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The title compounds, [CuFe2(C5H5)2(C9H8O2)2], (I), and [CuFe4(C5H5)4(C13H9O2)2], (II), are four-coordinate square-planar copper(II) complexes with two bidentate 1-ferrocenylbutane-1,3-dionate or 1,3-diferrocenylpropane-1,3-dionate ligands, respectively. The copper ion in (I) lies on an inversion centre, with one-half of the mol­ecule in the asymmetric unit, while in (II), there are two independent half mol­ecules in the asymmetric unit, with the copper ions also situated on inversion centres. The ferrocene substituents in (I) are in an anti arrangement. The mol­ecules assemble in the crystal structure in layers with ferrocene groups at the surface. The pairs of ferrocene substituents on each ligand in complex (II) are syn and these adopt an anti arrangement with respect to the pair on the other diketonate ligand. As found in (I), complexes assemble in a layered structure with ferrocene-coated surfaces.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270106041886/av3044sup1.cif
Contains datablocks global, I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270106041886/av3044Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270106041886/av3044IIsup3.hkl
Contains datablock II

CCDC references: 632919; 632920

Comment top

The 1,3-β-diketones 1-ferrocenylbutane-1,3-dione (HL1; FcCOCH2COCH3; Cain et al. 1961; Hennig & Gurtler, 1968; Bell et al., 1992; Zakaraia or Zakaria et al.; 1995) and 1,3-diferrocenylpropane-1,3-dione (HL2; FcCOCH2COFc; Woisetschlager et al., 1999; du Plessis et al., 1998, 2001), form coordination (Zanello et al., 1998; Che et al., 1998; Li et al., 2002) and organometallic complexes of interest in catalysis (Abiko & Wang, 1996, 1998; Cullen et al., 1991; Swarts et al., 1993; Woisetschlager et al., 2000; Vosloo et al., 2002; Conradie et al., 2005).

Copper(II) complexes of these ligands, Cu(L1)2, (I), and Cu(L2)2, (II), are readily formed upon mixing of methanol solutions of copper acetate to methanol solutions of either HL1 or HL2. These complexes have been used in the purification of the ligands (Imai & Ota, 1974; Zanello et al., 1998; du Plessis et al., 1998). Compound (I) has been further characterized by elemental analysis and cyclic voltammetry (Zanello et al., 1998). Related complexes, bis(1-ethoxycarbonyl-3-ferrocenyl-propane-1,3-dionato-O,O')copper(II), (III), and bis[1,3-bis(2-methylferrocenyl)propane-1,3-dionato-O,O']copper(II) have been prepared and characterized (Prokop et al., 1999, 2001; Abiko & Wang, 1998).

The molecular structure of (I) is shown in Fig. 1. The four coordinate copper ion lies on a crystallographic inversion centre, leading to a near square-planar CuO4 unit (Table 1). The mean plane of the two butanedionate ligands (O1/C2–C4/O2, with an r.m.s. deviation of 0.018 Å) are anti with respect to the CuO4 plane, with tilt angles of 7.80 (9)°. The two ferrocene groups are anti in the complex, with the C5–C9 cyclopentadienyl ring rotated by 26.7 (1)° with respect to the ligand plane O1/C2–C4/O2. This arrangement differs from that of complex (III), in which the ferrocenyl groups are syn (Prokop et al., 1999), whilst in the aqua complex of (III) they are anti (Prokop et al., 2001). The cyclopentadienyl rings are in an eclipsed arrangement within each ferrocene group with pseuo-torsion angles C—Cg1—Cg2—C ranging from 0.79 to 1.39° (Cg1 and Cg2 are centroids of the C5/C9 and C10/C14 cyclopentadienyl rings). The Fe to Cg1 and Cg2 distances are 1.651 (1) and 1.655 (1) Å, respectively, with a Cg1···Fe···Cg2 angle of 179.0°.

