metal-organic compounds
(2,2′-Bipyridyl)dicarbonylbis(triethoxyphosphine-κP)rhenium(I) hexafluorophosphate
aSchool of Chemistry, The University of Nottingham, University Park, Nottingham NG7 2RD, England
*Correspondence e-mail: a.j.blake@nottingham.ac.uk
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 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), is of interest because it has been shown to be a photocatalyst for CO2 reduction (Ishitani et al., 1994). A 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)°.
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).
Experimental
The title compound was prepared using the method reported previously by Ishitani et al. (1994) 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 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
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The 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 refined to 0.265 (7), indicating the presence of some inversion 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.
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 The wide range ofData collection: SMART (Bruker, 2001); cell 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 (Allen et al., 2004; PLATON).
Supporting information
https://doi.org/10.1107/S1600536805030643/om6264sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536805030643/om6264Isup2.hkl
Data collection: SMART (Bruker, 2001); cell
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).[Re(C10H8N2)(C6H15O3P)2(CO)2]PF6 | Dx = 1.715 Mg m−3 |
Mr = 875.66 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pca21 | Cell parameters from 7686 reflections |
a = 30.821 (6) Å | θ = 2.4–28.8° |
b = 14.136 (3) Å | µ = 3.80 mm−1 |
c = 15.571 (3) Å | T = 150 K |
V = 6784 (2) Å3 | Cuboid, yellow |
Z = 8 | 0.42 × 0.41 × 0.37 mm |
F(000) = 3472 |
Bruker SMART APEX CCD area-detector diffractometer | 12592 independent reflections |
Radiation source: sealed tube | 11418 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.043 |
ω scans | θmax = 29.0°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2001) | h = −41→41 |
Tmin = 0.114, Tmax = 0.245 | k = −19→19 |
42198 measured reflections | l = −11→20 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.033 | H-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 reflections | Δρmax = 1.26 e Å−3 |
790 parameters | Δρmin = −1.28 e Å−3 |
17 restraints | Absolute structure: Flack (1983), 3084 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.265 (7) |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Re1 | 0.362857 (7) | 0.223761 (17) | −0.087268 (12) | 0.02148 (6) | |
P1 | 0.43886 (5) | 0.25000 (12) | −0.09253 (16) | 0.0277 (4) | |
P2 | 0.28643 (5) | 0.20979 (12) | −0.07425 (15) | 0.0287 (4) | |
C1 | 0.3537 (3) | 0.3136 (6) | −0.1759 (6) | 0.0344 (18) | |
O1 | 0.3484 (2) | 0.3682 (4) | −0.2320 (4) | 0.0543 (16) | |
C2 | 0.3685 (3) | 0.1268 (7) | −0.1739 (6) | 0.033 (2) | |
O2 | 0.3728 (2) | 0.0704 (4) | −0.2261 (5) | 0.0523 (17) | |
N1 | 0.35976 (16) | 0.3203 (5) | 0.0202 (5) | 0.0220 (14) | |
N2 | 0.37129 (17) | 0.1374 (4) | 0.0272 (4) | 0.0214 (13) | |
O3 | 0.46529 (13) | 0.1553 (4) | −0.0823 (5) | 0.0466 (14) | |
O4 | 0.45965 (18) | 0.3028 (4) | −0.1726 (4) | 0.0384 (14) | |
O5 | 0.45462 (16) | 0.3191 (5) | −0.0187 (4) | 0.0523 (18) | |
O6 | 0.25890 (15) | 0.1418 (3) | −0.1351 (3) | 0.0342 (11) | |
O7 | 0.27313 (14) | 0.1824 (4) | 0.0222 (3) | 0.0464 (13) | |
O8 | 0.26278 (15) | 0.3079 (3) | −0.0920 (5) | 0.0620 (17) | |
C3 | 0.3562 (2) | 0.4155 (5) | 0.0117 (6) | 0.0298 (16) | |
H3A | 0.3518 | 0.4412 | −0.0441 | 0.036* | |
C4 | 0.3585 (2) | 0.4760 (6) | 0.0802 (7) | 0.039 (2) | |
H4A | 0.3566 | 0.5423 | 0.0715 | 0.047* | |
C5 | 0.3637 (2) | 0.4399 (6) | 0.1619 (7) | 0.043 (2) | |
H5A | 0.3652 | 0.4805 | 0.2104 | 0.052* | |
C6 | 0.3668 (2) | 0.3437 (6) | 0.1711 (6) | 0.038 (2) | |
H6A | 0.3703 | 0.3168 | 0.2266 | 0.046* | |
