene C atoms and none of the methyl C atoms, were refined over split sites. Similarity restraints were applied to all C—O and C—C distances involving disordered atoms. The major and minor disorder components refined to occupancies of 0.53 (1) and 0.47 (1), respectively, and these were fixed at 0.50 in the final cycles of least-squares refinement. The wide range of Ueq values for the C atoms is a reflection of the approximate nature of the disorder model. H atoms were placed geometrically and refined using a riding model, with C—H distances of 0.95–0.99 Å and with Uiso(H) = 1.5Ueq(C) for methyl H atoms and 1.2Ueq(C) for the other H atoms. The Flack parameter refined to 0.265 (7), indicating the presence of some inversion twinning. The highest peak and deepest trough in the final difference Fourier synthesis are located 0.81 Å from atom Re1A and 1.48 Å from Re1, respectively.

Data collection: SMART (Bruker, 2001[Bruker (2001). SAINT (Version 6.02a), SMART (Version 5.625) and SHELXTL (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2001[Bruker (2001). SAINT (Version 6.02a), SMART (Version 5.625) and SHELXTL (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT and SHELXTL (Bruker, 2001[Bruker (2001). SAINT (Version 6.02a), SMART (Version 5.625) and SHELXTL (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA.]); program(s) used to solve structure: SIR92 (Altomare et al., 1994[Altomare, A., Burla, M. C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A. & Polidori, G. (1994). J. Appl. Cryst. 27, 435.]; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997[Sheldrick, G. M. (1997). SHELXL97. University of Göttingen, Germany.]); molecular graphics: PLATON (Spek, 2003[Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.]); software used to prepare material for publication: enCIFer (Allen et al., 2004[Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338.]; PLATON).

Supporting information


Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT and SHELXTL (Bruker, 2001); program(s) used to solve structure: SIR92 (Altomare et al., 1994; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: enCIFer (Version 1.1; Allen et al., 2004; PLATON).

(2,2'-Bipyridyl)dicarbonylbis(triethoxyphosphine-κP)rhenium(I) hexafluorophosphate top
Crystal data top
[Re(C10H8N2)(C6H15O3P)2(CO)2]PF6Dx = 1.715 Mg m3
Mr = 875.66Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pca21Cell parameters from 7686 reflections
a = 30.821 (6) Åθ = 2.4–28.8°
b = 14.136 (3) ŵ = 3.80 mm1
c = 15.571 (3) ÅT = 150 K
V = 6784 (2) Å3Cuboid, yellow
Z = 80.42 × 0.41 × 0.37 mm
F(000) = 3472
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
12592 independent reflections
Radiation source: sealed tube11418 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.043
ω scansθmax = 29.0°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2001)
h = 4141
Tmin = 0.114, Tmax = 0.245k = 1919
42198 measured reflectionsl = 1120
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)] = 0.033H-atom parameters constrained
wR(F2) = 0.074 w = 1/[σ2(Fo2) + (0.027P)2 + 11.37P]
