Bis(tert-butyl isocyanide)-1κ2C-di-μ-carbonyl-2:3κ4C-octa­carbonyl-1κ2C,2κ3C,3κ3C-triangulo-diironosmium

Evans, C.; Farrugia, L.J.; Tegel, M.

doi:10.1107/S1600536806004247

metal-organic compounds

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 62| Part 3| March 2006| Pages m478-m479

https://doi.org/10.1107/S1600536806004247

Bis(tert-butyl isocyanide)-1κ²C-di-μ-carbonyl-2:3κ⁴C-octacarbonyl-1κ²C,2κ³C,3κ³C-triangulo-diironosmium

Cameron Evans,^a ^* Louis J. Farrugia ^a and Marcus Tegel ^a

^aWest CHEM, Department of Chemistry, University of Glasgow, Joseph Black Building, University Avenue, Glasgow G12 8QQ, Scotland
^*Correspondence e-mail: cevans@chem.gla.ac.uk

(Received 24 January 2006; accepted 3 February 2006; online 10 February 2006)

The preparation of the mixed-metal cluster, [Fe₂Os(C₅H₉N)₂(CO)₁₀], and its crystal structure at 100 K are reported. This complex, along with the cluster in the preceding paper, are the first structurally characterized substitution derivatives of Fe₂Os(CO)₁₂. The isonitrile ligands adopt axial positions on the osmium centre and the cluster is isostructural with the Fe₂Ru analogue.

Comment

The background to this study has been set out in the preceding paper (Evans et al., 2006 ). We report here and in that paper the synthesis and structures of Fe₂Os(CO)_12−n(CNBu^t)_n (n = 1 and 2).

Fe₂Os(CO)₁₀(CNBu^t)₂, (II), was prepared by carbonyl substitution of the parent Fe₂Os(CO)₁₂ cluster using standard methods (Farrugia & Mertes, 2002 ). The compound was characterized spectroscopically, by FAB mass spectrometry, and by single-crystal X-ray structure determination. The structure was determined at room temperature and 100 K with no discernible metal atom disorder at either temperature. As the structures at different temperatures are essentially identical, only the more precise low-temperature structure will be discussed here.

The structure of (II) at 100 K is shown in Fig. 1. Both isonitrile ligands adopt axial positions on the Os atom, identical to that reported for the Fe₂Ru analogue but contrasting with Fe₃(CO)₁₀(CNBu^t)₂ [where one isonitrile is axial and the other equatorial (Murray et al., 1990 )] and M₃(CO)₁₀(CNR)₂ [M = Ru and Os; R = Bu^t and Me] (Dawson et al., 1982 ; Bruce et al., 1983 ; Farrugia et al., 1998 ), where the two isonitrile ligands are axial but attached to different metal centres. The average Fe—Os distance [2.7590 (3) Å] and Fe—Fe distance [2.5738 (3) Å] are longer than those reported (Farrugia & Mertes, 2002) for the ruthenium analogue [Ru—Fe = 2.7527 (3) Å and Fe—Fe = 2.5678 (2) Å]. Two carbonyl ligands symmetrically bridge the Fe—Fe bond [δ(M—C) = 0.009 and 0.003 Å for C14 and C24, respectively].

Figure 1
A view of Fe₂Os(CO)₁₀(CNBu^t)₂, showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level, with H atoms represented by circles of arbitrary size.

Experimental

Complex (II) was prepared in the same manner as reported for the ruthenium analogue (Farrugia & Mertes, 2002) by reaction of the parent carbonyl with a 1:2 molar ratio of isonitrile. The product was purified by chromatography on Florisil using hexane/CH₂Cl₂ mixtures as eluant. Crystals were obtained from a concentrated hexane solution at 25 K. Analysis calculated for C₂₀H₁₈Fe₂N₂O₁₀Os: C 32.10, H 2.42, N 3.74%; found: C 32.15, H 2.20, N 3.74%. IR [ν(CN), cm⁻¹] 2200 (vw), 2170 (m); IR [ν(CO), cm⁻¹] 2053 (w), 2021 (vs), 2015 (vs), 1981 (m), 1975 (m), 1901 (vw), 1834 (vw), 1802 (w). ¹H NMR: δ 1.54 (s, CH₃). Mass spectrum, m/z = 750.2 [M⁺], 694.2 [M⁺ − 2CO], 666.2 [M⁺ − 3CO], 638.2 [M⁺ − 4CO], 610.2 [M⁺ − 5CO], 582.2 [M⁺ − 6CO], 554.3 [M⁺ − 7CO], 526.3 [M⁺ − 8CO], 498.3 [M⁺ − 9CO], 470.3 [M⁺ − 10CO].

