Azido­[1,1'-bis­(di­phenyl­phosphino)­ferrocene](penta­methyl­cyclo­penta­dienyl)­rhodium(III) hexa­fluoro­phosphate

In the title compound, azido-2[kappa]N-bis­[[mu]-(1[eta]⁵:2[kappa]P)-di­phenyl­phosphino­cyclo­penta­dienyl][2([eta]⁵)-penta­methyl­cyclo­penta­di­enyl]­iron(III)­rhodium(III) hexa­fluoro­phosphate, [{Rh(C₁₀H₁₅)(N₃)}{Fe([mu]-C₁₇H₁₄P)₂}]PF₆ or [FeRh(C₁₀H₁₅)([mu]-C₁₇H₁₄P)₂(N₃)]PF₆, the coordination sphere of Rh^III can be described as pseudo-tetrahedral, composed of two P atoms from a 1,1'-bis­(di­phenyl­phosphino)­ferrocene (dppf) ligand, an azido N atom and the centroid of the ring of a C₅Me₅ (Cp*) ligand. The two cyclo­penta­dienyl rings in the dppf moiety adopt an eclipsed conformation. The Rh...Fe distance is 4.340 (2) Å.

S1. Comment

Various redox-active ligands are employed to control the reactivities of transition-metal complexes (Gan & Hor, 1995). The dppf ligand [1,1'-bis(diphenylphosphino)ferrocene, Fe(C₅H₄PPh₂)₂] and its derivatives are well known redox-active ligands, and their complexes usually exhibit a ferrocene-based oxidation process, together with additional redox processes at other metal centres. Recently, an interesting Rh–dppf chloro complex, [Cp*RhCl(dppf)]PF₆, was reported (Cp* is C₅Me₅), which was prepared by treating a chloro-bridged Rh^III dimer, [Cp*RhCl₂]₂, with dppf and NaPF₆ (Ma & Yamamoto, 1999). In order to compare structural features and to examine the redox properties of the Rh-dppf azido complex with respect to its chloro analogue, we have prepared the title compound, (I), and present its structure here. \sch

The coordination sphere of the Rh metal in (I) can be described as pseudo-tetrahedral. The two Cp (cyclopentadienyl) rings of the dppf ligand are not perfectly parallel, but are twisted from each other with a dihedral angle of 3.4 (1)°. The P1—C11···C16—P2 pseudo-torsion angle is 3.0 (4)°, indicating that the two Cp rings adopt an eclipsed conformation. For comparison, the ideal torsion angle for a gauche (or staggered) conformation is 36°. Both Fe—Cg (Cg is the centroid of a Cp ring) distances are 1.633 Å, and the Cg1—Fe—Cg2 angle (Cg1 is the centroid of the C11–C15 ring and Cg2 is the centroid of the C16–C20 ring) is 177.45°. The Cg*···Rh1—P1, Cg*···Rh1—P2 and Cg*···Rh1—N1 angles (Cg* is the centroid of the C1–C5 ring) are 125.45, 127.01 and 126.84°, respectively. The P1···Fe···P2 bite angle is 60.68 (5)°, and the P1···P2 distance is 3.526 (3) Å. These bonding parameters within a ferrocene moiety are consistent with those found in the chloro analogue, [Cp*RhCl(dppf)]PF₆ (Ma & Yamamoto, 1999).

The Rh—N1—N2 bond angle of 127.6 (7)° in (I) agrees well with those found in six-coordinate Rh^III azido complexes (Seok et al., 2002). Atom N3 in the azido ligand has a large displacement ellipsoid, probably due to its terminal position. The Rh—N bond length of 2.111 (7) Å indicates an Rh—N single bond (Davis et al., 1969; Lee & Lee, 1999). The Rh···Fe distance is 4.340 (2) Å, which clearly rules out a direct bonding interaction between the two metal atoms.

S2. Experimental

A solution of [Cp*RhCl(dppf)]PF₆ (100 mg, 0.12 mmol) and AgNO₃ (62 mg, 0.36 mmol) in a mixed solvent of dichloromethane and acetone (1:1, 30 ml) was stirred for 3 h at room temperature, and the solvent was removed under vacuum. The resulting solid was extracted with dichloromethane and neat N₃SiMe₃ (16 µl, 0.12 mmol) was added. The resulting solution was then stirred for 18 h and the solvent was removed. The remaining solid was washed with diethyl ether (20 ml × 2) to give the title compound, (I), which was recrystallized from dichloromethane-hexane (Ratio?) to give red crystals (0.074 g, 62.6%; m.p. 471–473 K). Spectroscopic analysis: IR (KBr, ν, cm⁻¹): 2029 (N₃), 843 (PF₆); ¹H NMR (CDCl₃, δ, p.p.m.): 7.74–7.33 (20H, m, Ph), 4.91, 4.39, 4.29, 4.12 (8H, C₅H₄), 1.15 (15H, t, J_PH = 4.0 Hz, C₅Me₅); ¹³C{¹H} NMR (CDCl₃, δ, p.p.m.): 135.7–128.8 (Ph), 104.7 (d, J_RhC = 6.4 Hz, Cp* C₅), 77.5–76.6 (C₅H₄), 8.59 (Cp* Me₅); ³¹P{¹H} NMR (CDCl₃, δ, p.p.m.): 38.79 (d, J_RhP = 146.5 Hz, dppf), −143.8 (sep, J_PF = 708.2); analysis calculated for C₄₄H₄₃F₆N₃P₃FeRh: C 53.95, H 4.43, N 4.29%; found: C 54.23, H 4.39, N 4.24%.