where P = (Fo2 + 2Fc2)/3
S = 1.15(Δ/σ)max = 0.003
12592 reflectionsΔρmax = 1.26 e Å3
790 parametersΔρmin = 1.28 e Å3
17 restraintsAbsolute structure: Flack (1983), 3084 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.265 (7)
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Re10.362857 (7)0.223761 (17)0.087268 (12)0.02148 (6)
P10.43886 (5)0.25000 (12)0.09253 (16)0.0277 (4)
P20.28643 (5)0.20979 (12)0.07425 (15)0.0287 (4)
C10.3537 (3)0.3136 (6)0.1759 (6)0.0344 (18)
O10.3484 (2)0.3682 (4)0.2320 (4)0.0543 (16)
C20.3685 (3)0.1268 (7)0.1739 (6)0.033 (2)
O20.3728 (2)0.0704 (4)0.2261 (5)0.0523 (17)
N10.35976 (16)0.3203 (5)0.0202 (5)0.0220 (14)
N20.37129 (17)0.1374 (4)0.0272 (4)0.0214 (13)
O30.46529 (13)0.1553 (4)0.0823 (5)0.0466 (14)
O40.45965 (18)0.3028 (4)0.1726 (4)0.0384 (14)
O50.45462 (16)0.3191 (5)0.0187 (4)0.0523 (18)
O60.25890 (15)0.1418 (3)0.1351 (3)0.0342 (11)
O70.27313 (14)0.1824 (4)0.0222 (3)0.0464 (13)
O80.26278 (15)0.3079 (3)0.0920 (5)0.0620 (17)
C30.3562 (2)0.4155 (5)0.0117 (6)0.0298 (16)
H3A0.35180.44120.04410.036*
C40.3585 (2)0.4760 (6)0.0802 (7)0.039 (2)
H4A0.35660.54230.07150.047*
C50.3637 (2)0.4399 (6)0.1619 (7)0.043 (2)
H5A0.36520.48050.21040.052*
C60.3668 (2)0.3437 (6)0.1711 (6)0.038 (2)
H6A0.37030.31680.22660.046*
C70.36490 (18)0.2867 (5)0.1004 (7)0.0259 (18)
C80.36995 (18)0.1809 (5)0.1039 (4)0.0220 (13)
C90.3736 (2)0.1318 (5)0.1817 (5)0.0366 (16)
H9A0.37250.16390.23520.044*
C100.3789 (2)0.0342 (6)0.1778 (6)0.0442 (19)
H10A0.38160.00120.22930.053*
C110.3802 (2)0.0115 (5)0.0997 (6)0.042 (2)
H11A0.38330.07830.09660.050*
C120.3769 (2)0.0430 (5)0.0256 (5)0.0298 (15)
H12A0.37870.01220.02850.036*
C130.5127 (2)0.1515 (6)0.0887 (9)0.060 (3)
H13A0.52580.15450.03080.072*
H13B0.52350.20580.12270.072*
C140.5249 (3)0.0593 (8)0.1323 (9)0.079 (4)
H14A0.55650.05530.13740.119*
H14B0.51180.05700.18960.119*
H14C0.51430.00610.09790.119*
C150.4557 (3)0.2603 (6)0.2584 (8)0.054 (2)
H15A0.42500.24520.27050.065*
H15B0.47270.20080.26090.065*
C160.4723 (3)0.3278 (8)0.3227 (6)0.061 (3)
H16A0.46940.30050.38020.091*
H16B0.50290.34130.31110.091*
H16C0.45550.38670.31950.091*
C170.4936 (3)0.3769 (7)0.0161 (7)0.058 (3)
H17A0.50760.37760.07330.069*
H17B0.51440.35020.02580.069*
C180.4816 (3)0.4753 (7)0.0095 (8)0.070 (3)
H18A0.50780.51450.01180.105*
H18B0.46790.47430.06620.105*
H18C0.46140.50180.03260.105*
C190.2668 (3)0.0429 (5)0.1348 (7)0.062 (3)
H19A0.27500.02260.07620.074*
H19B0.29130.02850.17380.074*
C200.2286 (3)0.0098 (7)0.1624 (9)0.099 (4)
H20A0.23510.07760.16270.148*
H20B0.22030.01040.22040.148*
H20C0.20450.00260.12270.148*
C210.2282 (3)0.1790 (9)0.0516 (6)0.082 (3)
H21A0.21350.23900.03670.098*
H21B0.21280.12680.02220.098*
C220.2262 (3)0.1649 (9)0.1417 (6)0.081 (3)
H22A0.19580.16450.16010.121*
H22B0.24170.21620.17080.121*
H22C0.23970.10420.15620.121*
C230.2239 (3)0.3238 (6)0.1366 (8)0.077 (3)
H23A0.20060.28350.11240.093*
H23B0.22760.30670.19780.093*
C240.2118 (3)0.4212 (6)0.1298 (7)0.079 (3)
H24A0.18430.43160.16000.119*
H24B0.23450.46070.15550.119*
H24C0.20840.43800.06910.119*
Re1A0.367270 (7)0.725429 (16)0.737972 (12)0.02039 (6)