Crystal data

[Fe₂Os(C₅H₉N)₂(CO)₁₀]
M_r = 748.26
Monoclinic, P 2₁ /a
a = 11.6903 (2) Å
b = 12.4357 (2) Å
c = 17.6041 (3) Å
β = 91.753 (1)°
V = 2558.03 (7) Å³
Z = 4
D_x = 1.943 Mg m⁻³
Mo Kα radiation
Cell parameters from 11369 reflections
θ = 2.2–35.0°
μ = 6.13 mm⁻¹
T = 100 (2) K
Prism, purple
0.3 × 0.3 × 0.2 mm

Data collection

Nonius KappaCCD diffractometer
φ or ω scans
Absorption correction: multi-scan(Blessing, 1995 )T_min = 0.197, T_max = 0.294
64585 measured reflections
10967 independent reflections
9945 reflections with I > 2σ(I)
R_int = 0.032
θ_max = 35.0°
h = −18 → 18
k = −20 → 20
l = −27 → 28

Refinement

Refinement on F²
R[F² > 2σ(F²)] = 0.021
wR(F²) = 0.042
S = 1.1
10967 reflections
317 parameters
H-atom parameters constrained
w = 1/[σ²(F_o²) + (0.0113P)² + 1.9594P] where P = (F_o² + 2F_c²)/3
(Δ/σ)_max = 0.002
Δρ_max = 1.28 e Å⁻³
Δρ_min = −0.94 e Å⁻³
Extinction correction: SHELXL97
Extinction coefficient: 0.00024 (4)

All H atoms were placed in calculated positions and refined using a riding model [C—H = 0.98 Å and U_iso(H) = 1.5U_eq(C)]. The highest features in the difference map are associated with the Os atom.

Data collection: COLLECT (Nonius, 2000 ); cell refinement: SCALEPACK (Otwinowski & Minor, 1997 ); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ); software used to prepare material for publication: WinGX (Farrugia, 1999 ).

Supporting information

Crystal structure: contains datablocks II, global. DOI: https://doi.org/10.1107/S1600536806004247/hg6301sup1.cif

Structure factors: contains datablock II. DOI: https://doi.org/10.1107/S1600536806004247/hg6301IIsup2.hkl

Computing details top

Data collection: COLLECT (Nonius, 2000); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Bis(tert-butyl isocyanide)-1κ²C-di-µ-carbonyl-2:3κ⁴C-octacarbonyl- 1κ²C,2κ³C,3κ³C-triangulo-diironosmium top

Crystal data top

[Fe₂Os(C₅H₉N)₂(CO)₁₀]	F(000) = 1440
M_r = 748.26	D_x = 1.943 Mg m⁻³
Monoclinic, P2₁/a	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yab	Cell parameters from 11369 reflections
a = 11.6903 (2) Å	θ = 2.2–35.0°
b = 12.4357 (2) Å	µ = 6.13 mm⁻¹
c = 17.6041 (3) Å	T = 100 K
β = 91.753 (1)°	Prism, purple
V = 2558.03 (7) Å³	0.3 × 0.3 × 0.2 mm
Z = 4

Data collection top

KappaCCD diffractometer	9945 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.032
CCD rotation images, thick slices scans	θ_max = 35.0°, θ_min = 2.4°
Absorption correction: multi-scan (Blessing, 1995)	h = −18→18
T_min = 0.197, T_max = 0.294	k = −20→20
64585 measured reflections	l = −27→28
10967 independent reflections

Refinement top

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)] = 0.021	H-atom parameters constrained
wR(F²) = 0.042	w = 1/[σ²(F_o²) + (0.0113P)² + 1.9594P] where P = (F_o² + 2F_c²)/3
S = 1.1	(Δ/σ)_max = 0.002
10967 reflections	Δρ_max = 1.28 e Å⁻³
317 parameters	Δρ_min = −0.94 e Å⁻³
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00024 (4)

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.