S3. Refinement

All the H atoms were generated in ideal positions and refined in a riding model, with C—H distances in the range 0.93–0.96 Å and U_iso(H) = 1.2U_eq(C). Please check added text.

Computing details

Data collection: XSCANS (Siemens, 1995); cell refinement: XSCANS; data reduction: SHELXTL (Sheldrick, 1997); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures

Fig. 1. The molecular structure of (I), showing 50% probability displacement ellipsoids. H atoms have been omitted for clarity.

Azido-2κN-bis[µ-(1η⁵:2κP)-diphenylphosphinocyclopentadienyl][2(η⁵)- pentamethylcyclopentadienyl]iron(III)rhodium(III) hexafluorophosphate

Crystal data

[FeRh(C10H15)(C17H14P)2(N3)]PF6	F(000) = 1992
Mr = 979.48	Dx = 1.573 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 14.759 (3) Å	Cell parameters from 26 reflections
b = 17.829 (4) Å	θ = 5.1–13.1°
c = 15.736 (4) Å	µ = 0.93 mm^−1
β = 92.669 (12)°	T = 295 K
V = 4136.3 (16) Å^3	Block, red
Z = 4	0.26 × 0.24 × 0.18 mm

Data collection

Siemens P4 diffractometer	3968 reflections with I > 2σ(I)
Radiation source: sealed tube	Rint = 0.052
Graphite monochromator	θmax = 25.0°, θmin = 2.2°
ω scans	h = −17→0
Absorption correction: ψ scan (North et al., 1968)	k = 0→21
Tmin = 0.698, Tmax = 0.914	l = −18→18
7547 measured reflections	3 standard reflections every 97 reflections
7252 independent reflections	intensity decay: none

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.065	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.159	H-atom parameters constrained
S = 1.01	w = 1/[σ^2(Fo^2) + (0.0584P)^2 + 2.6079P] where P = (Fo^2 + 2Fc^2)/3
7252 reflections	(Δ/σ)max < 0.001
523 parameters	Δρmax = 0.58 e Å^−3
0 restraints	Δρmin = −0.46 e Å^−3

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. All non-hydrogen atoms were refined anisotropically. 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 (Ų)