P1A0.44335 (5)0.75241 (12)0.74876 (15)0.0258 (4)
P2A0.29260 (5)0.69640 (13)0.71431 (13)0.0259 (4)
C1A0.3700 (2)0.6348 (6)0.8267 (7)0.029 (2)
O1A0.37199 (19)0.5784 (4)0.8817 (5)0.0526 (18)
C2A0.3548 (2)0.8199 (6)0.8226 (6)0.0291 (17)
O2A0.34769 (18)0.8762 (4)0.8741 (4)0.0408 (13)
N1A0.36712 (14)0.8149 (5)0.6244 (5)0.0224 (14)
N2A0.38027 (18)0.6311 (4)0.6299 (4)0.0211 (12)
O3A0.46161 (16)0.8171 (4)0.6737 (4)0.0397 (14)
O4A0.46906 (13)0.6550 (3)0.7461 (5)0.0422 (14)
O5A0.46236 (16)0.8049 (4)0.8318 (4)0.0337 (13)
O6A0.2879 (2)0.5875 (5)0.6828 (5)0.0311 (17)*0.50
O6B0.2816 (3)0.6208 (6)0.6450 (7)0.033 (2)*0.50
O7A0.2614 (3)0.6643 (8)0.7862 (5)0.037 (2)*0.50
O7B0.2574 (3)0.7128 (6)0.7887 (5)0.0299 (19)*0.50
O8A0.2682 (3)0.7494 (6)0.6386 (7)0.028 (2)*0.50
O8B0.2721 (3)0.7910 (8)0.6754 (8)0.061 (3)*0.50
C3A0.36113 (19)0.9097 (5)0.6266 (6)0.0268 (16)
H3AA0.35540.93890.68040.032*
C4A0.36302 (19)0.9657 (5)0.5544 (7)0.0348 (19)
H4AA0.36001.03240.55840.042*
C5A0.3694 (2)0.9230 (6)0.4772 (7)0.0374 (19)
H5AA0.37030.96030.42640.045*
C6A0.3744 (2)0.8261 (5)0.4715 (5)0.0281 (14)
H6AA0.37830.79610.41740.034*
C7A0.3738 (2)0.7725 (4)0.5481 (5)0.0201 (13)
C8A0.38072 (17)0.6702 (4)0.5504 (4)0.0220 (13)
C9A0.38623 (19)0.6140 (5)0.4790 (5)0.0286 (14)
H9AA0.38680.64190.42350.034*
C10A0.3910 (2)0.5181 (5)0.4872 (6)0.0361 (18)
H10B0.39470.47940.43800.043*
C11A0.3902 (2)0.4791 (5)0.5677 (6)0.0349 (17)
H11B0.39320.41270.57490.042*
C12A0.3851 (2)0.5365 (4)0.6374 (5)0.0285 (15)
H12B0.38490.50890.69310.034*
C13A0.4999 (2)0.8780 (6)0.6731 (7)0.053 (2)
H13C0.52180.85260.63280.063*
H13D0.51300.88010.73120.063*
C14A0.4869 (4)0.9744 (8)0.6464 (10)0.093 (4)
H14D0.51251.01580.64630.140*
H14E0.46530.99920.68660.140*
H14F0.47450.97200.58850.140*
C15A0.5166 (2)0.6497 (5)0.7496 (7)0.048 (2)
H15C0.52890.65850.69140.058*
H15D0.52810.70010.78740.058*
C16A0.5286 (3)0.5570 (6)0.7831 (7)0.059 (3)
H16D0.56030.55200.78550.088*
H16E0.51710.50760.74540.088*
H16F0.51660.54930.84090.088*
C17A0.4567 (2)0.7682 (6)0.9181 (6)0.0434 (19)
H17C0.47630.71370.92720.052*
H17D0.42640.74610.92570.052*
C18A0.4664 (3)0.8432 (6)0.9813 (7)0.050 (2)
H18D0.46260.81821.03950.075*
H18E0.44670.89660.97250.075*
H18F0.49650.86450.97390.075*
C19A0.2479 (3)0.5477 (6)0.6486 (7)0.077 (3)
H19C0.22430.54960.69180.093*0.50
H19D0.23840.58200.59640.093*0.50
H19E0.22480.56600.60960.093*0.50
H19F0.23570.54810.70610.093*0.50
C20A0.2599 (3)0.4517 (6)0.6287 (9)0.087 (4)
H20D0.23420.41100.63210.130*
H20E0.28170.42990.66990.130*
H20F0.27200.44900.57050.130*
C21A0.2638 (3)0.6849 (8)0.8772 (5)0.068 (3)
H21C0.27750.74760.88520.081*0.50
H21D0.28260.63720.90530.081*0.50
H21E0.28300.72930.90570.081*0.50
H21F0.27680.62240.88000.081*0.50
C22A0.2216 (3)0.6848 (7)0.9185 (6)0.067 (2)
H22D0.22470.66520.97850.101*
H22E0.20230.64060.88850.101*
H22F0.20910.74860.91620.101*
C23A0.2462 (6)0.8383 (9)0.6577 (9)0.050 (4)*0.50
H23C0.26660.88400.68420.060*0.50
H23D0.22160.82780.69750.060*0.50
C23B0.2280 (4)0.7971 (9)0.6403 (9)0.049 (4)*0.50
H23E0.20700.81400.68580.059*0.50
H23F0.21920.73610.61430.059*0.50