Refinement. 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) top

	x	y	z	U_iso*/U_eq
Os1	0.796803 (5)	0.078714 (5)	0.264536 (3)	0.01175 (2)
Fe1	0.715245 (19)	−0.128082 (18)	0.246561 (13)	0.01250 (4)
Fe2	0.567762 (19)	0.024601 (19)	0.256179 (14)	0.01351 (4)
N1	0.79148 (13)	0.09910 (12)	0.08484 (9)	0.0182 (3)
N2	0.79307 (13)	0.04302 (13)	0.44331 (9)	0.0176 (3)
O11	0.59757 (13)	−0.33642 (11)	0.23028 (9)	0.0249 (3)
O12	0.88483 (13)	−0.14605 (12)	0.12654 (8)	0.0261 (3)
O13	0.88504 (13)	−0.19340 (12)	0.36481 (9)	0.0270 (3)
O14	0.58792 (12)	−0.07302 (11)	0.10291 (8)	0.0207 (2)
O21	0.33447 (12)	−0.06186 (13)	0.23777 (10)	0.0294 (3)
O22	0.53743 (15)	0.20690 (13)	0.15018 (10)	0.0320 (3)
O23	0.53714 (14)	0.17035 (13)	0.38615 (9)	0.0308 (3)
O24	0.58865 (12)	−0.12054 (11)	0.39045 (8)	0.0212 (2)
O31	0.79104 (13)	0.32166 (11)	0.28107 (9)	0.0265 (3)
O32	1.05737 (12)	0.07111 (12)	0.26688 (10)	0.0273 (3)
C1	0.79257 (14)	0.09169 (13)	0.15043 (10)	0.0149 (3)
C2	0.79353 (14)	0.05589 (13)	0.37818 (10)	0.0158 (3)
C11	0.64394 (15)	−0.25598 (14)	0.23622 (10)	0.0166 (3)
C12	0.81911 (15)	−0.13642 (14)	0.17307 (10)	0.0180 (3)
C13	0.81919 (15)	−0.16485 (14)	0.31989 (10)	0.0180 (3)
C14	0.61172 (14)	−0.06415 (13)	0.16762 (10)	0.0163 (3)
C21	0.42448 (15)	−0.02751 (14)	0.24587 (10)	0.0182 (3)
C22	0.55314 (15)	0.13531 (15)	0.19031 (11)	0.0201 (3)
C23	0.55223 (15)	0.11236 (15)	0.33704 (11)	0.0202 (3)
C24	0.61162 (14)	−0.09012 (14)	0.32994 (10)	0.0168 (3)
C31	0.79279 (14)	0.22992 (14)	0.27532 (10)	0.0170 (3)
C32	0.95936 (15)	0.07170 (13)	0.26613 (10)	0.0168 (3)
C100	0.78631 (17)	0.10920 (16)	0.00192 (10)	0.0206 (3)
C101	0.6633 (2)	0.1395 (2)	−0.02095 (14)	0.0380 (6)
H11A	0.6444	0.2092	0.0015	0.057*
H11B	0.6109	0.0845	−0.0025	0.057*
H11C	0.6557	0.1443	−0.0764	0.057*
C102	0.8185 (3)	0.00110 (19)	−0.03189 (13)	0.0362 (5)
H12A	0.7626	−0.0533	−0.0175	0.054*
H12B	0.8948	−0.0199	−0.0126	0.054*
H12C	0.819	0.0069	−0.0874	0.054*
C103	0.8706 (2)	0.19684 (19)	−0.01871 (13)	0.0317 (5)
H13A	0.8473	0.2651	0.0039	0.048*
H13B	0.8716	0.2044	−0.0741	0.048*
H13C	0.9473	0.1775	0.0008	0.048*
C200	0.78282 (16)	0.02367 (16)	0.52508 (10)	0.0203 (3)
C201	0.8067 (2)	−0.09521 (18)	0.53928 (12)	0.0321 (5)
H21A	0.7491	−0.1386	0.5117	0.048*
H21B	0.8035	−0.1102	0.5938	0.048*
H21C	0.8829	−0.1132	0.5214	0.048*
C202	0.6608 (2)	0.0530 (2)	0.54526 (13)	0.0358 (5)
H22A	0.6068	0.0062	0.5174	0.054*
H22B	0.6457	0.1281	0.5314	0.054*
H22C	0.6515	0.0437	0.6	0.054*
C203	0.8706 (2)	0.0943 (2)	0.56696 (12)	0.0328 (5)
H23A	0.9478	0.073	0.5529	0.049*
H23B	0.8629	0.0857	0.6219	0.049*