The molecules in the crystal structure of (I) assemble in layers aligned with the bc plane. The copper β-diketonates are stacked along the b axis (Cu···Cu = 7.413 Å), with methyl groups from complexes in adjacent stacks interleaved between them (Fig. 2). The complexes are connected via C—H···O interactions (C12—H···O1 = 2.684 Å) between adjacent stacks and C—H···π contacts between ferrocene groups (C13—H···centroid C5–C9 ring = 2.944 Å and C6—H···centroid C10–C14 ring = 3.099 Å) on the surface of the layers. Each ferrocene group on the surface adopts a near orthogonal arrangement with respect to a ferrocene ring on a neighbouring layer (Fe···Fe = 5.437 Å).

The molecular structure of (II) is shown in Fig. 3. The asymmetric unit consists of two independent half molecules of bis(1,3-diferrocenyl-1,3-propanedionato-O,O')copper(II) with the copper ions situated on crystallographic inversion centres, again leading to two near square-planar CuO4 units (Table 2). The two propanedionate ligand planes are tilted in an anti arrangement with tilt angles of the two ligand planes (O1/C41–C43/O2 with an r.m.s. deviation of 0.016 Å and O3/C44–C46/O4 with an r.m.s. deviation of 0.012 Å) of 6.5 (2) and 5.3 (2)° with respect to the Cu1O4 and Cu2O4 planes, respectively. Within each copper complex, the two ferrocene groups on each propanedionate ligand are in a syn arrangment and these are anti to the two ferrocene substituents on the other ligand (Fig. 3). The cyclopentadienyl rings on the ferrocene groups attached to the Cu1 complex are in a near eclipsed arrangement with average pseudo-torsion angles C—Cg3—Cg4—C for ferrocene Fe3 and Fe4 of 13.3 and 14.3°, respectively (Cg3 and Cg4 are the centroids of either the Fe3 or Fe4 cyclopentadienyl rings). The Fe3···Cg and Fe4···Cg distances are 1.662 (2) and 1.652 (2) Å, respectively, for Cg3, and 1.656 (2) and 1.649(2) Å for Cg4, with Cg3···Fe···Cg4 angles of 179.7 and 178.2°. A ferrocene group, Fe1, attached to the Cu2 complex contains a disordered cyclopentadienyl ring in either a near staggered (major component, C1–C5; average pseudo-torsion angle C—Cg5—Cg6—C = 25.5°; Cg5 and Cg6 are centroids of either the Fe3 or Fe4 cyclopentadienyl rings) or a near eclipsed arrangement (minor component, C47–C51; average pseudo-torsion angles C—Cg5—Cg6—C = 7.0°), whilst those on Fe2 are eclipsed (average pseudo-torsion angles C—Cg5—Cg6—C = 7.5°). The Fe1···Cg and Fe2···Cg distances are 1.653 (2) and 1.679 (5) Å, respectively, for Cg5, and 1.649 (2) and 1.655 (2) Å for Cg6, with Cg5.·Fe..Cg6 angles of 179.8 and 179.5°. The ferrocene groups are slightly tilted with respect to the ligand propanedionate mean planes [14.9 (1)° for the C26–C30 ring and 8.1 (2)° for the C36–C40 ring with resepct to the O12/C41–C43 plane, and 13.4 (1)° for the C11/C15 ring and 6.8 (2)° for the C1–C5 ring with respect to the O3/O4/C44–C46 plane).

The copper complexes assemble in the crystal structure of (II) via ferrocene C—H···O and C—H···π interactions (Table 3). Four complexes are arranged in a rectangular arrangement of four pairs of ferrocene groups (Fig. 4a). Within this arrangement is a 44 Å 3 solvent-accessible void with no residual electron density (PLATON; Spek, 2003). These arrangements continue in the bc plane, giving a layered structure with interdigitated ferrocene groups on the surfaces of each layer (Fig. 4b).