C24A0.2303 (3)0.8742 (6)0.5724 (7)0.076 (3)
H24D0.21530.93470.58060.115*0.50
H24E0.21020.82810.54730.115*0.50
H24F0.25500.88330.53370.115*0.50
H24G0.20230.88180.54630.115*0.50
H24H0.25110.85670.52930.115*0.50
H24I0.23890.93280.59850.115*0.50
P30.39157 (7)0.72574 (13)0.21217 (14)0.0355 (4)
F10.36602 (16)0.8078 (4)0.2599 (4)0.0576 (16)
F20.36496 (19)0.7472 (6)0.1267 (5)0.079 (2)
F30.41680 (15)0.6437 (4)0.1636 (4)0.0556 (14)
F40.41860 (15)0.7056 (3)0.2975 (3)0.0506 (12)
F50.35538 (14)0.6523 (3)0.2418 (6)0.0685 (18)
F60.42756 (18)0.7991 (3)0.1839 (4)0.0609 (15)
P40.60029 (5)0.78284 (12)0.06173 (13)0.0265 (4)
F70.58061 (16)0.8604 (4)0.0002 (4)0.0638 (17)
F80.57075 (15)0.8221 (4)0.1379 (4)0.0642 (16)
F90.61997 (18)0.7056 (4)0.1265 (4)0.0575 (15)
F100.62998 (14)0.7446 (4)0.0139 (4)0.0555 (15)
F110.56293 (13)0.7092 (3)0.0359 (3)0.0411 (11)
F120.63835 (12)0.8546 (3)0.0910 (5)0.0432 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Re10.02439 (10)0.02392 (13)0.01614 (15)0.00483 (8)0.00090 (10)0.00229 (14)
P10.0277 (7)0.0359 (8)0.0196 (10)0.0086 (6)0.0044 (8)0.0047 (10)
P20.0241 (6)0.0346 (8)0.0274 (10)0.0009 (6)0.0057 (7)0.0012 (8)
C10.049 (4)0.035 (4)0.019 (4)0.008 (4)0.003 (4)0.000 (3)
O10.074 (4)0.056 (4)0.033 (4)0.008 (3)0.011 (3)0.023 (3)
C20.040 (4)0.038 (4)0.021 (5)0.007 (3)0.000 (3)0.008 (4)
O20.080 (4)0.047 (3)0.030 (4)0.019 (3)0.012 (3)0.021 (3)
N10.025 (3)0.019 (3)0.022 (4)0.0056 (19)0.001 (2)0.000 (2)
N20.019 (2)0.021 (3)0.024 (3)0.0012 (19)0.004 (2)0.008 (2)
O30.030 (2)0.053 (3)0.056 (4)0.0003 (19)0.009 (3)0.012 (4)
O40.048 (3)0.043 (3)0.024 (3)0.015 (2)0.016 (2)0.001 (3)
O50.029 (3)0.084 (5)0.044 (4)0.028 (3)0.009 (3)0.022 (4)
O60.037 (2)0.032 (2)0.034 (3)0.0072 (19)0.013 (2)0.004 (2)
O70.026 (2)0.091 (4)0.022 (3)0.016 (2)0.003 (2)0.005 (3)
O80.043 (3)0.040 (3)0.103 (5)0.010 (2)0.017 (4)0.017 (3)
C30.035 (3)0.026 (3)0.028 (4)0.002 (3)0.004 (3)0.001 (3)
C40.036 (3)0.037 (4)0.043 (5)0.002 (3)0.005 (3)0.001 (4)
C50.045 (4)0.042 (4)0.042 (6)0.002 (3)0.001 (3)0.018 (4)
C60.049 (4)0.045 (4)0.022 (4)0.007 (3)0.004 (3)0.003 (3)
C70.026 (3)0.019 (3)0.033 (5)0.005 (2)0.003 (3)0.001 (3)
C80.020 (3)0.033 (3)0.014 (3)0.002 (2)0.002 (2)0.005 (3)
C90.040 (3)0.045 (4)0.025 (4)0.007 (3)0.003 (3)0.010 (3)
C100.051 (4)0.048 (4)0.034 (4)0.008 (3)0.006 (4)0.026 (4)
C110.046 (4)0.027 (3)0.054 (6)0.008 (3)0.009 (4)0.019 (4)
C120.032 (3)0.028 (3)0.029 (4)0.004 (3)0.008 (3)0.005 (3)
C130.030 (3)0.071 (6)0.078 (7)0.006 (3)0.008 (5)0.005 (7)
C140.041 (4)0.092 (8)0.105 (11)0.020 (5)0.001 (6)0.024 (8)
C150.070 (5)0.059 (5)0.033 (5)0.017 (4)0.010 (5)0.009 (5)
C160.065 (5)0.091 (7)0.027 (5)0.005 (5)0.005 (4)0.014 (5)
C170.039 (4)0.085 (7)0.049 (6)0.038 (4)0.004 (4)0.014 (5)
C180.062 (6)0.083 (8)0.065 (8)0.027 (5)0.014 (5)0.021 (6)
C190.057 (5)0.032 (4)0.096 (8)0.001 (3)0.008 (5)0.003 (4)
C200.099 (8)0.069 (6)0.129 (12)0.035 (6)0.001 (8)0.025 (7)
C210.043 (5)0.157 (10)0.045 (6)0.026 (5)0.011 (4)0.019 (7)
C220.072 (6)0.127 (9)0.043 (5)0.021 (6)0.018 (5)0.009 (6)
C230.080 (6)0.055 (5)0.097 (9)0.017 (5)0.030 (6)0.005 (6)
C240.095 (7)0.065 (6)0.078 (8)0.021 (5)0.019 (6)0.013 (5)