H23C	0.8576	0.1697	0.553	0.049*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Os1	0.01157 (3)	0.01227 (3)	0.01136 (3)	−0.00138 (2)	−0.00030 (2)	0.00027 (2)
Fe1	0.01141 (9)	0.01120 (9)	0.01485 (10)	0.00009 (7)	−0.00012 (7)	−0.00092 (7)
Fe2	0.01043 (9)	0.01270 (9)	0.01735 (10)	0.00028 (7)	−0.00046 (8)	−0.00107 (8)
N1	0.0176 (6)	0.0210 (7)	0.0161 (6)	−0.0007 (5)	0.0000 (5)	0.0036 (5)
N2	0.0175 (6)	0.0206 (7)	0.0148 (6)	−0.0028 (5)	−0.0002 (5)	−0.0020 (5)
O11	0.0254 (7)	0.0174 (6)	0.0317 (8)	−0.0042 (5)	−0.0045 (6)	0.0005 (5)
O12	0.0241 (7)	0.0309 (7)	0.0237 (7)	0.0057 (6)	0.0058 (5)	−0.0002 (6)
O13	0.0269 (7)	0.0290 (7)	0.0246 (7)	0.0034 (6)	−0.0082 (6)	0.0002 (6)
O14	0.0216 (6)	0.0230 (6)	0.0173 (6)	0.0020 (5)	−0.0034 (5)	−0.0020 (5)
O21	0.0170 (6)	0.0325 (8)	0.0388 (9)	−0.0052 (5)	0.0000 (6)	−0.0067 (6)
O22	0.0361 (8)	0.0272 (7)	0.0329 (8)	0.0083 (6)	0.0025 (7)	0.0084 (6)
O23	0.0309 (8)	0.0314 (8)	0.0300 (8)	0.0043 (6)	−0.0008 (6)	−0.0121 (6)
O24	0.0224 (6)	0.0236 (6)	0.0179 (6)	−0.0021 (5)	0.0028 (5)	0.0013 (5)
O31	0.0250 (7)	0.0162 (6)	0.0383 (8)	−0.0008 (5)	0.0025 (6)	−0.0014 (5)
O32	0.0152 (6)	0.0293 (7)	0.0375 (8)	0.0000 (5)	−0.0006 (5)	0.0005 (6)
C1	0.0122 (6)	0.0147 (7)	0.0177 (7)	−0.0004 (5)	−0.0001 (5)	0.0012 (5)
C2	0.0146 (7)	0.0162 (7)	0.0165 (7)	−0.0022 (5)	−0.0001 (5)	−0.0010 (5)
C11	0.0181 (7)	0.0160 (7)	0.0156 (7)	0.0018 (5)	−0.0028 (5)	0.0003 (5)
C12	0.0168 (7)	0.0183 (7)	0.0188 (7)	0.0023 (6)	−0.0011 (6)	0.0013 (6)
C13	0.0177 (7)	0.0177 (7)	0.0186 (7)	−0.0006 (6)	−0.0004 (6)	−0.0008 (6)
C14	0.0135 (7)	0.0159 (7)	0.0195 (7)	−0.0010 (5)	−0.0002 (5)	0.0002 (5)
C21	0.0165 (7)	0.0188 (7)	0.0194 (8)	0.0006 (6)	0.0007 (6)	−0.0022 (6)
C22	0.0179 (7)	0.0200 (8)	0.0226 (8)	0.0033 (6)	0.0013 (6)	−0.0012 (6)
C23	0.0167 (7)	0.0207 (8)	0.0232 (8)	0.0015 (6)	−0.0014 (6)	−0.0017 (6)
C24	0.0147 (7)	0.0173 (7)	0.0184 (7)	−0.0026 (5)	−0.0010 (5)	−0.0019 (6)
C31	0.0142 (7)	0.0182 (7)	0.0188 (8)	−0.0014 (5)	0.0013 (6)	−0.0003 (6)
C32	0.0164 (7)	0.0157 (7)	0.0182 (7)	−0.0002 (5)	−0.0007 (5)	0.0007 (6)
C100	0.0243 (8)	0.0244 (8)	0.0130 (7)	0.0007 (6)	−0.0001 (6)	0.0042 (6)
C101	0.0302 (11)	0.0592 (16)	0.0241 (10)	0.0038 (10)	−0.0075 (8)	0.0130 (10)
C102	0.0589 (16)	0.0281 (10)	0.0214 (10)	0.0033 (10)	−0.0012 (10)	−0.0045 (8)
C103	0.0414 (12)	0.0319 (11)	0.0222 (9)	−0.0078 (9)	0.0072 (8)	0.0065 (8)
C200	0.0223 (8)	0.0285 (9)	0.0102 (7)	−0.0030 (7)	0.0013 (6)	−0.0010 (6)
C201	0.0475 (13)	0.0293 (10)	0.0194 (9)	−0.0012 (9)	0.0018 (9)	0.0061 (7)
C202	0.0257 (10)	0.0606 (16)	0.0214 (10)	0.0030 (10)	0.0062 (8)	−0.0039 (9)
C203	0.0390 (12)	0.0418 (12)	0.0171 (8)	−0.0133 (10)	−0.0059 (8)	−0.0048 (8)