Experimental top

Complex (I)<schemer id="scheme1"> was prepared by mixing a warm solution of H<it>L</it><inf>1</inf> (500&emsp14;mg, 1.85&emsp14;mmol, in 20&emsp14;ml methanol) with a warm solution of copper(II) acetate dihydrate (176&emsp14;mg, 0.88&emsp14;mmol, in 20&emsp14;ml methanol). A brown&ndash;gold precipitate formed which was filtered off, washed with methanol and dried to give 482&emsp14;mg of (I)<schemer id="scheme1"> (91% yield). Red crystals of (I)<schemer id="scheme1"> were grown by vapour diffusion of ethanol into a benzene solution. Complex (II)<schemer id="scheme1"> was prepared by mixing a warm solution of H<it>L</it><inf>2</inf> (371&emsp14;mg, 0.84&emsp14;mmol, in 20&emsp14;ml methanol) with a warm solution of copper(II) acetate dihydrate (84&emsp14;mg, 0.42&emsp14;mmol, in 20&emsp14;ml methanol). The solution was refuxed for 30&emsp14;min, cooled to room temperature, filtered and washed with ethyl acetate to give 182&emsp14;mg of a red crystalline precipitate (46% yield). Red crystals of (II)<schemer id="scheme1"> were grown by vapour diffusion of hexane into a benzene solution.

Refinement top

H atoms were placed in calculated positions and refined using a riding model (C—H = 0.93–0.97 Å), with Uiso(H) values of 1.2 or 1.5 times Ueq(C) for aromatic and methyl groups, respectively. Methyl groups were rotated to fit the H-atom positions to the observed electron density. Electron density difference maps in structure (II) indicated disorder of a cyclopentadienyl ring attached to Fe1. A two-site disorder model was constructed and refined to give a site occupation factor of 0.67 (2) for C6–C10 and 0.33 (2) for C47–C51. The final refinement included restraints on the displacement parameters of C6–C10 and C47–C51 (SHELX, SIMU, DELU; Sheldrick, 1997).

Computing details top

For both compounds, data collection: SMART (Siemens, 1995); cell refinement: SAINT (Siemens, 1995); data reduction: SAINT; 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).