Re1A0.02380 (10)0.02149 (12)0.01588 (14)0.00457 (8)0.00004 (10)0.00149 (14)
P1A0.0257 (6)0.0292 (8)0.0225 (11)0.0063 (5)0.0015 (8)0.0004 (9)
P2A0.0210 (6)0.0335 (8)0.0232 (10)0.0037 (6)0.0031 (6)0.0020 (7)
C1A0.026 (3)0.024 (3)0.036 (6)0.008 (2)0.001 (3)0.011 (4)
O1A0.074 (4)0.042 (3)0.042 (5)0.014 (3)0.012 (3)0.020 (3)
C2A0.027 (3)0.032 (4)0.028 (5)0.005 (3)0.009 (3)0.004 (3)
O2A0.061 (3)0.034 (3)0.027 (3)0.001 (2)0.014 (3)0.011 (2)
N1A0.019 (3)0.025 (3)0.023 (4)0.0025 (18)0.002 (2)0.001 (3)
N2A0.021 (2)0.025 (3)0.017 (3)0.004 (2)0.001 (2)0.002 (2)
O3A0.042 (3)0.060 (4)0.017 (3)0.026 (2)0.001 (2)0.002 (3)
O4A0.029 (2)0.047 (3)0.051 (4)0.0024 (18)0.011 (3)0.018 (3)
O5A0.035 (3)0.048 (3)0.018 (3)0.017 (2)0.004 (2)0.000 (3)
C3A0.028 (3)0.022 (3)0.030 (4)0.001 (2)0.003 (3)0.003 (3)
C4A0.035 (3)0.029 (3)0.041 (5)0.002 (3)0.000 (3)0.015 (4)
C5A0.039 (4)0.038 (4)0.035 (4)0.000 (3)0.003 (3)0.019 (4)
C6A0.036 (3)0.033 (3)0.016 (3)0.007 (3)0.003 (3)0.005 (3)
C7A0.021 (2)0.028 (3)0.011 (3)0.002 (2)0.002 (2)0.002 (3)
C8A0.017 (3)0.028 (3)0.021 (3)0.003 (2)0.003 (2)0.000 (3)
C9A0.030 (3)0.038 (3)0.017 (3)0.003 (3)0.001 (3)0.003 (3)
C10A0.030 (3)0.045 (4)0.034 (4)0.007 (3)0.002 (3)0.014 (3)
C11A0.036 (3)0.028 (3)0.041 (5)0.003 (3)0.001 (3)0.009 (3)
C12A0.037 (3)0.019 (3)0.030 (4)0.002 (2)0.002 (3)0.000 (3)
C13A0.033 (4)0.070 (6)0.054 (7)0.026 (4)0.002 (4)0.009 (5)
C14A0.093 (8)0.084 (8)0.102 (11)0.045 (6)0.034 (8)0.039 (8)
C15A0.028 (3)0.060 (5)0.057 (6)0.008 (3)0.012 (4)0.012 (5)
C16A0.047 (4)0.064 (6)0.066 (8)0.011 (4)0.002 (5)0.005 (5)
C17A0.050 (4)0.061 (5)0.019 (4)0.020 (3)0.013 (4)0.027 (4)
C18A0.052 (5)0.065 (5)0.034 (5)0.003 (4)0.003 (4)0.015 (4)
C19A0.062 (5)0.071 (5)0.099 (9)0.027 (5)0.013 (6)0.035 (6)
C20A0.076 (6)0.065 (6)0.119 (11)0.006 (5)0.019 (7)0.021 (6)
C21A0.047 (4)0.127 (8)0.029 (4)0.027 (5)0.009 (4)0.007 (5)
C22A0.062 (5)0.102 (7)0.038 (5)0.021 (5)0.022 (5)0.006 (5)
C24A0.082 (6)0.068 (5)0.079 (8)0.025 (5)0.019 (6)0.010 (6)
P30.0550 (10)0.0280 (9)0.0233 (11)0.0031 (8)0.0000 (8)0.0006 (8)
F10.083 (4)0.040 (2)0.049 (4)0.016 (2)0.005 (3)0.012 (2)
F20.094 (5)0.102 (5)0.043 (4)0.034 (3)0.025 (3)0.012 (4)
F30.058 (3)0.049 (3)0.059 (4)0.006 (2)0.008 (3)0.019 (3)
F40.068 (3)0.056 (3)0.029 (2)0.006 (2)0.004 (2)0.011 (2)
F50.052 (2)0.049 (3)0.104 (6)0.013 (2)0.015 (4)0.001 (4)
F60.092 (4)0.041 (3)0.049 (4)0.019 (2)0.011 (3)0.013 (2)
P40.0294 (7)0.0274 (8)0.0227 (10)0.0061 (6)0.0014 (6)0.0011 (7)
F70.056 (3)0.053 (3)0.082 (5)0.006 (2)0.012 (3)0.041 (3)
F80.056 (3)0.076 (3)0.061 (4)0.010 (2)0.027 (3)0.030 (3)
F90.065 (3)0.058 (3)0.049 (3)0.007 (3)0.022 (3)0.025 (3)
F100.046 (3)0.075 (3)0.046 (4)0.014 (2)0.017 (2)0.028 (3)
F110.036 (2)0.047 (2)0.040 (3)0.0151 (17)0.0016 (19)0.004 (2)
F120.0415 (19)0.042 (2)0.046 (3)0.0165 (17)0.002 (2)0.002 (3)
Geometric parameters (Å, º) top
Re1—C11.896 (9)P4—F71.581 (5)
Re1—C21.931 (10)P4—F81.595 (5)
Re1—N12.162 (8)P4—F91.605 (5)
Re1—N22.176 (6)P4—F101.587 (6)
Re1—P12.3730 (15)P4—F111.603 (4)
Re1—P22.3724 (16)P4—F121.616 (4)
P1—O31.575 (5)C3—H3A0.95
P1—O41.588 (6)C4—H4A0.95