C7 | 0.36490 (18) | 0.2867 (5) | 0.1004 (7) | 0.0259 (18) | |
C8 | 0.36995 (18) | 0.1809 (5) | 0.1039 (4) | 0.0220 (13) | |
C9 | 0.3736 (2) | 0.1318 (5) | 0.1817 (5) | 0.0366 (16) | |
H9A | 0.3725 | 0.1639 | 0.2352 | 0.044* | |
C10 | 0.3789 (2) | 0.0342 (6) | 0.1778 (6) | 0.0442 (19) | |
H10A | 0.3816 | −0.0012 | 0.2293 | 0.053* | |
C11 | 0.3802 (2) | −0.0115 (5) | 0.0997 (6) | 0.042 (2) | |
H11A | 0.3833 | −0.0783 | 0.0966 | 0.050* | |
C12 | 0.3769 (2) | 0.0430 (5) | 0.0256 (5) | 0.0298 (15) | |
H12A | 0.3787 | 0.0122 | −0.0285 | 0.036* | |
C13 | 0.5127 (2) | 0.1515 (6) | −0.0887 (9) | 0.060 (3) | |
H13A | 0.5258 | 0.1545 | −0.0308 | 0.072* | |
H13B | 0.5235 | 0.2058 | −0.1227 | 0.072* | |
C14 | 0.5249 (3) | 0.0593 (8) | −0.1323 (9) | 0.079 (4) | |
H14A | 0.5565 | 0.0553 | −0.1374 | 0.119* | |
H14B | 0.5118 | 0.0570 | −0.1896 | 0.119* | |
H14C | 0.5143 | 0.0061 | −0.0979 | 0.119* | |
C15 | 0.4557 (3) | 0.2603 (6) | −0.2584 (8) | 0.054 (2) | |
H15A | 0.4250 | 0.2452 | −0.2705 | 0.065* | |
H15B | 0.4727 | 0.2008 | −0.2609 | 0.065* | |
C16 | 0.4723 (3) | 0.3278 (8) | −0.3227 (6) | 0.061 (3) | |
H16A | 0.4694 | 0.3005 | −0.3802 | 0.091* | |
H16B | 0.5029 | 0.3413 | −0.3111 | 0.091* | |
H16C | 0.4555 | 0.3867 | −0.3195 | 0.091* | |
C17 | 0.4936 (3) | 0.3769 (7) | −0.0161 (7) | 0.058 (3) | |
H17A | 0.5076 | 0.3776 | −0.0733 | 0.069* | |
H17B | 0.5144 | 0.3502 | 0.0258 | 0.069* | |
C18 | 0.4816 (3) | 0.4753 (7) | 0.0095 (8) | 0.070 (3) | |
H18A | 0.5078 | 0.5145 | 0.0118 | 0.105* | |
H18B | 0.4679 | 0.4743 | 0.0662 | 0.105* | |
H18C | 0.4614 | 0.5018 | −0.0326 | 0.105* | |
C19 | 0.2668 (3) | 0.0429 (5) | −0.1348 (7) | 0.062 (3) | |
H19A | 0.2750 | 0.0226 | −0.0762 | 0.074* | |
H19B | 0.2913 | 0.0285 | −0.1738 | 0.074* | |
C20 | 0.2286 (3) | −0.0098 (7) | −0.1624 (9) | 0.099 (4) | |
H20A | 0.2351 | −0.0776 | −0.1627 | 0.148* | |
H20B | 0.2203 | 0.0104 | −0.2204 | 0.148* | |
H20C | 0.2045 | 0.0026 | −0.1227 | 0.148* | |
C21 | 0.2282 (3) | 0.1790 (9) | 0.0516 (6) | 0.082 (3) | |
H21A | 0.2135 | 0.2390 | 0.0367 | 0.098* | |
H21B | 0.2128 | 0.1268 | 0.0222 | 0.098* | |
C22 | 0.2262 (3) | 0.1649 (9) | 0.1417 (6) | 0.081 (3) | |
H22A | 0.1958 | 0.1645 | 0.1601 | 0.121* | |
H22B | 0.2417 | 0.2162 | 0.1708 | 0.121* | |
H22C | 0.2397 | 0.1042 | 0.1562 | 0.121* | |
C23 | 0.2239 (3) | 0.3238 (6) | −0.1366 (8) | 0.077 (3) | |
H23A | 0.2006 | 0.2835 | −0.1124 | 0.093* | |
H23B | 0.2276 | 0.3067 | −0.1978 | 0.093* | |
C24 | 0.2118 (3) | 0.4212 (6) | −0.1298 (7) | 0.079 (3) | |
H24A | 0.1843 | 0.4316 | −0.1600 | 0.119* | |
H24B | 0.2345 | 0.4607 | −0.1555 | 0.119* | |
H24C | 0.2084 | 0.4380 | −0.0691 | 0.119* | |
Re1A | 0.367270 (7) | 0.725429 (16) | 0.737972 (12) | 0.02039 (6) | |
P1A | 0.44335 (5) | 0.75241 (12) | 0.74876 (15) | 0.0258 (4) | |
P2A | 0.29260 (5) | 0.69640 (13) | 0.71431 (13) | 0.0259 (4) | |
C1A | 0.3700 (2) | 0.6348 (6) | 0.8267 (7) | 0.029 (2) | |
O1A | 0.37199 (19) | 0.5784 (4) | 0.8817 (5) | 0.0526 (18) | |
C2A | 0.3548 (2) | 0.8199 (6) | 0.8226 (6) | 0.0291 (17) | |
O2A | 0.34769 (18) | 0.8762 (4) | 0.8741 (4) | 0.0408 (13) | |
N1A | 0.36712 (14) | 0.8149 (5) | 0.6244 (5) | 0.0224 (14) | |
N2A | 0.38027 (18) | 0.6311 (4) | 0.6299 (4) | 0.0211 (12) | |
O3A | 0.46161 (16) | 0.8171 (4) | 0.6737 (4) | 0.0397 (14) | |
O4A | 0.46906 (13) | 0.6550 (3) | 0.7461 (5) | 0.0422 (14) | |
O5A | 0.46236 (16) | 0.8049 (4) | 0.8318 (4) | 0.0337 (13) | |
O6A | 0.2879 (2) | 0.5875 (5) | 0.6828 (5) | 0.0311 (17)* | 0.50 |
O6B | 0.2816 (3) | 0.6208 (6) | 0.6450 (7) | 0.033 (2)* | 0.50 |
O7A | 0.2614 (3) | 0.6643 (8) | 0.7862 (5) | 0.037 (2)* | 0.50 |
O7B | 0.2574 (3) | 0.7128 (6) | 0.7887 (5) | 0.0299 (19)* | 0.50 |
O8A | 0.2682 (3) | 0.7494 (6) | 0.6386 (7) | 0.028 (2)* | 0.50 |
O8B | 0.2721 (3) | 0.7910 (8) | 0.6754 (8) | 0.061 (3)* | 0.50 |
C3A | 0.36113 (19) | 0.9097 (5) | 0.6266 (6) | 0.0268 (16) | |
H3AA | 0.3554 | 0.9389 | 0.6804 | 0.032* | |
C4A | 0.36302 (19) | 0.9657 (5) | 0.5544 (7) | 0.0348 (19) | |