Figures top
[Figure 1] Fig. 1. : The structure of (I), showing 50% probability displacement ellipsoids for non-H atoms. Unlabelled atoms are related to labelled atoms by the symmetry code (1/2 − x,1/2 − y,1 − z).
[Figure 2] Fig. 2. : The arrangement of complex (I) in the crystal: (a) view along the b axis; (b) view along the c axis.
[Figure 3] Fig. 3. : The structure of (II), showing 50% probability displacement ellipsoids for non-H atoms: (a) the Cu1 complex; (b) the Cu2 complex. Unlabelled atoms are related to labelled atoms by the symmetry codes (1 − x, 1 − y, 1 − z) for the Cu1 complex and (1 − x, −y, −z) for the Cu2 complex.
[Figure 4] Fig. 4. : The arrangement of complex (II) in the crystal: (a) view along the a axis; (b) view along the b axis.
(I) Bis(1-ferrocenylbutane-1,3-dionato-κ2O,O')copper(II) top
Crystal data top
[CuFe2(C5H5)2(C9H8O2)2]F(000) = 1228
Mr = 601.73Dx = 1.723 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 29.6410 (3) ÅCell parameters from 4092 reflections
b = 7.4132 (1) Åθ = 1.4–27.5°
c = 10.5656 (2) ŵ = 2.18 mm1
β = 92.109 (1)°T = 203 K
V = 2320.06 (6) Å3Plate, red
Z = 40.38 × 0.28 × 0.03 mm
Data collection top
Siemens SMART CCD area-detector
diffractometer
2558 independent reflections
Radiation source: fine-focus sealed tube2195 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
ω scansθmax = 27.5°, θmin = 1.4°
Absorption correction: multi-scan
SADABS; Sheldrick, 1997
h = 3835
Tmin = 0.655, Tmax = 0.952k = 98
7126 measured reflectionsl = 1313
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.100H-atom parameters constrained
S = 1.21 w = 1/[σ2(Fo2) + (0.0525P)2 + 1.6252P]
where P = (Fo2 + 2Fc2)/3
2558 reflections(Δ/σ)max < 0.001
161 parametersΔρmax = 0.50 e Å3
0 restraintsΔρmin = 0.69 e Å3
Crystal data top
[CuFe2(C5H5)2(C9H8O2)2]V = 2320.06 (6) Å3
Mr = 601.73Z = 4
Monoclinic, C2/cMo Kα radiation
a = 29.6410 (3) ŵ = 2.18 mm1
b = 7.4132 (1) ÅT = 203 K
c = 10.5656 (2) Å0.38 × 0.28 × 0.03 mm
β = 92.109 (1)°
Data collection top
Siemens SMART CCD area-detector
diffractometer
2558 independent reflections
Absorption correction: multi-scan
SADABS; Sheldrick, 1997
2195 reflections with I > 2σ(I)
Tmin = 0.655, Tmax = 0.952Rint = 0.021
7126 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0320 restraints
wR(F2) = 0.100H-atom parameters constrained
S = 1.21Δρmax = 0.50 e Å3
2558 reflectionsΔρmin = 0.69 e Å3
161 parameters
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
xyzUiso*/Ueq
Cu0.25000.25000.50000.02167 (14)
Fe0.087286 (11)0.22994 (4)0.17950 (3)0.01826 (13)
O10.27841 (6)0.1878 (3)0.34736 (17)0.0287 (4)
O20.19080 (6)0.1852 (3)0.43599 (16)0.0263 (4)
C10.28831 (9)0.1382 (4)0.1310 (3)0.0315 (6)
H1A0.30270.25380.11750.047*
H1B0.27060.10470.05550.047*
H1C0.31120.04720.14850.047*