P1—O51.585 (7)C5—H5A0.95
P2—O61.594 (5)C6—H6A0.95
P2—O71.604 (5)C9—H9A0.95
P2—O81.591 (5)C10—H10A0.95
C1—O11.178 (10)C11—H11A0.95
C2—O21.147 (11)C12—H12A0.95
N1—C71.346 (13)C13—H13A0.99
N1—C31.357 (10)C13—H13B0.99
N2—C81.344 (9)C14—H14A0.98
N2—C121.346 (9)C14—H14B0.98
O3—C131.466 (7)C14—H14C0.98
O4—C151.470 (13)C15—H15A0.99
O5—C171.454 (8)C15—H15B0.99
O6—C191.419 (8)C16—H16A0.98
O7—C211.458 (9)C16—H16B0.98
O8—C231.405 (10)C16—H16C0.98
C3—C41.368 (12)C17—H17A0.99
C4—C51.381 (14)C17—H17B0.99
C5—C61.370 (12)C18—H18A0.98
C6—C71.366 (13)C18—H18B0.98
C7—C81.504 (10)C18—H18C0.98
C8—C91.400 (10)C19—H19A0.99
C9—C101.390 (11)C19—H19B0.99
C10—C111.377 (13)C20—H20A0.98
C11—C121.392 (11)C20—H20B0.98
C13—C141.516 (13)C20—H20C0.98
C15—C161.474 (13)C21—H21A0.99
C17—C181.493 (13)C21—H21B0.99
C19—C201.459 (11)C22—H22A0.98
C21—C221.417 (13)C22—H22B0.98
C23—C241.431 (11)C22—H22C0.98
Re1A—C1A1.886 (9)C23—H23A0.99
Re1A—C2A1.915 (9)C23—H23B0.99
Re1A—N1A2.174 (8)C24—H24A0.98
Re1A—N2A2.184 (6)C24—H24B0.98
Re1A—P1A2.3817 (15)C24—H24C0.98
Re1A—P2A2.3664 (16)C3A—H3AA0.95
P1A—O3A1.587 (6)C4A—H4AA0.95
P1A—O4A1.589 (5)C5A—H5AA0.95
P1A—O5A1.602 (6)C6A—H6AA0.95
P2A—O6B1.557 (9)C9A—H9AA0.95
P2A—O7A1.545 (10)C10A—H10B0.95
P2A—O8A1.586 (10)C11A—H11B0.95
P2A—O8B1.598 (11)C12A—H12B0.95
P2A—O7B1.604 (8)C13A—H13C0.99
P2A—O6A1.623 (7)C13A—H13D0.99
C1A—O1A1.172 (11)C14A—H14D0.98
C2A—O2A1.151 (10)C14A—H14E0.98
N1A—C7A1.346 (11)C14A—H14F0.98
N1A—C3A1.354 (10)C15A—H15C0.99
N2A—C12A1.351 (8)C15A—H15D0.99
N2A—C8A1.356 (9)C16A—H16D0.98
O3A—C13A1.462 (8)C16A—H16E0.98
O4A—C15A1.468 (7)C16A—H16F0.98
O5A—C17A1.450 (10)C17A—H17C0.99
O6A—C19A1.457 (8)C17A—H17D0.99
O6B—C19A1.467 (8)C18A—H18D0.98
O7A—C21A1.448 (8)C18A—H18E0.98
O7B—C21A1.447 (8)C18A—H18F0.98
O8A—C23A1.458 (9)C19A—H19C0.99
O8B—C23B1.467 (8)C19A—H19D0.99
C3A—C4A1.376 (12)C19A—H19E0.97
C4A—C5A1.360 (14)C19A—H19F0.97
C5A—C6A1.382 (11)C20A—H20D0.98
C6A—C7A1.413 (10)C20A—H20E0.98
C7A—C8A1.461 (9)C20A—H20F0.98
C8A—C9A1.378 (9)C21A—H21C0.99
C9A—C10A1.368 (9)C21A—H21D0.99
C10A—C11A1.369 (12)C21A—H21E0.97
C11A—C12A1.364 (11)C21A—H21F0.97
C13A—C14A1.479 (13)C22A—H22D0.98
C15A—C16A1.458 (11)C22A—H22E0.98
C17A—C18A1.478 (13)C22A—H22F0.98
C19A—C20A1.440 (11)C23A—H23C0.99
C21A—C22A1.453 (10)C23A—H23D0.99
C23A—C24A1.506 (15)C23B—H23E0.99
C23B—C24A1.521 (14)C23B—H23F0.99
P3—F11.586 (5)C24A—H24D0.98
P3—F21.592 (7)C24A—H24E0.98
P3—F31.588 (5)C24A—H24F0.98
P3—F41.594 (5)C24A—H24G0.96
P3—F51.592 (5)C24A—H24H0.96
P3—F61.581 (5)C24A—H24I0.96
C1—Re1—C288.9 (4)C17—C18—H18B109.5
C1—Re1—N197.7 (3)H18A—C18—H18B109.5
C2—Re1—N1173.2 (3)C17—C18—H18C109.5
C1—Re1—N2171.7 (3)H18A—C18—H18C109.5
C2—Re1—N299.4 (3)H18B—C18—H18C109.5
N1—Re1—N274.0 (3)O6—C19—H19A109.1
C1—Re1—P288.3 (3)C20—C19—H19A109.1
C2—Re1—P295.2 (2)O6—C19—H19B109.1
N1—Re1—P286.71 (14)C20—C19—H19B109.1
N2—Re1—P290.11 (15)H19A—C19—H19B107.8
C1—Re1—P190.9 (3)C19—C20—H20A109.5
C2—Re1—P189.9 (2)C19—C20—H20B109.5
N1—Re1—P188.37 (14)H20A—C20—H20B109.5
N2—Re1—P189.89 (15)C19—C20—H20C109.5
P2—Re1—P1174.88 (7)H20A—C20—H20C109.5
O3—P1—O5107.0 (4)H20B—C20—H20C109.5
O3—P1—O4105.7 (3)C22—C21—H21A109.4