H4AA | 0.3600 | 1.0324 | 0.5584 | 0.042* | |
C5A | 0.3694 (2) | 0.9230 (6) | 0.4772 (7) | 0.0374 (19) | |
H5AA | 0.3703 | 0.9603 | 0.4264 | 0.045* | |
C6A | 0.3744 (2) | 0.8261 (5) | 0.4715 (5) | 0.0281 (14) | |
H6AA | 0.3783 | 0.7961 | 0.4174 | 0.034* | |
C7A | 0.3738 (2) | 0.7725 (4) | 0.5481 (5) | 0.0201 (13) | |
C8A | 0.38072 (17) | 0.6702 (4) | 0.5504 (4) | 0.0220 (13) | |
C9A | 0.38623 (19) | 0.6140 (5) | 0.4790 (5) | 0.0286 (14) | |
H9AA | 0.3868 | 0.6419 | 0.4235 | 0.034* | |
C10A | 0.3910 (2) | 0.5181 (5) | 0.4872 (6) | 0.0361 (18) | |
H10B | 0.3947 | 0.4794 | 0.4380 | 0.043* | |
C11A | 0.3902 (2) | 0.4791 (5) | 0.5677 (6) | 0.0349 (17) | |
H11B | 0.3932 | 0.4127 | 0.5749 | 0.042* | |
C12A | 0.3851 (2) | 0.5365 (4) | 0.6374 (5) | 0.0285 (15) | |
H12B | 0.3849 | 0.5089 | 0.6931 | 0.034* | |
C13A | 0.4999 (2) | 0.8780 (6) | 0.6731 (7) | 0.053 (2) | |
H13C | 0.5218 | 0.8526 | 0.6328 | 0.063* | |
H13D | 0.5130 | 0.8801 | 0.7312 | 0.063* | |
C14A | 0.4869 (4) | 0.9744 (8) | 0.6464 (10) | 0.093 (4) | |
H14D | 0.5125 | 1.0158 | 0.6463 | 0.140* | |
H14E | 0.4653 | 0.9992 | 0.6866 | 0.140* | |
H14F | 0.4745 | 0.9720 | 0.5885 | 0.140* | |
C15A | 0.5166 (2) | 0.6497 (5) | 0.7496 (7) | 0.048 (2) | |
H15C | 0.5289 | 0.6585 | 0.6914 | 0.058* | |
H15D | 0.5281 | 0.7001 | 0.7874 | 0.058* | |
C16A | 0.5286 (3) | 0.5570 (6) | 0.7831 (7) | 0.059 (3) | |
H16D | 0.5603 | 0.5520 | 0.7855 | 0.088* | |
H16E | 0.5171 | 0.5076 | 0.7454 | 0.088* | |
H16F | 0.5166 | 0.5493 | 0.8409 | 0.088* | |
C17A | 0.4567 (2) | 0.7682 (6) | 0.9181 (6) | 0.0434 (19) | |
H17C | 0.4763 | 0.7137 | 0.9272 | 0.052* | |
H17D | 0.4264 | 0.7461 | 0.9257 | 0.052* | |
C18A | 0.4664 (3) | 0.8432 (6) | 0.9813 (7) | 0.050 (2) | |
H18D | 0.4626 | 0.8182 | 1.0395 | 0.075* | |
H18E | 0.4467 | 0.8966 | 0.9725 | 0.075* | |
H18F | 0.4965 | 0.8645 | 0.9739 | 0.075* | |
C19A | 0.2479 (3) | 0.5477 (6) | 0.6486 (7) | 0.077 (3) | |
H19C | 0.2243 | 0.5496 | 0.6918 | 0.093* | 0.50 |
H19D | 0.2384 | 0.5820 | 0.5964 | 0.093* | 0.50 |
H19E | 0.2248 | 0.5660 | 0.6096 | 0.093* | 0.50 |
H19F | 0.2357 | 0.5481 | 0.7061 | 0.093* | 0.50 |
C20A | 0.2599 (3) | 0.4517 (6) | 0.6287 (9) | 0.087 (4) | |
H20D | 0.2342 | 0.4110 | 0.6321 | 0.130* | |
H20E | 0.2817 | 0.4299 | 0.6699 | 0.130* | |
H20F | 0.2720 | 0.4490 | 0.5705 | 0.130* | |
C21A | 0.2638 (3) | 0.6849 (8) | 0.8772 (5) | 0.068 (3) | |
H21C | 0.2775 | 0.7476 | 0.8852 | 0.081* | 0.50 |
H21D | 0.2826 | 0.6372 | 0.9053 | 0.081* | 0.50 |
H21E | 0.2830 | 0.7293 | 0.9057 | 0.081* | 0.50 |
H21F | 0.2768 | 0.6224 | 0.8800 | 0.081* | 0.50 |
C22A | 0.2216 (3) | 0.6848 (7) | 0.9185 (6) | 0.067 (2) | |
H22D | 0.2247 | 0.6652 | 0.9785 | 0.101* | |
H22E | 0.2023 | 0.6406 | 0.8885 | 0.101* | |
H22F | 0.2091 | 0.7486 | 0.9162 | 0.101* | |
C23A | 0.2462 (6) | 0.8383 (9) | 0.6577 (9) | 0.050 (4)* | 0.50 |
H23C | 0.2666 | 0.8840 | 0.6842 | 0.060* | 0.50 |
H23D | 0.2216 | 0.8278 | 0.6975 | 0.060* | 0.50 |
C23B | 0.2280 (4) | 0.7971 (9) | 0.6403 (9) | 0.049 (4)* | 0.50 |
H23E | 0.2070 | 0.8140 | 0.6858 | 0.059* | 0.50 |
H23F | 0.2192 | 0.7361 | 0.6143 | 0.059* | 0.50 |
C24A | 0.2303 (3) | 0.8742 (6) | 0.5724 (7) | 0.076 (3) | |
H24D | 0.2153 | 0.9347 | 0.5806 | 0.115* | 0.50 |
H24E | 0.2102 | 0.8281 | 0.5473 | 0.115* | 0.50 |
H24F | 0.2550 | 0.8833 | 0.5337 | 0.115* | 0.50 |
H24G | 0.2023 | 0.8818 | 0.5463 | 0.115* | 0.50 |
H24H | 0.2511 | 0.8567 | 0.5293 | 0.115* | 0.50 |
H24I | 0.2389 | 0.9328 | 0.5985 | 0.115* | 0.50 |
P3 | 0.39157 (7) | 0.72574 (13) | 0.21217 (14) | 0.0355 (4) | |
F1 | 0.36602 (16) | 0.8078 (4) | 0.2599 (4) | 0.0576 (16) | |
F2 | 0.36496 (19) | 0.7472 (6) | 0.1267 (5) | 0.079 (2) | |
F3 | 0.41680 (15) | 0.6437 (4) | 0.1636 (4) | 0.0556 (14) | |
F4 | 0.41860 (15) | 0.7056 (3) | 0.2975 (3) | 0.0506 (12) | |
F5 | 0.35538 (14) | 0.6523 (3) | 0.2418 (6) | 0.0685 (18) | |
F6 | 0.42756 (18) | 0.7991 (3) | 0.1839 (4) | 0.0609 (15) | |