C20.25785 (8)0.1518 (3)0.2417 (2)0.0232 (5)
C30.21138 (8)0.1272 (3)0.2241 (2)0.0248 (5)
H30.200000.10050.14200.030*
C40.18079 (8)0.1398 (3)0.3210 (2)0.0212 (5)
C50.13259 (8)0.0958 (3)0.2965 (2)0.0207 (5)
C60.09588 (8)0.1623 (3)0.3677 (2)0.0232 (5)
H60.09820.24250.43650.028*
C70.05528 (8)0.0857 (3)0.3160 (2)0.0257 (5)
H70.02610.10660.34460.031*
C80.06660 (8)0.0285 (3)0.2132 (2)0.0277 (6)
H80.04610.09660.16290.033*
C90.11413 (8)0.0223 (3)0.1995 (2)0.0239 (5)
H90.13050.08380.13840.029*
C100.04393 (10)0.4292 (4)0.1163 (3)0.0337 (6)
H100.01500.45300.14570.040*
C110.08503 (11)0.5040 (3)0.1650 (2)0.0369 (7)
H110.08800.58520.23310.044*
C120.12087 (10)0.4361 (4)0.0938 (3)0.0333 (6)
H120.15160.46510.10530.040*
C130.10174 (9)0.3159 (4)0.0016 (2)0.0304 (6)
H130.11780.25020.05810.036*
C140.05431 (9)0.3124 (4)0.0154 (2)0.0300 (6)
H140.03340.24440.03380.036*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu0.0166 (2)0.0274 (3)0.0206 (2)0.00069 (15)0.00472 (17)0.00207 (15)
Fe0.0189 (2)0.01796 (19)0.0176 (2)0.00056 (12)0.00378 (14)0.00091 (12)
O10.0200 (9)0.0385 (10)0.0272 (9)0.0004 (8)0.0034 (7)0.0050 (8)
O20.0190 (8)0.0368 (10)0.0226 (8)0.0031 (7)0.0050 (7)0.0038 (7)
C10.0265 (13)0.0375 (15)0.0308 (13)0.0021 (11)0.0028 (11)0.0043 (11)
C20.0263 (12)0.0211 (11)0.0221 (11)0.0014 (9)0.0004 (9)0.0019 (9)
C30.0241 (12)0.0286 (13)0.0214 (12)0.0000 (10)0.0054 (9)0.0023 (9)
C40.0220 (11)0.0180 (11)0.0230 (11)0.0004 (9)0.0066 (9)0.0019 (9)
C50.0223 (12)0.0197 (11)0.0197 (11)0.0011 (9)0.0062 (9)0.0041 (9)
C60.0225 (12)0.0279 (12)0.0190 (11)0.0017 (9)0.0038 (9)0.0054 (9)
C70.0213 (12)0.0274 (13)0.0282 (12)0.0028 (10)0.0018 (10)0.0081 (10)
C80.0258 (13)0.0221 (12)0.0343 (13)0.0057 (10)0.0118 (10)0.0038 (10)
C90.0269 (12)0.0165 (11)0.0275 (12)0.0007 (9)0.0077 (10)0.0003 (9)
C100.0382 (15)0.0339 (15)0.0288 (13)0.0155 (12)0.0014 (11)0.0108 (11)
C110.067 (2)0.0173 (13)0.0265 (14)0.0031 (12)0.0055 (14)0.0026 (10)
C120.0351 (14)0.0303 (14)0.0339 (14)0.0097 (11)0.0051 (11)0.0121 (11)
C130.0367 (15)0.0345 (14)0.0202 (12)0.0033 (12)0.0035 (10)0.0061 (10)
C140.0325 (14)0.0344 (14)0.0223 (12)0.0023 (11)0.0104 (10)0.0065 (11)
Geometric parameters (Å, º) top
Cu—O1i1.9033 (18)C3—H30.9400
Cu—O11.9033 (18)C4—C51.479 (3)
Cu—O21.9182 (16)C5—C61.433 (3)
Cu—O2i1.9182 (16)C5—C91.440 (3)
Fe—C112.039 (3)C6—C71.422 (3)
Fe—C92.040 (2)C6—H60.9400
Fe—C132.045 (3)C7—C81.427 (4)
Fe—C82.047 (3)C7—H70.9400
Fe—C52.049 (2)C8—C91.422 (4)
Fe—C142.052 (2)C8—H80.9400
Fe—C122.052 (3)C9—H90.9400
Fe—C102.054 (3)C10—C141.416 (4)
Fe—C72.056 (2)C10—C111.418 (4)
Fe—C62.057 (2)C10—H100.9400
O1—C21.280 (3)C11—C121.416 (4)
O2—C41.285 (3)C11—H110.9400
C1—C21.507 (3)C12—C131.422 (4)
C1—H1A0.9700C12—H120.9400
C1—H1B0.9700C13—C141.419 (4)
C1—H1C0.9700C13—H130.9400
C2—C31.395 (3)C14—H140.9400
C3—C41.396 (3)