	x	y	z	Uiso*/Ueq
Rh1	0.41021 (4)	0.18591 (4)	0.23054 (4)	0.03903 (19)
Fe1	0.13159 (7)	0.27169 (7)	0.24276 (7)	0.0423 (3)
P1	0.32248 (13)	0.24939 (12)	0.12276 (12)	0.0373 (5)
P2	0.34342 (13)	0.24491 (12)	0.34686 (12)	0.0383 (5)
N1	0.2960 (5)	0.1145 (5)	0.2281 (5)	0.056 (2)
N2	0.2927 (5)	0.0555 (5)	0.2514 (6)	0.071 (3)
N3	0.2820 (9)	−0.0043 (6)	0.2774 (10)	0.176 (7)
C1	0.5092 (5)	0.1164 (6)	0.1645 (6)	0.058 (3)
C2	0.5162 (5)	0.0970 (6)	0.2534 (6)	0.060 (3)
C3	0.5443 (5)	0.1591 (6)	0.2995 (5)	0.056 (2)
C4	0.5565 (5)	0.2201 (5)	0.2414 (5)	0.050 (2)
C5	0.5382 (5)	0.1920 (6)	0.1582 (5)	0.053 (2)
C6	0.4937 (7)	0.0618 (6)	0.0931 (6)	0.083 (3)
H6A	0.4742	0.0147	0.1154	0.099*
H6B	0.5491	0.0547	0.0646	0.099*
H6C	0.4479	0.0809	0.0536	0.099*
C7	0.5059 (7)	0.0197 (6)	0.2866 (7)	0.092 (4)
H7A	0.4856	−0.0129	0.2410	0.110*
H7B	0.4622	0.0197	0.3299	0.110*
H7C	0.5632	0.0024	0.3103	0.110*
C8	0.5764 (6)	0.1613 (6)	0.3921 (5)	0.069 (3)
H8A	0.5916	0.2120	0.4079	0.083*
H8B	0.6289	0.1300	0.4006	0.083*
H8C	0.5290	0.1435	0.4266	0.083*
C9	0.6029 (5)	0.2931 (5)	0.2638 (5)	0.064 (3)
H9A	0.6072	0.2989	0.3245	0.076*
H9B	0.5685	0.3339	0.2390	0.076*
H9C	0.6627	0.2931	0.2422	0.076*
C10	0.5594 (6)	0.2311 (6)	0.0752 (5)	0.073 (3)
H10A	0.5400	0.2000	0.0280	0.087*
H10B	0.6235	0.2398	0.0738	0.087*
H10C	0.5279	0.2782	0.0716	0.087*
C11	0.2020 (5)	0.2617 (5)	0.1356 (4)	0.0383 (19)
C12	0.1342 (5)	0.2049 (5)	0.1394 (5)	0.048 (2)
H12	0.1446	0.1534	0.1394	0.058*
C13	0.0481 (5)	0.2399 (6)	0.1430 (5)	0.055 (2)
H13	−0.0071	0.2152	0.1461	0.066*
C14	0.0600 (5)	0.3164 (6)	0.1412 (5)	0.054 (2)
H14	0.0139	0.3519	0.1429	0.065*
C15	0.1552 (5)	0.3328 (5)	0.1361 (4)	0.045 (2)
H15	0.1814	0.3801	0.1337	0.054*
C16	0.2221 (5)	0.2624 (5)	0.3415 (4)	0.042 (2)
C17	0.1568 (5)	0.2020 (5)	0.3429 (5)	0.050 (2)
H17	0.1692	0.1510	0.3406	0.060*
C18	0.0706 (6)	0.2352 (6)	0.3483 (5)	0.060 (3)
H18	0.0159	0.2094	0.3495	0.072*
C19	0.0804 (6)	0.3134 (6)	0.3516 (5)	0.061 (3)
H19	0.0335	0.3479	0.3552	0.073*
C20	0.1735 (5)	0.3310 (5)	0.3485 (5)	0.055 (2)
H20	0.1986	0.3789	0.3506	0.065*
C21	0.3587 (5)	0.3425 (4)	0.0955 (5)	0.0396 (19)
C22	0.3167 (6)	0.3845 (5)	0.0288 (5)	0.057 (2)
H22	0.2691	0.3636	−0.0040	0.069*
C23	0.3452 (7)	0.4559 (6)	0.0116 (7)	0.075 (3)
H23	0.3177	0.4822	−0.0337	0.090*
C24	0.4144 (8)	0.4895 (6)	0.0609 (8)	0.083 (3)
H24	0.4325	0.5384	0.0501	0.099*
C25	0.4550 (7)	0.4492 (6)	0.1250 (7)	0.075 (3)
H25	0.5016	0.4708	0.1585	0.090*
C26	0.4283 (5)	0.3772 (5)	0.1415 (5)	0.049 (2)
H26	0.4584	0.3508	0.1853	0.059*
C27	0.3197 (5)	0.1957 (5)	0.0230 (4)	0.043 (2)
C28	0.3507 (5)	0.2245 (5)	−0.0529 (5)	0.050 (2)
H28	0.3764	0.2721	−0.0538	0.059*
C29	0.3432 (6)	0.1819 (6)	−0.1279 (5)	0.064 (3)
H29	0.3629	0.2019	−0.1785	0.077*