Geometric parameters (Å, º) top

Os1—C31	1.8906 (18)	O24—C24	1.169 (2)
Os1—C32	1.9017 (17)	O31—C31	1.146 (2)
Os1—C1	2.0143 (17)	O32—C32	1.145 (2)
Os1—C2	2.0221 (17)	C100—C103	1.521 (3)
Os1—Fe1	2.7576 (2)	C100—C102	1.522 (3)
Os1—Fe2	2.7604 (2)	C100—C101	1.528 (3)
Fe1—C11	1.8023 (17)	C101—H11A	0.98
Fe1—C13	1.8044 (18)	C101—H11B	0.98
Fe1—C12	1.8041 (18)	C101—H11C	0.98
Fe1—C14	1.9812 (17)	C102—H12A	0.98
Fe1—C24	1.9884 (18)	C102—H12B	0.98
Fe1—Fe2	2.5738 (3)	C102—H12C	0.98
Fe2—C21	1.8000 (18)	C103—H13A	0.98
Fe2—C22	1.8047 (19)	C103—H13B	0.98
Fe2—C23	1.8073 (19)	C103—H13C	0.98
Fe2—C24	1.9858 (18)	C200—C202	1.525 (3)
Fe2—C14	1.9904 (18)	C200—C203	1.524 (3)
N1—C1	1.158 (2)	C200—C201	1.524 (3)
N1—C100	1.465 (2)	C201—H21A	0.98
N2—C2	1.158 (2)	C201—H21B	0.98
N2—C200	1.468 (2)	C201—H21C	0.98
O11—C11	1.141 (2)	C202—H22A	0.98
O12—C12	1.146 (2)	C202—H22B	0.98
O13—C13	1.143 (2)	C202—H22C	0.98
O14—C14	1.169 (2)	C203—H23A	0.98
O21—C21	1.141 (2)	C203—H23B	0.98
O22—C22	1.148 (2)	C203—H23C	0.98
O23—C23	1.144 (2)

