metal-organic compounds
Bis(tert-butyl isocyanide)-1κ2C-di-μ-carbonyl-2:3κ4C-octacarbonyl-1κ2C,2κ3C,3κ3C-triangulo-diironosmium
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
The preparation of the mixed-metal cluster, [Fe2Os(C5H9N)2(CO)10], and its 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(CNBut)n (n = 1 and 2).
Fe2Os(CO)10(CNBut)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 and by single-crystal X-ray 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(CNBut)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 = But 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].
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 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). 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
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Refinement
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All H atoms were placed in calculated positions and refined using a riding model [C—H = 0.98 Å and Uiso(H) = 1.5Ueq(C)]. The highest features in the difference map are associated with the Os atom.
Data collection: COLLECT (Nonius, 2000); cell 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
https://doi.org/10.1107/S1600536806004247/hg6301sup1.cif
contains datablocks II, global. DOI:Structure factors: contains datablock II. DOI: https://doi.org/10.1107/S1600536806004247/hg6301IIsup2.hkl
Data collection: COLLECT (Nonius, 2000); cell
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).[Fe2Os(C5H9N)2(CO)10] | F(000) = 1440 |
Mr = 748.26 | Dx = 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 |
KappaCCD diffractometer | 9945 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
CCD rotation images, thick slices scans | θmax = 35.0°, θmin = 2.4° |
Absorption correction: multi-scan (Blessing, 1995) | h = −18→18 |
Tmin = 0.197, Tmax = 0.294 | k = −20→20 |
64585 measured reflections | l = −27→28 |
10967 independent reflections |
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(Fo2) + (0.0113P)2 + 1.9594P] where P = (Fo2 + 2Fc2)/3 |
S = 1.1 | (Δ/σ)max = 0.002 |
10967 reflections | Δρmax = 1.28 e Å−3 |
317 parameters | Δρmin = −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) |
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. |
x | y | z | Uiso*/Ueq | ||
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* |
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) |
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).
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