P4 | 0.60029 (5) | 0.78284 (12) | −0.06173 (13) | 0.0265 (4) | |
F7 | 0.58061 (16) | 0.8604 (4) | 0.0002 (4) | 0.0638 (17) | |
F8 | 0.57075 (15) | 0.8221 (4) | −0.1379 (4) | 0.0642 (16) | |
F9 | 0.61997 (18) | 0.7056 (4) | −0.1265 (4) | 0.0575 (15) | |
F10 | 0.62998 (14) | 0.7446 (4) | 0.0139 (4) | 0.0555 (15) | |
F11 | 0.56293 (13) | 0.7092 (3) | −0.0359 (3) | 0.0411 (11) | |
F12 | 0.63835 (12) | 0.8546 (3) | −0.0910 (5) | 0.0432 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re1 | 0.02439 (10) | 0.02392 (13) | 0.01614 (15) | −0.00483 (8) | −0.00090 (10) | 0.00229 (14) |
P1 | 0.0277 (7) | 0.0359 (8) | 0.0196 (10) | −0.0086 (6) | 0.0044 (8) | 0.0047 (10) |
P2 | 0.0241 (6) | 0.0346 (8) | 0.0274 (10) | −0.0009 (6) | −0.0057 (7) | −0.0012 (8) |
C1 | 0.049 (4) | 0.035 (4) | 0.019 (4) | −0.008 (4) | −0.003 (4) | 0.000 (3) |
O1 | 0.074 (4) | 0.056 (4) | 0.033 (4) | −0.008 (3) | −0.011 (3) | 0.023 (3) |
C2 | 0.040 (4) | 0.038 (4) | 0.021 (5) | −0.007 (3) | 0.000 (3) | 0.008 (4) |
O2 | 0.080 (4) | 0.047 (3) | 0.030 (4) | −0.019 (3) | 0.012 (3) | −0.021 (3) |
N1 | 0.025 (3) | 0.019 (3) | 0.022 (4) | −0.0056 (19) | −0.001 (2) | 0.000 (2) |
N2 | 0.019 (2) | 0.021 (3) | 0.024 (3) | −0.0012 (19) | 0.004 (2) | 0.008 (2) |
O3 | 0.030 (2) | 0.053 (3) | 0.056 (4) | −0.0003 (19) | 0.009 (3) | 0.012 (4) |
O4 | 0.048 (3) | 0.043 (3) | 0.024 (3) | −0.015 (2) | 0.016 (2) | −0.001 (3) |
O5 | 0.029 (3) | 0.084 (5) | 0.044 (4) | −0.028 (3) | 0.009 (3) | −0.022 (4) |
O6 | 0.037 (2) | 0.032 (2) | 0.034 (3) | −0.0072 (19) | −0.013 (2) | −0.004 (2) |
O7 | 0.026 (2) | 0.091 (4) | 0.022 (3) | −0.016 (2) | 0.003 (2) | −0.005 (3) |
O8 | 0.043 (3) | 0.040 (3) | 0.103 (5) | 0.010 (2) | −0.017 (4) | −0.017 (3) |
C3 | 0.035 (3) | 0.026 (3) | 0.028 (4) | −0.002 (3) | −0.004 (3) | 0.001 (3) |
C4 | 0.036 (3) | 0.037 (4) | 0.043 (5) | −0.002 (3) | −0.005 (3) | 0.001 (4) |
C5 | 0.045 (4) | 0.042 (4) | 0.042 (6) | 0.002 (3) | 0.001 (3) | −0.018 (4) |
C6 | 0.049 (4) | 0.045 (4) | 0.022 (4) | −0.007 (3) | −0.004 (3) | 0.003 (3) |
C7 | 0.026 (3) | 0.019 (3) | 0.033 (5) | −0.005 (2) | −0.003 (3) | −0.001 (3) |
C8 | 0.020 (3) | 0.033 (3) | 0.014 (3) | −0.002 (2) | 0.002 (2) | 0.005 (3) |
C9 | 0.040 (3) | 0.045 (4) | 0.025 (4) | 0.007 (3) | 0.003 (3) | 0.010 (3) |
C10 | 0.051 (4) | 0.048 (4) | 0.034 (4) | 0.008 (3) | 0.006 (4) | 0.026 (4) |
C11 | 0.046 (4) | 0.027 (3) | 0.054 (6) | 0.008 (3) | 0.009 (4) | 0.019 (4) |
C12 | 0.032 (3) | 0.028 (3) | 0.029 (4) | 0.004 (3) | 0.008 (3) | 0.005 (3) |
C13 | 0.030 (3) | 0.071 (6) | 0.078 (7) | 0.006 (3) | 0.008 (5) | −0.005 (7) |
C14 | 0.041 (4) | 0.092 (8) | 0.105 (11) | 0.020 (5) | −0.001 (6) | −0.024 (8) |
C15 | 0.070 (5) | 0.059 (5) | 0.033 (5) | −0.017 (4) | 0.010 (5) | 0.009 (5) |
C16 | 0.065 (5) | 0.091 (7) | 0.027 (5) | 0.005 (5) | −0.005 (4) | 0.014 (5) |
C17 | 0.039 (4) | 0.085 (7) | 0.049 (6) | −0.038 (4) | 0.004 (4) | −0.014 (5) |
C18 | 0.062 (6) | 0.083 (8) | 0.065 (8) | −0.027 (5) | 0.014 (5) | −0.021 (6) |
C19 | 0.057 (5) | 0.032 (4) | 0.096 (8) | 0.001 (3) | −0.008 (5) | 0.003 (4) |
C20 | 0.099 (8) | 0.069 (6) | 0.129 (12) | −0.035 (6) | 0.001 (8) | −0.025 (7) |
C21 | 0.043 (5) | 0.157 (10) | 0.045 (6) | −0.026 (5) | 0.011 (4) | −0.019 (7) |
C22 | 0.072 (6) | 0.127 (9) | 0.043 (5) | −0.021 (6) | 0.018 (5) | −0.009 (6) |
C23 | 0.080 (6) | 0.055 (5) | 0.097 (9) | 0.017 (5) | −0.030 (6) | 0.005 (6) |
C24 | 0.095 (7) | 0.065 (6) | 0.078 (8) | 0.021 (5) | −0.019 (6) | 0.013 (5) |
Re1A | 0.02380 (10) | 0.02149 (12) | 0.01588 (14) | −0.00457 (8) | −0.00004 (10) | 0.00149 (14) |
P1A | 0.0257 (6) | 0.0292 (8) | 0.0225 (11) | −0.0063 (5) | −0.0015 (8) | −0.0004 (9) |
P2A | 0.0210 (6) | 0.0335 (8) | 0.0232 (10) | −0.0037 (6) | 0.0031 (6) | 0.0020 (7) |
C1A | 0.026 (3) | 0.024 (3) | 0.036 (6) | −0.008 (2) | −0.001 (3) | 0.011 (4) |
O1A | 0.074 (4) | 0.042 (3) | 0.042 (5) | −0.014 (3) | −0.012 (3) | 0.020 (3) |
C2A | 0.027 (3) | 0.032 (4) | 0.028 (5) | −0.005 (3) | 0.009 (3) | 0.004 (3) |