C30	0.3075 (6)	0.1119 (7)	−0.1271 (6)	0.071 (3)
H30	0.3022	0.0841	−0.1771	0.085*
C31	0.2786 (6)	0.0817 (5)	−0.0512 (6)	0.064 (3)
H31	0.2550	0.0333	−0.0504	0.077*
C32	0.2850 (6)	0.1231 (5)	0.0222 (5)	0.055 (2)
H32	0.2658	0.1022	0.0725	0.066*
C33	0.3966 (5)	0.3336 (5)	0.3768 (4)	0.042 (2)
C34	0.3781 (6)	0.3967 (5)	0.3285 (5)	0.056 (2)
H34	0.3317	0.3956	0.2864	0.068*
C35	0.4278 (8)	0.4618 (6)	0.3419 (6)	0.072 (3)
H35	0.4133	0.5047	0.3105	0.086*
C36	0.4987 (8)	0.4628 (7)	0.4019 (8)	0.087 (4)
H36	0.5343	0.5056	0.4092	0.104*
C37	0.5166 (7)	0.4015 (7)	0.4500 (6)	0.075 (3)
H37	0.5635	0.4028	0.4915	0.090*
C38	0.4660 (5)	0.3365 (5)	0.4383 (5)	0.054 (2)
H38	0.4790	0.2947	0.4721	0.065*
C39	0.3463 (5)	0.1905 (5)	0.4459 (4)	0.046 (2)
C40	0.3617 (6)	0.1143 (5)	0.4451 (6)	0.057 (2)
H40	0.3792	0.0909	0.3956	0.068*
C41	0.3506 (6)	0.0718 (6)	0.5198 (6)	0.073 (3)
H41	0.3618	0.0205	0.5203	0.087*
C42	0.3232 (7)	0.1071 (8)	0.5916 (6)	0.079 (3)
H42	0.3139	0.0789	0.6401	0.094*
C43	0.3092 (6)	0.1826 (7)	0.5936 (5)	0.065 (3)
H43	0.2926	0.2059	0.6434	0.079*
C44	0.3202 (5)	0.2244 (5)	0.5197 (5)	0.054 (2)
H44	0.3098	0.2759	0.5202	0.065*
P3	0.80550 (19)	0.09362 (17)	0.23625 (18)	0.0692 (8)
F1	0.7686 (7)	0.1722 (4)	0.2378 (8)	0.207 (5)
F2	0.7490 (7)	0.0775 (8)	0.3119 (6)	0.232 (6)
F3	0.8587 (7)	0.1089 (7)	0.1615 (7)	0.229 (6)
F4	0.8867 (6)	0.1104 (6)	0.2955 (7)	0.202 (5)
F5	0.7212 (5)	0.0742 (6)	0.1815 (6)	0.186 (4)
F6	0.8387 (5)	0.0111 (4)	0.2351 (7)	0.169 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh1	0.0299 (3)	0.0533 (4)	0.0335 (3)	0.0038 (3)	−0.0035 (2)	−0.0043 (3)
Fe1	0.0286 (6)	0.0624 (8)	0.0356 (6)	−0.0002 (6)	0.0001 (5)	−0.0015 (6)
P1	0.0314 (10)	0.0499 (14)	0.0304 (10)	0.0022 (10)	−0.0014 (8)	−0.0018 (10)
P2	0.0306 (10)	0.0530 (14)	0.0312 (10)	−0.0024 (10)	−0.0023 (8)	−0.0003 (10)
N1	0.044 (4)	0.055 (5)	0.067 (5)	−0.005 (4)	−0.004 (4)	0.017 (4)
N2	0.065 (5)	0.044 (5)	0.099 (7)	0.002 (5)	−0.035 (5)	−0.023 (5)
N3	0.161 (12)	0.062 (8)	0.295 (18)	−0.031 (8)	−0.116 (11)	0.043 (10)
C1	0.033 (5)	0.076 (7)	0.065 (6)	0.013 (5)	−0.006 (4)	−0.021 (5)
C2	0.037 (5)	0.074 (7)	0.066 (6)	0.019 (5)	−0.012 (4)	0.006 (6)
C3	0.037 (5)	0.087 (8)	0.043 (5)	0.013 (5)	−0.010 (4)	−0.008 (5)
C4	0.026 (4)	0.077 (7)	0.047 (5)	0.000 (4)	−0.007 (4)	−0.021 (5)
C5	0.024 (4)	0.082 (7)	0.052 (5)	0.015 (5)	0.001 (3)	−0.008 (5)
C6	0.074 (7)	0.088 (8)	0.083 (7)	0.036 (6)	−0.014 (6)	−0.043 (6)
C7	0.079 (7)	0.093 (9)	0.101 (9)	0.046 (7)	−0.016 (6)	0.001 (7)
C8	0.055 (6)	0.099 (8)	0.052 (5)	0.017 (5)	−0.009 (4)	0.000 (5)
C9	0.034 (5)	0.099 (8)	0.057 (5)	0.000 (5)	−0.006 (4)	−0.018 (5)
C10	0.038 (5)	0.133 (10)	0.048 (5)	0.007 (6)	0.012 (4)	−0.011 (6)