O5—P1—O499.0 (3)O7—C21—H21A109.5
O3—P1—Re1111.99 (18)C22—C21—H21B109.5
O5—P1—Re1112.0 (2)O7—C21—H21B109.5
O4—P1—Re1119.9 (2)H21A—C21—H21B108.0
O8—P2—O6100.3 (3)C21—C22—H22A109.5
O8—P2—O7104.8 (4)C21—C22—H22B109.5
O6—P2—O7105.9 (3)H22A—C22—H22B109.5
O8—P2—Re1111.6 (2)C21—C22—H22C109.5
O6—P2—Re1121.9 (2)H22A—C22—H22C109.5
O7—P2—Re1110.72 (18)H22B—C22—H22C109.5
O1—C1—Re1178.8 (9)O8—C23—H23A109.9
O2—C2—Re1178.2 (8)C24—C23—H23A110.0
C7—N1—C3116.8 (8)O8—C23—H23B110.0
C7—N1—Re1119.3 (5)C24—C23—H23B110.0
C3—N1—Re1123.6 (6)H23A—C23—H23B108.4
C8—N2—C12118.3 (7)C23—C24—H24A109.5
C8—N2—Re1117.9 (4)C23—C24—H24B109.4
C12—N2—Re1123.8 (6)H24A—C24—H24B109.5
C13—O3—P1122.7 (5)C23—C24—H24C109.5
C15—O4—P1119.2 (5)H24A—C24—H24C109.5
C17—O5—P1128.3 (6)H24B—C24—H24C109.5
C19—O6—P2120.1 (5)N1A—C3A—H3AA118.7
C21—O7—P2123.0 (5)C4A—C3A—H3AA118.7
C23—O8—P2128.0 (5)C5A—C4A—H4AA120.8
N1—C3—C4122.5 (9)C3A—C4A—H4AA120.9
C3—C4—C5119.6 (8)C4A—C5A—H5AA119.6
C6—C5—C4118.1 (9)C6A—C5A—H5AA119.6
C7—C6—C5119.9 (9)C5A—C6A—H6AA120.8
N1—C7—C6123.0 (7)C7A—C6A—H6AA120.8
N1—C7—C8113.4 (7)C10A—C9A—H9AA119.6
C6—C7—C8123.6 (8)C8A—C9A—H9AA119.6
N2—C8—C9122.6 (6)C9A—C10A—H10B120.5
N2—C8—C7115.2 (6)C11A—C10A—H10B120.4
C9—C8—C7122.2 (7)C12A—C11A—H11B120.6
C10—C9—C8117.7 (7)C10A—C11A—H11B120.6
C11—C10—C9120.5 (7)N2A—C12A—H12B119.0
C10—C11—C12118.1 (7)C11A—C12A—H12B119.0
N2—C12—C11122.9 (8)O3A—C13A—H13C110.0
O3—C13—C14108.0 (7)C14A—C13A—H13C110.0
O4—C15—C16108.9 (7)O3A—C13A—H13D110.0
O5—C17—C18109.1 (7)C14A—C13A—H13D110.0
O6—C19—C20111.3 (7)H13C—C13A—H13D108.4
C22—C21—O7110.9 (8)C13A—C14A—H14D109.5
O8—C23—C24109.8 (8)C13A—C14A—H14E109.5
C1A—Re1A—C2A88.8 (4)H14D—C14A—H14E109.5
C1A—Re1A—N1A172.4 (4)C13A—C14A—H14F109.5
C2A—Re1A—N1A98.8 (3)H14D—C14A—H14F109.5
C1A—Re1A—N2A98.1 (3)H14E—C14A—H14F109.5
C2A—Re1A—N2A173.1 (3)C16A—C15A—H15C110.1
N1A—Re1A—N2A74.3 (3)O4A—C15A—H15C110.1
C1A—Re1A—P2A92.3 (2)C16A—C15A—H15D110.1
C2A—Re1A—P2A91.9 (2)O4A—C15A—H15D110.1
N1A—Re1A—P2A88.41 (13)H15C—C15A—H15D108.4
N2A—Re1A—P2A87.28 (15)C15A—C16A—H16D109.5
C1A—Re1A—P1A90.8 (2)C15A—C16A—H16E109.5
C2A—Re1A—P1A92.2 (2)H16D—C16A—H16E109.5
N1A—Re1A—P1A88.07 (13)C15A—C16A—H16F109.5
N2A—Re1A—P1A88.36 (15)H16D—C16A—H16F109.5
P2A—Re1A—P1A175.01 (8)H16E—C16A—H16F109.5
O3A—P1A—O4A107.6 (4)O5A—C17A—H17C109.8
O3A—P1A—O5A101.4 (3)C18A—C17A—H17C109.9
O4A—P1A—O5A103.9 (3)O5A—C17A—H17D109.9
O3A—P1A—Re1A112.9 (2)C18A—C17A—H17D109.8
O4A—P1A—Re1A110.51 (17)H17C—C17A—H17D108.3
O5A—P1A—Re1A119.4 (2)C17A—C18A—H18D109.5
O7A—P2A—O8A112.4 (5)C17A—C18A—H18E109.5
O6B—P2A—O8B103.0 (6)H18D—C18A—H18E109.5
O6B—P2A—O7B116.9 (4)C17A—C18A—H18F109.4
O8B—P2A—O7B83.4 (5)H18D—C18A—H18F109.5
O7A—P2A—O6A83.3 (5)H18E—C18A—H18F109.5
O8A—P2A—O6A100.4 (5)C20A—C19A—H19C111.0
O7A—P2A—Re1A123.0 (3)O6A—C19A—H19C111.0
O6B—P2A—Re1A116.1 (3)O6B—C19A—H19C121.3
O8A—P2A—Re1A119.7 (3)C20A—C19A—H19D111.0
O8B—P2A—Re1A107.4 (4)O6A—C19A—H19D111.0
O7B—P2A—Re1A121.4 (3)H19C—C19A—H19D109.0
O6A—P2A—Re1A107.4 (2)C20A—C19A—H19E107.3
O1A—C1A—Re1A179.5 (8)O6B—C19A—H19E107.8
O2A—C2A—Re1A179.1 (8)C20A—C19A—H19F107.4
C7A—N1A—C3A119.0 (8)O6B—C19A—H19F107.5