O2A | 0.061 (3) | 0.034 (3) | 0.027 (3) | −0.001 (2) | 0.014 (3) | −0.011 (2) |
N1A | 0.019 (3) | 0.025 (3) | 0.023 (4) | −0.0025 (18) | 0.002 (2) | 0.001 (3) |
N2A | 0.021 (2) | 0.025 (3) | 0.017 (3) | −0.004 (2) | −0.001 (2) | −0.002 (2) |
O3A | 0.042 (3) | 0.060 (4) | 0.017 (3) | −0.026 (2) | −0.001 (2) | 0.002 (3) |
O4A | 0.029 (2) | 0.047 (3) | 0.051 (4) | 0.0024 (18) | −0.011 (3) | −0.018 (3) |
O5A | 0.035 (3) | 0.048 (3) | 0.018 (3) | −0.017 (2) | −0.004 (2) | 0.000 (3) |
C3A | 0.028 (3) | 0.022 (3) | 0.030 (4) | 0.001 (2) | −0.003 (3) | −0.003 (3) |
C4A | 0.035 (3) | 0.029 (3) | 0.041 (5) | 0.002 (3) | 0.000 (3) | 0.015 (4) |
C5A | 0.039 (4) | 0.038 (4) | 0.035 (4) | 0.000 (3) | 0.003 (3) | 0.019 (4) |
C6A | 0.036 (3) | 0.033 (3) | 0.016 (3) | −0.007 (3) | 0.003 (3) | 0.005 (3) |
C7A | 0.021 (2) | 0.028 (3) | 0.011 (3) | −0.002 (2) | −0.002 (2) | −0.002 (3) |
C8A | 0.017 (3) | 0.028 (3) | 0.021 (3) | −0.003 (2) | −0.003 (2) | 0.000 (3) |
C9A | 0.030 (3) | 0.038 (3) | 0.017 (3) | 0.003 (3) | −0.001 (3) | 0.003 (3) |
C10A | 0.030 (3) | 0.045 (4) | 0.034 (4) | 0.007 (3) | −0.002 (3) | −0.014 (3) |
C11A | 0.036 (3) | 0.028 (3) | 0.041 (5) | −0.003 (3) | 0.001 (3) | −0.009 (3) |
C12A | 0.037 (3) | 0.019 (3) | 0.030 (4) | −0.002 (2) | −0.002 (3) | 0.000 (3) |
C13A | 0.033 (4) | 0.070 (6) | 0.054 (7) | −0.026 (4) | −0.002 (4) | 0.009 (5) |
C14A | 0.093 (8) | 0.084 (8) | 0.102 (11) | −0.045 (6) | −0.034 (8) | 0.039 (8) |
C15A | 0.028 (3) | 0.060 (5) | 0.057 (6) | 0.008 (3) | −0.012 (4) | −0.012 (5) |
C16A | 0.047 (4) | 0.064 (6) | 0.066 (8) | 0.011 (4) | 0.002 (5) | 0.005 (5) |
C17A | 0.050 (4) | 0.061 (5) | 0.019 (4) | −0.020 (3) | −0.013 (4) | 0.027 (4) |
C18A | 0.052 (5) | 0.065 (5) | 0.034 (5) | 0.003 (4) | 0.003 (4) | −0.015 (4) |
C19A | 0.062 (5) | 0.071 (5) | 0.099 (9) | −0.027 (5) | 0.013 (6) | −0.035 (6) |
C20A | 0.076 (6) | 0.065 (6) | 0.119 (11) | −0.006 (5) | −0.019 (7) | −0.021 (6) |
C21A | 0.047 (4) | 0.127 (8) | 0.029 (4) | −0.027 (5) | 0.009 (4) | −0.007 (5) |
C22A | 0.062 (5) | 0.102 (7) | 0.038 (5) | −0.021 (5) | 0.022 (5) | −0.006 (5) |
C24A | 0.082 (6) | 0.068 (5) | 0.079 (8) | 0.025 (5) | −0.019 (6) | 0.010 (6) |
P3 | 0.0550 (10) | 0.0280 (9) | 0.0233 (11) | 0.0031 (8) | 0.0000 (8) | −0.0006 (8) |
F1 | 0.083 (4) | 0.040 (2) | 0.049 (4) | 0.016 (2) | −0.005 (3) | −0.012 (2) |
F2 | 0.094 (5) | 0.102 (5) | 0.043 (4) | 0.034 (3) | −0.025 (3) | −0.012 (4) |
F3 | 0.058 (3) | 0.049 (3) | 0.059 (4) | 0.006 (2) | 0.008 (3) | −0.019 (3) |
F4 | 0.068 (3) | 0.056 (3) | 0.029 (2) | 0.006 (2) | −0.004 (2) | 0.011 (2) |
F5 | 0.052 (2) | 0.049 (3) | 0.104 (6) | −0.013 (2) | 0.015 (4) | 0.001 (4) |
F6 | 0.092 (4) | 0.041 (3) | 0.049 (4) | −0.019 (2) | 0.011 (3) | 0.013 (2) |
P4 | 0.0294 (7) | 0.0274 (8) | 0.0227 (10) | −0.0061 (6) | −0.0014 (6) | −0.0011 (7) |
F7 | 0.056 (3) | 0.053 (3) | 0.082 (5) | −0.006 (2) | 0.012 (3) | −0.041 (3) |
F8 | 0.056 (3) | 0.076 (3) | 0.061 (4) | −0.010 (2) | −0.027 (3) | 0.030 (3) |
F9 | 0.065 (3) | 0.058 (3) | 0.049 (3) | −0.007 (3) | 0.022 (3) | −0.025 (3) |
F10 | 0.046 (3) | 0.075 (3) | 0.046 (4) | −0.014 (2) | −0.017 (2) | 0.028 (3) |
F11 | 0.036 (2) | 0.047 (2) | 0.040 (3) | −0.0151 (17) | 0.0016 (19) | −0.004 (2) |
F12 | 0.0415 (19) | 0.042 (2) | 0.046 (3) | −0.0165 (17) | 0.002 (2) | −0.002 (3) |
Re1—C1 | 1.896 (9) | P4—F7 | 1.581 (5) |
Re1—C2 | 1.931 (10) | P4—F8 | 1.595 (5) |
Re1—N1 | 2.162 (8) | P4—F9 | 1.605 (5) |
Re1—N2 | 2.176 (6) | P4—F10 | 1.587 (6) |
Re1—P1 | 2.3730 (15) | P4—F11 | 1.603 (4) |
Re1—P2 | 2.3724 (16) | P4—F12 | 1.616 (4) |
P1—O3 | 1.575 (5) | C3—H3A | 0.95 |
P1—O4 | 1.588 (6) | C4—H4A | 0.95 |
P1—O5 | 1.585 (7) | C5—H5A | 0.95 |
P2—O6 | 1.594 (5) | C6—H6A | 0.95 |
P2—O7 | 1.604 (5) | C9—H9A | 0.95 |
P2—O8 | 1.591 (5) | C10—H10A | 0.95 |
C1—O1 | 1.178 (10) | C11—H11A | 0.95 |
C2—O2 | 1.147 (11) | C12—H12A | 0.95 |
N1—C7 | 1.346 (13) | C13—H13A | 0.99 |