C11	0.034 (4)	0.058 (6)	0.023 (4)	0.003 (4)	−0.005 (3)	0.004 (4)
C12	0.037 (4)	0.065 (6)	0.042 (5)	0.001 (4)	−0.004 (4)	−0.003 (4)
C13	0.034 (5)	0.087 (8)	0.042 (5)	−0.021 (5)	−0.004 (4)	−0.003 (5)
C14	0.036 (4)	0.082 (7)	0.044 (5)	0.014 (5)	−0.001 (4)	0.004 (5)
C15	0.043 (4)	0.054 (6)	0.037 (4)	0.005 (4)	0.000 (4)	0.001 (4)
C16	0.040 (4)	0.064 (6)	0.021 (4)	0.007 (4)	−0.003 (3)	−0.005 (4)
C17	0.039 (4)	0.065 (6)	0.045 (5)	0.001 (4)	0.002 (4)	0.006 (4)
C18	0.041 (5)	0.098 (9)	0.041 (5)	0.005 (5)	0.013 (4)	0.006 (5)
C19	0.044 (5)	0.095 (8)	0.043 (5)	0.017 (6)	0.003 (4)	−0.015 (6)
C20	0.043 (5)	0.074 (7)	0.047 (5)	0.008 (5)	0.000 (4)	−0.016 (5)
C21	0.035 (4)	0.046 (5)	0.038 (4)	−0.003 (4)	0.009 (3)	−0.006 (4)
C22	0.062 (6)	0.061 (6)	0.050 (5)	−0.001 (5)	0.004 (4)	−0.002 (5)
C23	0.070 (7)	0.078 (8)	0.079 (7)	0.014 (6)	0.022 (6)	0.027 (6)
C24	0.093 (9)	0.056 (7)	0.103 (9)	−0.011 (7)	0.044 (7)	0.012 (7)
C25	0.085 (8)	0.070 (8)	0.073 (7)	−0.039 (7)	0.024 (6)	−0.012 (6)
C26	0.050 (5)	0.065 (6)	0.033 (4)	−0.018 (5)	0.001 (4)	−0.007 (4)
C27	0.026 (4)	0.069 (6)	0.035 (4)	0.007 (4)	−0.002 (3)	−0.003 (4)
C28	0.036 (4)	0.074 (6)	0.038 (5)	0.006 (4)	−0.003 (4)	−0.015 (4)
C29	0.046 (5)	0.102 (8)	0.044 (5)	0.000 (6)	0.001 (4)	−0.011 (6)
C30	0.056 (6)	0.099 (9)	0.057 (6)	0.012 (6)	0.004 (5)	−0.039 (6)
C31	0.056 (6)	0.064 (7)	0.073 (7)	−0.002 (5)	−0.001 (5)	−0.027 (6)
C32	0.063 (6)	0.056 (6)	0.047 (5)	0.003 (5)	0.003 (4)	−0.005 (5)
C33	0.045 (4)	0.055 (6)	0.027 (4)	−0.007 (4)	0.007 (3)	−0.010 (4)
C34	0.056 (6)	0.067 (7)	0.047 (5)	0.001 (5)	0.018 (4)	−0.008 (5)
C35	0.097 (8)	0.052 (7)	0.067 (7)	−0.014 (6)	0.009 (6)	0.001 (5)
C36	0.088 (9)	0.093 (10)	0.082 (8)	−0.037 (7)	0.029 (7)	−0.034 (7)
C37	0.063 (6)	0.110 (10)	0.053 (6)	−0.032 (7)	0.001 (5)	−0.023 (7)
C38	0.046 (5)	0.064 (7)	0.050 (5)	−0.001 (4)	−0.014 (4)	−0.013 (4)
C39	0.037 (4)	0.070 (6)	0.029 (4)	−0.005 (5)	−0.009 (3)	0.003 (4)
C40	0.055 (5)	0.063 (7)	0.052 (5)	−0.007 (5)	−0.011 (4)	0.013 (5)
C41	0.074 (7)	0.067 (7)	0.074 (7)	−0.014 (6)	−0.025 (6)	0.017 (6)
C42	0.066 (7)	0.116 (11)	0.053 (6)	−0.028 (7)	−0.016 (5)	0.033 (7)
C43	0.056 (6)	0.098 (9)	0.043 (5)	−0.003 (6)	0.006 (4)	−0.001 (6)
C44	0.052 (5)	0.076 (7)	0.035 (5)	−0.002 (5)	0.000 (4)	0.009 (5)
P3	0.0599 (16)	0.075 (2)	0.0726 (18)	0.0056 (15)	0.0058 (14)	−0.0193 (15)
F1	0.206 (10)	0.077 (6)	0.337 (15)	0.040 (6)	0.011 (10)	−0.040 (8)
F2	0.179 (10)	0.363 (17)	0.162 (9)	0.068 (10)	0.083 (8)	0.086 (10)
F3	0.193 (10)	0.313 (15)	0.192 (10)	0.093 (10)	0.125 (9)	0.103 (10)
F4	0.128 (7)	0.228 (11)	0.240 (11)	−0.038 (7)	−0.089 (8)	−0.042 (9)
F5	0.118 (6)	0.230 (11)	0.203 (10)	0.029 (7)	−0.077 (7)	−0.082 (8)
F6	0.112 (6)	0.093 (6)	0.303 (12)	0.033 (5)	0.005 (7)	−0.016 (7)