C7A—N1A—Re1A117.3 (5)H19E—C19A—H19F107.1
C3A—N1A—Re1A123.8 (6)C19A—C20A—H20D109.5
C12A—N2A—C8A118.8 (6)C19A—C20A—H20E109.5
C12A—N2A—Re1A124.0 (5)H20D—C20A—H20E109.5
C8A—N2A—Re1A117.2 (4)C19A—C20A—H20F109.5
C13A—O3A—P1A129.1 (6)H20D—C20A—H20F109.5
C15A—O4A—P1A122.8 (4)H20E—C20A—H20F109.5
C17A—O5A—P1A122.5 (5)O7A—C21A—H21C109.0
C19A—O6A—P2A123.6 (6)C22A—C21A—H21C109.0
C19A—O6B—P2A127.8 (8)O7A—C21A—H21D108.9
C21A—O7A—P2A128.1 (7)C22A—C21A—H21D108.9
C21A—O7B—P2A123.8 (6)H21C—C21A—H21D107.8
C23A—O8A—P2A118.4 (8)O7B—C21A—H21E110.1
N1A—C3A—C4A122.9 (8)C22A—C21A—H21E109.9
C5A—C4A—C3A118.3 (7)O7B—C21A—H21F110.6
C4A—C5A—C6A120.8 (8)C22A—C21A—H21F110.4
C5A—C6A—C7A118.5 (8)H21E—C21A—H21F108.5
N1A—C7A—C6A120.5 (6)C21A—C22A—H22D109.5
N1A—C7A—C8A116.2 (7)C21A—C22A—H22E109.5
C6A—C7A—C8A123.2 (7)H22D—C22A—H22E109.5
N2A—C8A—C9A120.2 (6)C21A—C22A—H22F109.4
N2A—C8A—C7A115.1 (6)H22D—C22A—H22F109.5
C9A—C8A—C7A124.7 (6)H22E—C22A—H22F109.5
C10A—C9A—C8A120.6 (7)O8A—C23A—H23C110.6
C9A—C10A—C11A118.9 (7)C24A—C23A—H23C110.6
C12A—C11A—C10A119.4 (7)O8A—C23A—H23D110.6
N2A—C12A—C11A122.2 (7)C24A—C23A—H23D110.6
O3A—C13A—C14A109.0 (7)H23C—C23A—H23D108.7
C16A—C15A—O4A108.3 (7)O8B—C23B—H23E110.7
O5A—C17A—C18A109.6 (7)C24A—C23B—H23E110.7
C20A—C19A—O6A102.9 (8)O8B—C23B—H23F110.7
O7B—C21A—C22A107.4 (8)C24A—C23B—H23F110.7
O7A—C21A—C22A112.6 (8)H23E—C23B—H23F108.8
O8A—C23A—C24A105.2 (9)C23A—C24A—H24D109.5
N1—C3—H3A118.5C23A—C24A—H24E109.5
C4—C3—H3A118.5H24D—C24A—H24E109.5
C3—C4—H4A120.3C23A—C24A—H24F109.4
C5—C4—H4A120.3H24D—C24A—H24F109.5
C6—C5—H5A121.0H24E—C24A—H24F109.5
C4—C5—H5A121.0C23B—C24A—H24G109.6
C7—C6—H6A119.6C23B—C24A—H24H109.1
C5—C6—H6A119.6H24D—C24A—H24H129.4
C10—C9—H9A120.9H24G—C24A—H24H109.5
C8—C9—H9A120.9C23B—C24A—H24I109.7
C9—C10—H10A119.8H24G—C24A—H24I109.5
C10—C11—H11A120.9H24H—C24A—H24I109.5
C12—C11—H11A120.9F6—P3—F190.0 (3)
N2—C12—H12A118.6F6—P3—F390.1 (3)
C11—C12—H12A118.6F1—P3—F3179.4 (3)
O3—C13—H13A110.0F6—P3—F290.2 (4)
C14—C13—H13A110.0F1—P3—F289.8 (4)
O3—C13—H13B110.0F3—P3—F289.6 (3)
C14—C13—H13B110.0F6—P3—F5179.3 (4)
H13A—C13—H13B108.4F1—P3—F589.6 (3)
C13—C14—H14A109.5F3—P3—F590.3 (3)
C13—C14—H14B109.5F2—P3—F590.3 (4)
H14A—C14—H14B109.5F6—P3—F489.0 (3)
C13—C14—H14C109.5F1—P3—F490.0 (3)
H14A—C14—H14C109.5F3—P3—F490.6 (3)
H14B—C14—H14C109.5F2—P3—F4179.2 (4)
O4—C15—H15A110.1F5—P3—F490.5 (4)
C16—C15—H15A110.2F7—P4—F1090.3 (4)
O4—C15—H15B110.1F7—P4—F889.6 (3)
C16—C15—H15B110.1F10—P4—F8179.5 (3)
H15A—C15—H15B108.4F7—P4—F1191.2 (3)
C15—C16—H16A109.5F10—P4—F1190.4 (3)
C15—C16—H16B109.5F8—P4—F1190.1 (3)
H16A—C16—H16B109.5F7—P4—F9178.6 (4)
C15—C16—H16C109.4F10—P4—F991.0 (4)
H16A—C16—H16C109.5F8—P4—F989.1 (3)
H16B—C16—H16C109.5F11—P4—F989.3 (3)
O5—C17—H17A109.9F7—P4—F1290.9 (3)
C18—C17—H17A109.9F10—P4—F1290.3 (3)
O5—C17—H17B109.8F8—P4—F1289.2 (3)
C18—C17—H17B109.9F11—P4—F12177.8 (3)
H17A—C17—H17B108.3F9—P4—F1288.6 (3)
C17—C18—H18A109.5
 

Acknowledgements

We thank the Overseas Research Students Awards Scheme for an ORS award to MKK, and EPSRC (UK) for the award of a diffractometer.

References

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