N1—C3 | 1.357 (10) | C13—H13B | 0.99 |
N2—C8 | 1.344 (9) | C14—H14A | 0.98 |
N2—C12 | 1.346 (9) | C14—H14B | 0.98 |
O3—C13 | 1.466 (7) | C14—H14C | 0.98 |
O4—C15 | 1.470 (13) | C15—H15A | 0.99 |
O5—C17 | 1.454 (8) | C15—H15B | 0.99 |
O6—C19 | 1.419 (8) | C16—H16A | 0.98 |
O7—C21 | 1.458 (9) | C16—H16B | 0.98 |
O8—C23 | 1.405 (10) | C16—H16C | 0.98 |
C3—C4 | 1.368 (12) | C17—H17A | 0.99 |
C4—C5 | 1.381 (14) | C17—H17B | 0.99 |
C5—C6 | 1.370 (12) | C18—H18A | 0.98 |
C6—C7 | 1.366 (13) | C18—H18B | 0.98 |
C7—C8 | 1.504 (10) | C18—H18C | 0.98 |
C8—C9 | 1.400 (10) | C19—H19A | 0.99 |
C9—C10 | 1.390 (11) | C19—H19B | 0.99 |
C10—C11 | 1.377 (13) | C20—H20A | 0.98 |
C11—C12 | 1.392 (11) | C20—H20B | 0.98 |
C13—C14 | 1.516 (13) | C20—H20C | 0.98 |
C15—C16 | 1.474 (13) | C21—H21A | 0.99 |
C17—C18 | 1.493 (13) | C21—H21B | 0.99 |
C19—C20 | 1.459 (11) | C22—H22A | 0.98 |
C21—C22 | 1.417 (13) | C22—H22B | 0.98 |
C23—C24 | 1.431 (11) | C22—H22C | 0.98 |
Re1A—C1A | 1.886 (9) | C23—H23A | 0.99 |
Re1A—C2A | 1.915 (9) | C23—H23B | 0.99 |
Re1A—N1A | 2.174 (8) | C24—H24A | 0.98 |
Re1A—N2A | 2.184 (6) | C24—H24B | 0.98 |
Re1A—P1A | 2.3817 (15) | C24—H24C | 0.98 |
Re1A—P2A | 2.3664 (16) | C3A—H3AA | 0.95 |
P1A—O3A | 1.587 (6) | C4A—H4AA | 0.95 |
P1A—O4A | 1.589 (5) | C5A—H5AA | 0.95 |
P1A—O5A | 1.602 (6) | C6A—H6AA | 0.95 |
P2A—O6B | 1.557 (9) | C9A—H9AA | 0.95 |
P2A—O7A | 1.545 (10) | C10A—H10B | 0.95 |
P2A—O8A | 1.586 (10) | C11A—H11B | 0.95 |
P2A—O8B | 1.598 (11) | C12A—H12B | 0.95 |
P2A—O7B | 1.604 (8) | C13A—H13C | 0.99 |
P2A—O6A | 1.623 (7) | C13A—H13D | 0.99 |
C1A—O1A | 1.172 (11) | C14A—H14D | 0.98 |
C2A—O2A | 1.151 (10) | C14A—H14E | 0.98 |
N1A—C7A | 1.346 (11) | C14A—H14F | 0.98 |
N1A—C3A | 1.354 (10) | C15A—H15C | 0.99 |
N2A—C12A | 1.351 (8) | C15A—H15D | 0.99 |
N2A—C8A | 1.356 (9) | C16A—H16D | 0.98 |
O3A—C13A | 1.462 (8) | C16A—H16E | 0.98 |
O4A—C15A | 1.468 (7) | C16A—H16F | 0.98 |
O5A—C17A | 1.450 (10) | C17A—H17C | 0.99 |
O6A—C19A | 1.457 (8) | C17A—H17D | 0.99 |
O6B—C19A | 1.467 (8) | C18A—H18D | 0.98 |
O7A—C21A | 1.448 (8) | C18A—H18E | 0.98 |
O7B—C21A | 1.447 (8) | C18A—H18F | 0.98 |
O8A—C23A | 1.458 (9) | C19A—H19C | 0.99 |
O8B—C23B | 1.467 (8) | C19A—H19D | 0.99 |
C3A—C4A | 1.376 (12) | C19A—H19E | 0.97 |
C4A—C5A | 1.360 (14) | C19A—H19F | 0.97 |
C5A—C6A | 1.382 (11) | C20A—H20D | 0.98 |
C6A—C7A | 1.413 (10) | C20A—H20E | 0.98 |
C7A—C8A | 1.461 (9) | C20A—H20F | 0.98 |
C8A—C9A | 1.378 (9) | C21A—H21C | 0.99 |
C9A—C10A | 1.368 (9) | C21A—H21D | 0.99 |
C10A—C11A | 1.369 (12) | C21A—H21E | 0.97 |
C11A—C12A | 1.364 (11) | C21A—H21F | 0.97 |
C13A—C14A | 1.479 (13) | C22A—H22D | 0.98 |
C15A—C16A | 1.458 (11) | C22A—H22E | 0.98 |
C17A—C18A | 1.478 (13) | C22A—H22F | 0.98 |
C19A—C20A | 1.440 (11) | C23A—H23C | 0.99 |
C21A—C22A | 1.453 (10) | C23A—H23D | 0.99 |
C23A—C24A | 1.506 (15) | C23B—H23E | 0.99 |
C23B—C24A | 1.521 (14) | C23B—H23F | 0.99 |
P3—F1 | 1.586 (5) | C24A—H24D | 0.98 |
P3—F2 | 1.592 (7) | C24A—H24E | 0.98 |
P3—F3 | 1.588 (5) | C24A—H24F | 0.98 |
P3—F4 | 1.594 (5) | C24A—H24G | 0.96 |
P3—F5 | 1.592 (5) | C24A—H24H | 0.96 |
P3—F6 | 1.581 (5) | C24A—H24I | 0.96 |
C1—Re1—C2 | 88.9 (4) | C17—C18—H18B | 109.5 |
C1—Re1—N1 | 97.7 (3) | H18A—C18—H18B | 109.5 |
C2—Re1—N1 | 173.2 (3) | C17—C18—H18C | 109.5 |
C1—Re1—N2 | 171.7 (3) | H18A—C18—H18C | 109.5 |
C2—Re1—N2 | 99.4 (3) | H18B—C18—H18C | 109.5 |
N1—Re1—N2 | 74.0 (3) | O6—C19—H19A | 109.1 |
C1—Re1—P2 | 88.3 (3) | C20—C19—H19A | 109.1 |
C2—Re1—P2 | 95.2 (2) | O6—C19—H19B | 109.1 |
N1—Re1—P2 | 86.71 (14) | C20—C19—H19B | 109.1 |
N2—Re1—P2 | 90.11 (15) | H19A—C19—H19B | 107.8 |
C1—Re1—P1 | 90.9 (3) | C19—C20—H20A | 109.5 |
C2—Re1—P1 | 89.9 (2) | C19—C20—H20B | 109.5 |
N1—Re1—P1 | 88.37 (14) | H20A—C20—H20B | 109.5 |
N2—Re1—P1 | 89.89 (15) | C19—C20—H20C | 109.5 |
P2—Re1—P1 | 174.88 (7) | H20A—C20—H20C | 109.5 |
O3—P1—O5 | 107.0 (4) | H20B—C20—H20C | 109.5 |
O3—P1—O4 | 105.7 (3) | C22—C21—H21A | 109.4 |