Geometric parameters (Å, º)

Rh1—N1	2.111 (7)	C16—C20	1.426 (11)
Rh1—C1	2.211 (8)	C16—C17	1.446 (11)
Rh1—C4	2.243 (8)	C17—C18	1.409 (11)
Rh1—C2	2.244 (9)	C17—H17	0.9300
Rh1—C5	2.254 (7)	C18—C19	1.402 (13)
Rh1—C3	2.264 (8)	C18—H18	0.9300
Rh1—P2	2.366 (2)	C19—C20	1.413 (11)
Rh1—P1	2.373 (2)	C19—H19	0.9300
Fe1—C16	2.009 (7)	C20—H20	0.9300
Fe1—C12	2.018 (8)	C21—C26	1.376 (10)
Fe1—C17	2.027 (8)	C21—C22	1.410 (11)
Fe1—C11	2.029 (7)	C22—C23	1.371 (12)
Fe1—C13	2.031 (8)	C22—H22	0.9300
Fe1—C18	2.032 (8)	C23—C24	1.390 (14)
Fe1—C14	2.038 (8)	C23—H23	0.9300
Fe1—C20	2.044 (8)	C24—C25	1.356 (14)
Fe1—C19	2.044 (8)	C24—H24	0.9300
Fe1—C15	2.044 (8)	C25—C26	1.371 (12)
P1—C21	1.802 (8)	C25—H25	0.9300
P1—C11	1.812 (7)	C26—H26	0.9300
P1—C27	1.837 (8)	C27—C32	1.393 (11)
P2—C16	1.815 (7)	C27—C28	1.396 (10)
P2—C33	1.818 (8)	C28—C29	1.403 (11)
P2—C39	1.836 (8)	C28—H28	0.9300
N1—N2	1.114 (10)	C29—C30	1.355 (13)
N2—N3	1.155 (12)	C29—H29	0.9300
C1—C5	1.420 (12)	C30—C31	1.395 (13)
C1—C2	1.440 (12)	C30—H30	0.9300
C1—C6	1.496 (12)	C31—C32	1.370 (11)
C2—C3	1.376 (12)	C31—H31	0.9300
C2—C7	1.484 (13)	C32—H32	0.9300
C3—C4	1.437 (12)	C33—C38	1.376 (10)
C3—C8	1.512 (10)	C33—C34	1.379 (11)
C4—C5	1.416 (10)	C34—C35	1.384 (12)
C4—C9	1.505 (11)	C34—H34	0.9300
C5—C10	1.526 (11)	C35—C36	1.377 (14)
C6—H6A	0.9600	C35—H35	0.9300
C6—H6B	0.9600	C36—C37	1.349 (14)
C6—H6C	0.9600	C36—H36	0.9300
C7—H7A	0.9600	C37—C38	1.385 (12)
C7—H7B	0.9600	C37—H37	0.9300
C7—H7C	0.9600	C38—H38	0.9300
C8—H8A	0.9600	C39—C40	1.377 (11)
C8—H8B	0.9600	C39—C44	1.380 (10)
C8—H8C	0.9600	C40—C41	1.415 (12)
C9—H9A	0.9600	C40—H40	0.9300
C9—H9B	0.9600	C41—C42	1.371 (14)
C9—H9C	0.9600	C41—H41	0.9300
C10—H10A	0.9600	C42—C43	1.361 (13)
C10—H10B	0.9600	C42—H42	0.9300
C10—H10C	0.9600	C43—C44	1.398 (11)
C11—C12	1.428 (10)	C43—H43	0.9300
C11—C15	1.444 (10)	C44—H44	0.9300
C12—C13	1.418 (11)	P3—F3	1.470 (8)
C12—H12	0.9300	P3—F1	1.504 (8)
C13—C14	1.376 (12)	P3—F2	1.512 (9)
C13—H13	0.9300	P3—F4	1.513 (8)
C14—C15	1.440 (10)	P3—F5	1.520 (7)
C14—H14	0.9300	P3—F6	1.552 (8)
C15—H15	0.9300
N1—Rh1—C1	101.4 (3)	C12—C11—C15	106.6 (6)
N1—Rh1—C4	158.5 (3)	C12—C11—P1	127.8 (6)
C1—Rh1—C4	62.2 (3)	C15—C11—P1	125.4 (6)
N1—Rh1—C2	97.3 (3)	C12—C11—Fe1	68.9 (4)
C1—Rh1—C2	37.7 (3)	C15—C11—Fe1	69.8 (4)
C4—Rh1—C2	61.2 (3)	P1—C11—Fe1	130.3 (4)
N1—Rh1—C5	135.0 (3)	C13—C12—C11	108.7 (8)
C1—Rh1—C5	37.1 (3)	C13—C12—Fe1	70.0 (5)
C4—Rh1—C5	36.7 (3)	C11—C12—Fe1	69.8 (4)
C2—Rh1—C5	61.4 (3)	C13—C12—H12	125.7
N1—Rh1—C3	124.1 (3)	C11—C12—H12	125.7
C1—Rh1—C3	61.6 (3)	Fe1—C12—H12	126.2
C4—Rh1—C3	37.2 (3)	C14—C13—C12	108.7 (7)
C2—Rh1—C3	35.5 (3)	C14—C13—Fe1	70.5 (5)