C31—Os1—C32	94.13 (7)	O12—C12—Fe1	177.30 (17)
C31—Os1—C1	91.18 (7)	O13—C13—Fe1	176.45 (16)
C32—Os1—C1	90.71 (7)	O14—C14—Fe1	140.12 (14)
C31—Os1—C2	92.23 (7)	O14—C14—Fe2	139.09 (14)
C32—Os1—C2	91.61 (7)	Fe1—C14—Fe2	80.79 (7)
C1—Os1—C2	175.73 (7)	O21—C21—Fe2	178.31 (17)
C31—Os1—Fe1	158.36 (5)	O22—C22—Fe2	175.85 (17)
C32—Os1—Fe1	107.50 (5)	O23—C23—Fe2	176.16 (17)
C1—Os1—Fe1	87.85 (5)	O24—C24—Fe2	140.02 (15)
C2—Os1—Fe1	88.03 (5)	O24—C24—Fe1	139.26 (15)
C31—Os1—Fe2	102.76 (5)	Fe2—C24—Fe1	80.73 (7)
C32—Os1—Fe2	163.11 (5)	O31—C31—Os1	179.18 (17)
C1—Os1—Fe2	88.41 (5)	O32—C32—Os1	177.73 (16)
C2—Os1—Fe2	88.33 (5)	N1—C100—C103	106.99 (16)
Fe1—Os1—Fe2	55.606 (7)	N1—C100—C102	108.10 (16)
C11—Fe1—C13	98.51 (8)	C103—C100—C102	111.69 (19)
C11—Fe1—C12	101.31 (8)	N1—C100—C101	107.07 (16)
C13—Fe1—C12	92.59 (8)	C103—C100—C101	111.83 (18)
C11—Fe1—C14	90.72 (7)	C102—C100—C101	110.9 (2)
C13—Fe1—C14	170.76 (7)	C100—C101—H11A	109.5
C12—Fe1—C14	85.99 (7)	C100—C101—H11B	109.5
C11—Fe1—C24	89.64 (7)	H11A—C101—H11B	109.5
C13—Fe1—C24	86.80 (8)	C100—C101—H11C	109.5
C12—Fe1—C24	168.99 (8)	H11A—C101—H11C	109.5
C14—Fe1—C24	92.84 (7)	H11B—C101—H11C	109.5
C11—Fe1—Fe2	110.43 (6)	C100—C102—H12A	109.5
C13—Fe1—Fe2	125.29 (6)	C100—C102—H12B	109.5
C12—Fe1—Fe2	123.81 (6)	H12A—C102—H12B	109.5
C14—Fe1—Fe2	49.76 (5)	C100—C102—H12C	109.5
C24—Fe1—Fe2	49.59 (5)	H12A—C102—H12C	109.5
C11—Fe1—Os1	172.65 (6)	H12B—C102—H12C	109.5
C13—Fe1—Os1	86.06 (6)	C100—C103—H13A	109.5
C12—Fe1—Os1	84.14 (6)	C100—C103—H13B	109.5
C14—Fe1—Os1	84.72 (5)	H13A—C103—H13B	109.5
C24—Fe1—Os1	84.85 (5)	C100—C103—H13C	109.5
Fe2—Fe1—Os1	62.253 (7)	H13A—C103—H13C	109.5
C21—Fe2—C22	98.07 (8)	H13B—C103—H13C	109.5
C21—Fe2—C23	100.44 (8)	N2—C200—C202	107.11 (16)
C22—Fe2—C23	92.04 (9)	N2—C200—C203	107.81 (16)
C21—Fe2—C24	91.61 (8)	C202—C200—C203	111.72 (18)
C22—Fe2—C24	170.28 (8)	N2—C200—C201	107.45 (15)
C23—Fe2—C24	87.07 (8)	C202—C200—C201	111.25 (19)
C21—Fe2—C14	89.04 (7)	C203—C200—C201	111.26 (18)
C22—Fe2—C14	86.64 (8)	C200—C201—H21A	109.5
C23—Fe2—C14	170.53 (8)	C200—C201—H21B	109.5
C24—Fe2—C14	92.64 (7)	H21A—C201—H21B	109.5
C21—Fe2—Fe1	110.55 (6)	C200—C201—H21C	109.5
C22—Fe2—Fe1	124.82 (6)	H21A—C201—H21C	109.5
C23—Fe2—Fe1	125.52 (6)	H21B—C201—H21C	109.5
C24—Fe2—Fe1	49.68 (5)	C200—C202—H22A	109.5
C14—Fe2—Fe1	49.45 (5)	C200—C202—H22B	109.5
C21—Fe2—Os1	172.43 (6)	H22A—C202—H22B	109.5
C22—Fe2—Os1	85.46 (6)	C200—C202—H22C	109.5
C23—Fe2—Os1	86.07 (6)	H22A—C202—H22C	109.5
C24—Fe2—Os1	84.82 (5)	H22B—C202—H22C	109.5
C14—Fe2—Os1	84.47 (5)	C200—C203—H23A	109.5
Fe1—Fe2—Os1	62.141 (7)	C200—C203—H23B	109.5
C1—N1—C100	178.22 (18)	H23A—C203—H23B	109.5
C2—N2—C200	175.33 (17)	C200—C203—H23C	109.5
N1—C1—Os1	179.22 (15)	H23A—C203—H23C	109.5
N2—C2—Os1	179.17 (15)	H23B—C203—H23C	109.5
O11—C11—Fe1	179.03 (17)