O5—P1—O4 | 99.0 (3) | O7—C21—H21A | 109.5 |
O3—P1—Re1 | 111.99 (18) | C22—C21—H21B | 109.5 |
O5—P1—Re1 | 112.0 (2) | O7—C21—H21B | 109.5 |
O4—P1—Re1 | 119.9 (2) | H21A—C21—H21B | 108.0 |
O8—P2—O6 | 100.3 (3) | C21—C22—H22A | 109.5 |
O8—P2—O7 | 104.8 (4) | C21—C22—H22B | 109.5 |
O6—P2—O7 | 105.9 (3) | H22A—C22—H22B | 109.5 |
O8—P2—Re1 | 111.6 (2) | C21—C22—H22C | 109.5 |
O6—P2—Re1 | 121.9 (2) | H22A—C22—H22C | 109.5 |
O7—P2—Re1 | 110.72 (18) | H22B—C22—H22C | 109.5 |
O1—C1—Re1 | 178.8 (9) | O8—C23—H23A | 109.9 |
O2—C2—Re1 | 178.2 (8) | C24—C23—H23A | 110.0 |
C7—N1—C3 | 116.8 (8) | O8—C23—H23B | 110.0 |
C7—N1—Re1 | 119.3 (5) | C24—C23—H23B | 110.0 |
C3—N1—Re1 | 123.6 (6) | H23A—C23—H23B | 108.4 |
C8—N2—C12 | 118.3 (7) | C23—C24—H24A | 109.5 |
C8—N2—Re1 | 117.9 (4) | C23—C24—H24B | 109.4 |
C12—N2—Re1 | 123.8 (6) | H24A—C24—H24B | 109.5 |
C13—O3—P1 | 122.7 (5) | C23—C24—H24C | 109.5 |
C15—O4—P1 | 119.2 (5) | H24A—C24—H24C | 109.5 |
C17—O5—P1 | 128.3 (6) | H24B—C24—H24C | 109.5 |
C19—O6—P2 | 120.1 (5) | N1A—C3A—H3AA | 118.7 |
C21—O7—P2 | 123.0 (5) | C4A—C3A—H3AA | 118.7 |
C23—O8—P2 | 128.0 (5) | C5A—C4A—H4AA | 120.8 |
N1—C3—C4 | 122.5 (9) | C3A—C4A—H4AA | 120.9 |
C3—C4—C5 | 119.6 (8) | C4A—C5A—H5AA | 119.6 |
C6—C5—C4 | 118.1 (9) | C6A—C5A—H5AA | 119.6 |
C7—C6—C5 | 119.9 (9) | C5A—C6A—H6AA | 120.8 |
N1—C7—C6 | 123.0 (7) | C7A—C6A—H6AA | 120.8 |
N1—C7—C8 | 113.4 (7) | C10A—C9A—H9AA | 119.6 |
C6—C7—C8 | 123.6 (8) | C8A—C9A—H9AA | 119.6 |
N2—C8—C9 | 122.6 (6) | C9A—C10A—H10B | 120.5 |
N2—C8—C7 | 115.2 (6) | C11A—C10A—H10B | 120.4 |
C9—C8—C7 | 122.2 (7) | C12A—C11A—H11B | 120.6 |
C10—C9—C8 | 117.7 (7) | C10A—C11A—H11B | 120.6 |
C11—C10—C9 | 120.5 (7) | N2A—C12A—H12B | 119.0 |
C10—C11—C12 | 118.1 (7) | C11A—C12A—H12B | 119.0 |
N2—C12—C11 | 122.9 (8) | O3A—C13A—H13C | 110.0 |
O3—C13—C14 | 108.0 (7) | C14A—C13A—H13C | 110.0 |
O4—C15—C16 | 108.9 (7) | O3A—C13A—H13D | 110.0 |
O5—C17—C18 | 109.1 (7) | C14A—C13A—H13D | 110.0 |
O6—C19—C20 | 111.3 (7) | H13C—C13A—H13D | 108.4 |
C22—C21—O7 | 110.9 (8) | C13A—C14A—H14D | 109.5 |
O8—C23—C24 | 109.8 (8) | C13A—C14A—H14E | 109.5 |
C1A—Re1A—C2A | 88.8 (4) | H14D—C14A—H14E | 109.5 |
C1A—Re1A—N1A | 172.4 (4) | C13A—C14A—H14F | 109.5 |
C2A—Re1A—N1A | 98.8 (3) | H14D—C14A—H14F | 109.5 |
C1A—Re1A—N2A | 98.1 (3) | H14E—C14A—H14F | 109.5 |
C2A—Re1A—N2A | 173.1 (3) | C16A—C15A—H15C | 110.1 |
N1A—Re1A—N2A | 74.3 (3) | O4A—C15A—H15C | 110.1 |
C1A—Re1A—P2A | 92.3 (2) | C16A—C15A—H15D | 110.1 |
C2A—Re1A—P2A | 91.9 (2) | O4A—C15A—H15D | 110.1 |
N1A—Re1A—P2A | 88.41 (13) | H15C—C15A—H15D | 108.4 |
N2A—Re1A—P2A | 87.28 (15) | C15A—C16A—H16D | 109.5 |
C1A—Re1A—P1A | 90.8 (2) | C15A—C16A—H16E | 109.5 |
C2A—Re1A—P1A | 92.2 (2) | H16D—C16A—H16E | 109.5 |
N1A—Re1A—P1A | 88.07 (13) | C15A—C16A—H16F | 109.5 |
N2A—Re1A—P1A | 88.36 (15) | H16D—C16A—H16F | 109.5 |
P2A—Re1A—P1A | 175.01 (8) | H16E—C16A—H16F | 109.5 |
O3A—P1A—O4A | 107.6 (4) | O5A—C17A—H17C | 109.8 |
O3A—P1A—O5A | 101.4 (3) | C18A—C17A—H17C | 109.9 |
O4A—P1A—O5A | 103.9 (3) | O5A—C17A—H17D | 109.9 |
O3A—P1A—Re1A | 112.9 (2) | C18A—C17A—H17D | 109.8 |
O4A—P1A—Re1A | 110.51 (17) | H17C—C17A—H17D | 108.3 |
O5A—P1A—Re1A | 119.4 (2) | C17A—C18A—H18D | 109.5 |
O7A—P2A—O8A | 112.4 (5) | C17A—C18A—H18E | 109.5 |
O6B—P2A—O8B | 103.0 (6) | H18D—C18A—H18E | 109.5 |
O6B—P2A—O7B | 116.9 (4) | C17A—C18A—H18F | 109.4 |
O8B—P2A—O7B | 83.4 (5) | H18D—C18A—H18F | 109.5 |
O7A—P2A—O6A | 83.3 (5) | H18E—C18A—H18F | 109.5 |
O8A—P2A—O6A | 100.4 (5) | C20A—C19A—H19C | 111.0 |
O7A—P2A—Re1A | 123.0 (3) | O6A—C19A—H19C | 111.0 |
O6B—P2A—Re1A | 116.1 (3) | O6B—C19A—H19C | 121.3 |
O8A—P2A—Re1A | 119.7 (3) | C20A—C19A—H19D | 111.0 |
O8B—P2A—Re1A | 107.4 (4) | O6A—C19A—H19D | 111.0 |
O7B—P2A—Re1A | 121.4 (3) | H19C—C19A—H19D | 109.0 |
O6A—P2A—Re1A | 107.4 (2) | C20A—C19A—H19E | 107.3 |
O1A—C1A—Re1A | 179.5 (8) | O6B—C19A—H19E | 107.8 |
O2A—C2A—Re1A | 179.1 (8) | C20A—C19A—H19F | 107.4 |
C7A—N1A—C3A | 119.0 (8) | O6B—C19A—H19F | 107.5 |