C5—Rh1—C3	61.1 (3)	C12—C13—Fe1	69.0 (4)
N1—Rh1—P2	85.5 (2)	C14—C13—H13	125.7
C1—Rh1—P2	157.0 (2)	C12—C13—H13	125.7
C4—Rh1—P2	104.7 (2)	Fe1—C13—H13	126.4
C2—Rh1—P2	120.2 (2)	C13—C14—C15	109.1 (8)
C5—Rh1—P2	139.3 (2)	C13—C14—Fe1	70.0 (5)
C3—Rh1—P2	96.3 (2)	C15—C14—Fe1	69.6 (4)
N1—Rh1—P1	82.3 (2)	C13—C14—H14	125.4
C1—Rh1—P1	106.4 (2)	C15—C14—H14	125.4
C4—Rh1—P1	114.6 (3)	Fe1—C14—H14	126.6
C2—Rh1—P1	143.6 (2)	C14—C15—C11	106.9 (8)
C5—Rh1—P1	93.3 (2)	C14—C15—Fe1	69.1 (5)
C3—Rh1—P1	151.6 (3)	C11—C15—Fe1	68.7 (4)
P2—Rh1—P1	96.19 (7)	C14—C15—H15	126.5
C16—Fe1—C12	122.6 (3)	C11—C15—H15	126.5
C16—Fe1—C17	42.0 (3)	Fe1—C15—H15	127.2
C12—Fe1—C17	104.8 (3)	C20—C16—C17	107.4 (7)
C16—Fe1—C11	106.7 (3)	C20—C16—P2	130.0 (6)
C12—Fe1—C11	41.3 (3)	C17—C16—P2	121.9 (6)
C17—Fe1—C11	120.6 (3)	C20—C16—Fe1	70.7 (4)
C16—Fe1—C13	158.9 (4)	C17—C16—Fe1	69.7 (4)
C12—Fe1—C13	41.0 (3)	P2—C16—Fe1	132.0 (4)
C17—Fe1—C13	120.8 (4)	C18—C17—C16	107.0 (8)
C11—Fe1—C13	69.4 (3)	C18—C17—Fe1	69.9 (5)
C16—Fe1—C18	69.2 (3)	C16—C17—Fe1	68.3 (4)
C12—Fe1—C18	119.7 (4)	C18—C17—H17	126.5
C17—Fe1—C18	40.6 (3)	C16—C17—H17	126.5
C11—Fe1—C18	156.1 (4)	Fe1—C17—H17	126.8
C13—Fe1—C18	105.5 (4)	C19—C18—C17	109.1 (8)
C16—Fe1—C14	160.3 (4)	C19—C18—Fe1	70.3 (5)
C12—Fe1—C14	68.1 (3)	C17—C18—Fe1	69.5 (5)
C17—Fe1—C14	156.8 (4)	C19—C18—H18	125.4
C11—Fe1—C14	69.5 (3)	C17—C18—H18	125.4
C13—Fe1—C14	39.5 (3)	Fe1—C18—H18	126.4
C18—Fe1—C14	122.2 (3)	C18—C19—C20	108.6 (8)
C16—Fe1—C20	41.2 (3)	C18—C19—Fe1	69.4 (5)
C12—Fe1—C20	161.0 (3)	C20—C19—Fe1	69.8 (4)
C17—Fe1—C20	69.3 (4)	C18—C19—H19	125.7
C11—Fe1—C20	125.1 (3)	C20—C19—H19	125.7
C13—Fe1—C20	157.5 (4)	Fe1—C19—H19	126.7
C18—Fe1—C20	68.2 (4)	C19—C20—C16	107.8 (8)
C14—Fe1—C20	124.2 (4)	C19—C20—Fe1	69.8 (5)
C16—Fe1—C19	68.9 (3)	C16—C20—Fe1	68.1 (4)
C12—Fe1—C19	155.8 (4)	C19—C20—H20	126.1
C17—Fe1—C19	68.5 (4)	C16—C20—H20	126.1
C11—Fe1—C19	162.1 (4)	Fe1—C20—H20	127.6
C13—Fe1—C19	121.0 (3)	C26—C21—C22	116.4 (8)
C18—Fe1—C19	40.2 (4)	C26—C21—P1	120.7 (6)
C14—Fe1—C19	108.5 (4)	C22—C21—P1	122.8 (6)
C20—Fe1—C19	40.4 (3)	C23—C22—C21	120.8 (9)
C16—Fe1—C15	123.2 (3)	C23—C22—H22	119.6
C12—Fe1—C15	69.0 (3)	C21—C22—H22	119.6
C17—Fe1—C15	158.9 (3)	C22—C23—C24	121.0 (10)
C11—Fe1—C15	41.5 (3)	C22—C23—H23	119.5
C13—Fe1—C15	68.6 (3)	C24—C23—H23	119.5
C18—Fe1—C15	160.1 (3)	C25—C24—C23	118.3 (10)
C14—Fe1—C15	41.3 (3)	C25—C24—H24	120.8
C20—Fe1—C15	109.6 (3)	C23—C24—H24	120.8
C19—Fe1—C15	125.3 (4)	C24—C25—C26	121.1 (10)
C21—P1—C11	102.6 (4)	C24—C25—H25	119.4
C21—P1—C27	105.7 (4)	C26—C25—H25	119.4
C11—P1—C27	100.1 (3)	C25—C26—C21	122.3 (9)
C21—P1—Rh1	116.8 (3)	C25—C26—H26	118.8
C11—P1—Rh1	118.9 (2)	C21—C26—H26	118.8