C31—Os1—Fe1—C13	−135.44 (15)	C2—Os1—Fe2—C22	137.62 (8)
C32—Os1—Fe1—C13	46.72 (8)	Fe1—Os1—Fe2—C22	−133.62 (6)
C1—Os1—Fe1—C13	136.79 (7)	C31—Os1—Fe2—C23	−46.65 (8)
C2—Os1—Fe1—C13	−44.35 (7)	C32—Os1—Fe2—C23	135.29 (19)
Fe2—Os1—Fe1—C13	−133.67 (6)	C1—Os1—Fe2—C23	−137.49 (8)
C31—Os1—Fe1—C12	131.54 (15)	C2—Os1—Fe2—C23	45.26 (8)
C32—Os1—Fe1—C12	−46.30 (8)	Fe1—Os1—Fe2—C23	134.03 (6)
C1—Os1—Fe1—C12	43.77 (7)	C31—Os1—Fe2—C24	−134.06 (7)
C2—Os1—Fe1—C12	−137.36 (7)	C32—Os1—Fe2—C24	47.88 (19)
Fe2—Os1—Fe1—C12	133.32 (6)	C1—Os1—Fe2—C24	135.09 (7)
C31—Os1—Fe1—C14	45.04 (15)	C2—Os1—Fe2—C24	−42.15 (7)
C32—Os1—Fe1—C14	−132.80 (8)	Fe1—Os1—Fe2—C24	46.61 (5)
C1—Os1—Fe1—C14	−42.73 (7)	C31—Os1—Fe2—C14	132.77 (7)
C2—Os1—Fe1—C14	136.14 (7)	C32—Os1—Fe2—C14	−45.29 (19)
Fe2—Os1—Fe1—C14	46.82 (5)	C1—Os1—Fe2—C14	41.92 (7)
C31—Os1—Fe1—C24	−48.31 (15)	C2—Os1—Fe2—C14	−135.32 (7)
C32—Os1—Fe1—C24	133.86 (8)	Fe1—Os1—Fe2—C14	−46.56 (5)
C1—Os1—Fe1—C24	−136.07 (7)	C31—Os1—Fe2—Fe1	179.33 (5)
C2—Os1—Fe1—C24	42.79 (7)	C32—Os1—Fe2—Fe1	1.27 (18)
Fe2—Os1—Fe1—C24	−46.53 (5)	C1—Os1—Fe2—Fe1	88.48 (5)
C31—Os1—Fe1—Fe2	−1.77 (14)	C2—Os1—Fe2—Fe1	−88.76 (5)
C32—Os1—Fe1—Fe2	−179.61 (6)	C11—Fe1—C14—O14	−63.4 (2)
C1—Os1—Fe1—Fe2	−89.54 (5)	C12—Fe1—C14—O14	37.9 (2)
C2—Os1—Fe1—Fe2	89.32 (5)	C24—Fe1—C14—O14	−153.1 (2)
C11—Fe1—Fe2—C21	−2.83 (9)	Fe2—Fe1—C14—O14	−180.0 (2)
C13—Fe1—Fe2—C21	−120.02 (9)	Os1—Fe1—C14—O14	122.3 (2)
C12—Fe1—Fe2—C21	117.26 (9)	C11—Fe1—C14—Fe2	116.52 (7)
C14—Fe1—Fe2—C21	69.86 (9)	C12—Fe1—C14—Fe2	−142.18 (7)
C24—Fe1—Fe2—C21	−73.82 (9)	C24—Fe1—C14—Fe2	26.85 (6)
Os1—Fe1—Fe2—C21	177.85 (6)	Os1—Fe1—C14—Fe2	−57.71 (4)
C11—Fe1—Fe2—C22	−119.14 (9)	C21—Fe2—C14—O14	61.5 (2)
C13—Fe1—Fe2—C22	123.67 (10)	C22—Fe2—C14—O14	−36.6 (2)
C12—Fe1—Fe2—C22	0.95 (10)	C24—Fe2—C14—O14	153.1 (2)