C7A—N1A—Re1A | 117.3 (5) | H19E—C19A—H19F | 107.1 |
C3A—N1A—Re1A | 123.8 (6) | C19A—C20A—H20D | 109.5 |
C12A—N2A—C8A | 118.8 (6) | C19A—C20A—H20E | 109.5 |
C12A—N2A—Re1A | 124.0 (5) | H20D—C20A—H20E | 109.5 |
C8A—N2A—Re1A | 117.2 (4) | C19A—C20A—H20F | 109.5 |
C13A—O3A—P1A | 129.1 (6) | H20D—C20A—H20F | 109.5 |
C15A—O4A—P1A | 122.8 (4) | H20E—C20A—H20F | 109.5 |
C17A—O5A—P1A | 122.5 (5) | O7A—C21A—H21C | 109.0 |
C19A—O6A—P2A | 123.6 (6) | C22A—C21A—H21C | 109.0 |
C19A—O6B—P2A | 127.8 (8) | O7A—C21A—H21D | 108.9 |
C21A—O7A—P2A | 128.1 (7) | C22A—C21A—H21D | 108.9 |
C21A—O7B—P2A | 123.8 (6) | H21C—C21A—H21D | 107.8 |
C23A—O8A—P2A | 118.4 (8) | O7B—C21A—H21E | 110.1 |
N1A—C3A—C4A | 122.9 (8) | C22A—C21A—H21E | 109.9 |
C5A—C4A—C3A | 118.3 (7) | O7B—C21A—H21F | 110.6 |
C4A—C5A—C6A | 120.8 (8) | C22A—C21A—H21F | 110.4 |
C5A—C6A—C7A | 118.5 (8) | H21E—C21A—H21F | 108.5 |
N1A—C7A—C6A | 120.5 (6) | C21A—C22A—H22D | 109.5 |
N1A—C7A—C8A | 116.2 (7) | C21A—C22A—H22E | 109.5 |
C6A—C7A—C8A | 123.2 (7) | H22D—C22A—H22E | 109.5 |
N2A—C8A—C9A | 120.2 (6) | C21A—C22A—H22F | 109.4 |
N2A—C8A—C7A | 115.1 (6) | H22D—C22A—H22F | 109.5 |
C9A—C8A—C7A | 124.7 (6) | H22E—C22A—H22F | 109.5 |
C10A—C9A—C8A | 120.6 (7) | O8A—C23A—H23C | 110.6 |
C9A—C10A—C11A | 118.9 (7) | C24A—C23A—H23C | 110.6 |
C12A—C11A—C10A | 119.4 (7) | O8A—C23A—H23D | 110.6 |
N2A—C12A—C11A | 122.2 (7) | C24A—C23A—H23D | 110.6 |
O3A—C13A—C14A | 109.0 (7) | H23C—C23A—H23D | 108.7 |
C16A—C15A—O4A | 108.3 (7) | O8B—C23B—H23E | 110.7 |
O5A—C17A—C18A | 109.6 (7) | C24A—C23B—H23E | 110.7 |
C20A—C19A—O6A | 102.9 (8) | O8B—C23B—H23F | 110.7 |
O7B—C21A—C22A | 107.4 (8) | C24A—C23B—H23F | 110.7 |
O7A—C21A—C22A | 112.6 (8) | H23E—C23B—H23F | 108.8 |
O8A—C23A—C24A | 105.2 (9) | C23A—C24A—H24D | 109.5 |
N1—C3—H3A | 118.5 | C23A—C24A—H24E | 109.5 |
C4—C3—H3A | 118.5 | H24D—C24A—H24E | 109.5 |
C3—C4—H4A | 120.3 | C23A—C24A—H24F | 109.4 |
C5—C4—H4A | 120.3 | H24D—C24A—H24F | 109.5 |
C6—C5—H5A | 121.0 | H24E—C24A—H24F | 109.5 |
C4—C5—H5A | 121.0 | C23B—C24A—H24G | 109.6 |
C7—C6—H6A | 119.6 | C23B—C24A—H24H | 109.1 |
C5—C6—H6A | 119.6 | H24D—C24A—H24H | 129.4 |
C10—C9—H9A | 120.9 | H24G—C24A—H24H | 109.5 |
C8—C9—H9A | 120.9 | C23B—C24A—H24I | 109.7 |
C9—C10—H10A | 119.8 | H24G—C24A—H24I | 109.5 |
C10—C11—H11A | 120.9 | H24H—C24A—H24I | 109.5 |
C12—C11—H11A | 120.9 | F6—P3—F1 | 90.0 (3) |
N2—C12—H12A | 118.6 | F6—P3—F3 | 90.1 (3) |
C11—C12—H12A | 118.6 | F1—P3—F3 | 179.4 (3) |
O3—C13—H13A | 110.0 | F6—P3—F2 | 90.2 (4) |
C14—C13—H13A | 110.0 | F1—P3—F2 | 89.8 (4) |
O3—C13—H13B | 110.0 | F3—P3—F2 | 89.6 (3) |
C14—C13—H13B | 110.0 | F6—P3—F5 | 179.3 (4) |
H13A—C13—H13B | 108.4 | F1—P3—F5 | 89.6 (3) |
C13—C14—H14A | 109.5 | F3—P3—F5 | 90.3 (3) |
C13—C14—H14B | 109.5 | F2—P3—F5 | 90.3 (4) |
H14A—C14—H14B | 109.5 | F6—P3—F4 | 89.0 (3) |
C13—C14—H14C | 109.5 | F1—P3—F4 | 90.0 (3) |
H14A—C14—H14C | 109.5 | F3—P3—F4 | 90.6 (3) |
H14B—C14—H14C | 109.5 | F2—P3—F4 | 179.2 (4) |
O4—C15—H15A | 110.1 | F5—P3—F4 | 90.5 (4) |
C16—C15—H15A | 110.2 | F7—P4—F10 | 90.3 (4) |
O4—C15—H15B | 110.1 | F7—P4—F8 | 89.6 (3) |
C16—C15—H15B | 110.1 | F10—P4—F8 | 179.5 (3) |
H15A—C15—H15B | 108.4 | F7—P4—F11 | 91.2 (3) |
C15—C16—H16A | 109.5 | F10—P4—F11 | 90.4 (3) |
C15—C16—H16B | 109.5 | F8—P4—F11 | 90.1 (3) |
H16A—C16—H16B | 109.5 | F7—P4—F9 | 178.6 (4) |
C15—C16—H16C | 109.4 | F10—P4—F9 | 91.0 (4) |
H16A—C16—H16C | 109.5 | F8—P4—F9 | 89.1 (3) |
H16B—C16—H16C | 109.5 | F11—P4—F9 | 89.3 (3) |
O5—C17—H17A | 109.9 | F7—P4—F12 | 90.9 (3) |
C18—C17—H17A | 109.9 | F10—P4—F12 | 90.3 (3) |
O5—C17—H17B | 109.8 | F8—P4—F12 | 89.2 (3) |
C18—C17—H17B | 109.9 | F11—P4—F12 | 177.8 (3) |
H17A—C17—H17B | 108.3 | F9—P4—F12 | 88.6 (3) |
C17—C18—H18A | 109.5 |
Acknowledgements
We thank the Overseas Research Students Awards Scheme for an ORS award to MKK, and EPSRC (UK) for the award of a diffractometer.
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