C27—P1—Rh1	110.6 (3)	C32—C27—C28	118.0 (7)
C16—P2—C33	106.0 (4)	C32—C27—P1	119.0 (6)
C16—P2—C39	96.5 (3)	C28—C27—P1	123.0 (7)
C33—P2—C39	104.3 (4)	C27—C28—C29	120.3 (9)
C16—P2—Rh1	119.1 (2)	C27—C28—H28	119.8
C33—P2—Rh1	113.4 (2)	C29—C28—H28	119.8
C39—P2—Rh1	115.3 (3)	C30—C29—C28	120.3 (9)
N2—N1—Rh1	127.6 (7)	C30—C29—H29	119.8
N1—N2—N3	174.3 (13)	C28—C29—H29	119.8
C5—C1—C2	106.7 (8)	C29—C30—C31	119.9 (9)
C5—C1—C6	127.0 (9)	C29—C30—H30	120.0
C2—C1—C6	125.1 (10)	C31—C30—H30	120.0
C5—C1—Rh1	73.1 (5)	C32—C31—C30	120.1 (9)
C2—C1—Rh1	72.4 (5)	C32—C31—H31	120.0
C6—C1—Rh1	129.5 (6)	C30—C31—H31	120.0
C3—C2—C1	109.0 (9)	C31—C32—C27	121.3 (8)
C3—C2—C7	126.5 (9)	C31—C32—H32	119.4
C1—C2—C7	124.1 (10)	C27—C32—H32	119.4
C3—C2—Rh1	73.0 (5)	C38—C33—C34	118.6 (8)
C1—C2—Rh1	69.9 (5)	C38—C33—P2	120.9 (7)
C7—C2—Rh1	129.1 (7)	C34—C33—P2	119.6 (6)
C2—C3—C4	108.5 (8)	C33—C34—C35	120.7 (9)
C2—C3—C8	127.1 (9)	C33—C34—H34	119.7
C4—C3—C8	123.3 (9)	C35—C34—H34	119.7
C2—C3—Rh1	71.4 (5)	C36—C35—C34	119.7 (10)
C4—C3—Rh1	70.6 (4)	C36—C35—H35	120.1
C8—C3—Rh1	133.1 (6)	C34—C35—H35	120.1
C5—C4—C3	107.2 (8)	C37—C36—C35	119.8 (11)
C5—C4—C9	126.0 (9)	C37—C36—H36	120.1
C3—C4—C9	125.1 (7)	C35—C36—H36	120.1
C5—C4—Rh1	72.1 (4)	C36—C37—C38	120.9 (10)
C3—C4—Rh1	72.2 (5)	C36—C37—H37	119.6
C9—C4—Rh1	132.8 (6)	C38—C37—H37	119.6
C4—C5—C1	108.4 (8)	C33—C38—C37	120.2 (9)
C4—C5—C10	126.3 (9)	C33—C38—H38	119.9
C1—C5—C10	124.7 (8)	C37—C38—H38	119.9
C4—C5—Rh1	71.2 (4)	C40—C39—C44	119.6 (8)
C1—C5—Rh1	69.8 (5)	C40—C39—P2	120.7 (6)
C10—C5—Rh1	131.6 (5)	C44—C39—P2	119.1 (7)
C1—C6—H6A	109.5	C39—C40—C41	119.6 (9)
C1—C6—H6B	109.5	C39—C40—H40	120.2
H6A—C6—H6B	109.5	C41—C40—H40	120.2
C1—C6—H6C	109.5	C42—C41—C40	119.2 (10)
H6A—C6—H6C	109.5	C42—C41—H41	120.4
H6B—C6—H6C	109.5	C40—C41—H41	120.4
C2—C7—H7A	109.5	C43—C42—C41	121.6 (10)
C2—C7—H7B	109.5	C43—C42—H42	119.2
H7A—C7—H7B	109.5	C41—C42—H42	119.2
C2—C7—H7C	109.5	C42—C43—C44	119.0 (9)
H7A—C7—H7C	109.5	C42—C43—H43	120.5
H7B—C7—H7C	109.5	C44—C43—H43	120.5
C3—C8—H8A	109.5	C39—C44—C43	120.9 (9)
C3—C8—H8B	109.5	C39—C44—H44	119.5
H8A—C8—H8B	109.5	C43—C44—H44	119.5
C3—C8—H8C	109.5	F3—P3—F1	92.7 (7)
H8A—C8—H8C	109.5	F3—P3—F2	178.8 (8)
H8B—C8—H8C	109.5	F1—P3—F2	87.2 (7)
C4—C9—H9A	109.5	F3—P3—F4	91.0 (7)
C4—C9—H9B	109.5	F1—P3—F4	94.7 (6)
H9A—C9—H9B	109.5	F2—P3—F4	90.2 (7)
C4—C9—H9C	109.5	F3—P3—F5	92.5 (7)
H9A—C9—H9C	109.5	F1—P3—F5	86.3 (6)
H9B—C9—H9C	109.5	F2—P3—F5	86.3 (6)
C5—C10—H10A	109.5	F4—P3—F5	176.3 (7)
C5—C10—H10B	109.5	F3—P3—F6	89.2 (6)
H10A—C10—H10B	109.5	F1—P3—F6	177.2 (6)
C5—C10—H10C	109.5	F2—P3—F6	90.8 (6)
H10A—C10—H10C	109.5	F4—P3—F6	87.3 (6)
H10B—C10—H10C	109.5	F5—P3—F6	91.6 (5)