C14—Fe1—Fe2—C22	−46.45 (10)	Fe1—Fe2—C14—O14	180.0 (2)
C24—Fe1—Fe2—C22	169.87 (10)	Os1—Fe2—C14—O14	−122.4 (2)
Os1—Fe1—Fe2—C22	61.54 (7)	C21—Fe2—C14—Fe1	−118.45 (7)
C11—Fe1—Fe2—C23	117.52 (10)	C22—Fe2—C14—Fe1	143.41 (7)
C13—Fe1—Fe2—C23	0.33 (10)	C24—Fe2—C14—Fe1	−26.88 (6)
C12—Fe1—Fe2—C23	−122.39 (10)	Os1—Fe2—C14—Fe1	57.65 (4)
C14—Fe1—Fe2—C23	−169.79 (10)	C21—Fe2—C24—O24	−63.6 (2)
C24—Fe1—Fe2—C23	46.53 (10)	C23—Fe2—C24—O24	36.7 (2)
Os1—Fe1—Fe2—C23	−61.80 (8)	C14—Fe2—C24—O24	−152.8 (2)
C11—Fe1—Fe2—C24	70.99 (9)	Fe1—Fe2—C24—O24	−179.5 (2)
C13—Fe1—Fe2—C24	−46.20 (9)	Os1—Fe2—C24—O24	123.0 (2)
C12—Fe1—Fe2—C24	−168.92 (9)	C21—Fe2—C24—Fe1	115.89 (7)
C14—Fe1—Fe2—C24	143.68 (9)	C23—Fe2—C24—Fe1	−143.74 (7)
Os1—Fe1—Fe2—C24	−108.33 (6)	C14—Fe2—C24—Fe1	26.78 (6)
C11—Fe1—Fe2—C14	−72.69 (9)	Os1—Fe2—C24—Fe1	−57.42 (4)
C13—Fe1—Fe2—C14	170.12 (9)	C11—Fe1—C24—O24	61.9 (2)
C12—Fe1—Fe2—C14	47.40 (9)	C13—Fe1—C24—O24	−36.6 (2)
C24—Fe1—Fe2—C14	−143.68 (9)	C12—Fe1—C24—O24	−123.7 (4)
Os1—Fe1—Fe2—C14	107.99 (6)	C14—Fe1—C24—O24	152.6 (2)
C11—Fe1—Fe2—Os1	179.32 (6)	Fe2—Fe1—C24—O24	179.5 (2)
C13—Fe1—Fe2—Os1	62.14 (7)	Os1—Fe1—C24—O24	−122.9 (2)
C12—Fe1—Fe2—Os1	−60.59 (7)	C11—Fe1—C24—Fe2	−117.62 (7)
C14—Fe1—Fe2—Os1	−107.99 (6)	C13—Fe1—C24—Fe2	143.84 (7)
C24—Fe1—Fe2—Os1	108.33 (6)	C12—Fe1—C24—Fe2	56.7 (4)
C31—Os1—Fe2—C22	45.71 (8)	C14—Fe1—C24—Fe2	−26.92 (6)
C32—Os1—Fe2—C22	−132.35 (19)	Os1—Fe1—C24—Fe2	57.51 (4)
C1—Os1—Fe2—C22	−45.13 (7)

Acknowledgements

CE thanks the New Zealand Foundation for Research, Science and Technology for a Postdoctoral Research Fellowship (contract No. UOGX0201).

References

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Volume 62| Part 3| March 2006| Pages m478-m479

https://doi.org/10.1107/S1600536806004247

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