O1i—Cu—O1180C4—C3—H3118.0
O1i—Cu—O286.09 (7)O2—C4—C3125.3 (2)
O1—Cu—O293.91 (7)O2—C4—C5114.3 (2)
O1i—Cu—O2i93.91 (7)C3—C4—C5120.4 (2)
O1—Cu—O2i86.09 (7)C6—C5—C9107.8 (2)
O2—Cu—O2i180C6—C5—C4125.4 (2)
C11—Fe—C9158.90 (11)C9—C5—C4126.7 (2)
C11—Fe—C1368.12 (11)C6—C5—Fe69.90 (13)
C9—Fe—C13106.68 (11)C9—C5—Fe69.03 (13)
C11—Fe—C8159.53 (12)C4—C5—Fe127.31 (16)
C9—Fe—C840.73 (10)C7—C6—C5108.0 (2)
C13—Fe—C8121.74 (11)C7—C6—Fe69.71 (13)
C11—Fe—C5123.23 (10)C5—C6—Fe69.26 (13)
C9—Fe—C541.26 (9)C7—C6—H6126.0
C13—Fe—C5123.44 (10)C5—C6—H6126.0
C8—Fe—C568.57 (9)Fe—C6—H6126.6
C11—Fe—C1468.05 (11)C6—C7—C8108.1 (2)
C9—Fe—C14122.18 (11)C6—C7—Fe69.85 (13)
C13—Fe—C1440.53 (11)C8—C7—Fe69.33 (14)
C8—Fe—C14106.83 (10)C6—C7—H7126.0
C5—Fe—C14159.34 (11)C8—C7—H7126.0
C11—Fe—C1240.51 (11)Fe—C7—H7126.4
C9—Fe—C12122.32 (11)C9—C8—C7108.6 (2)
C13—Fe—C1240.62 (11)C9—C8—Fe69.35 (14)
C8—Fe—C12157.97 (12)C7—C8—Fe69.97 (14)
C5—Fe—C12108.05 (10)C9—C8—H8125.7
C14—Fe—C1268.23 (11)C7—C8—H8125.7
C11—Fe—C1040.54 (11)Fe—C8—H8126.6
C9—Fe—C10158.46 (11)C8—C9—C5107.4 (2)
C13—Fe—C1068.07 (11)C8—C9—Fe69.92 (14)
C8—Fe—C10122.83 (11)C5—C9—Fe69.71 (13)
C5—Fe—C10159.03 (11)C8—C9—H9126.3
C14—Fe—C1040.35 (11)C5—C9—H9126.3
C12—Fe—C1068.20 (12)Fe—C9—H9125.7
C11—Fe—C7123.83 (11)C14—C10—C11107.7 (2)
C9—Fe—C768.82 (10)C14—C10—Fe69.75 (14)
C13—Fe—C7157.65 (11)C11—C10—Fe69.16 (14)
C8—Fe—C740.70 (11)C14—C10—H10126.1
C5—Fe—C768.49 (10)C11—C10—H10126.1
C14—Fe—C7122.01 (11)Fe—C10—H10126.5
C12—Fe—C7160.20 (11)C10—C11—C12108.6 (2)
C10—Fe—C7107.65 (11)C10—C11—Fe70.30 (15)
C11—Fe—C6108.56 (10)C12—C11—Fe70.27 (15)
C9—Fe—C669.05 (10)C10—C11—H11125.7
C13—Fe—C6160.32 (10)C12—C11—H11125.7
C8—Fe—C668.34 (10)Fe—C11—H11125.3
C5—Fe—C640.84 (9)C11—C12—C13107.4 (2)
C14—Fe—C6158.04 (11)C11—C12—Fe69.22 (15)
C12—Fe—C6124.27 (10)C13—C12—Fe69.39 (15)
C10—Fe—C6122.92 (11)C11—C12—H12126.3
C7—Fe—C640.44 (9)C13—C12—H12126.3
C2—O1—Cu125.33 (16)Fe—C12—H12126.6
C4—O2—Cu125.14 (16)C14—C13—C12108.2 (2)
C2—C1—H1A109.5C14—C13—Fe70.00 (14)
C2—C1—H1B109.5C12—C13—Fe69.99 (15)
H1A—C1—H1B109.5C14—C13—H13125.9
C2—C1—H1C109.5C12—C13—H13125.9
H1A—C1—H1C109.5Fe—C13—H13125.7
H1B—C1—H1C109.5C10—C14—C13108.0 (2)
O1—C2—C3125.4 (2)C10—C14—Fe69.90 (14)
O1—C2—C1114.3 (2)C13—C14—Fe69.47 (14)
C3—C2—C1120.3 (2)C10—C14—H14126.0
C2—C3—C4123.9 (2)C13—C14—H14126.0
C2—C3—H3118.0Fe—C14—H14126.2
Symmetry code: (i) x+1/2, y+1/2, z+1.
(II) Bis(1,3-diferrocenylpropane-1,3-dionateo-κ2O,O')copper(II) top
Crystal data top
[CuFe4(C5H5)4(C13H9O2)2]Z = 2
Mr = 941.70F(000) = 958
Triclinic, P1Dx = 1.653 Mg m3
a = 11.9182 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.8881 (1) ÅCell parameters from 8192 reflections
c = 12.9097 (1) Åθ = 1.6–26.4°
α = 89.670 (1)°µ = 2.10 mm1
β = 78.617 (1)°T = 200 K
γ = 76.987 (1)°Prism, brown
V = 1892.49 (4) Å30.16 × 0.14 × 0.1 mm
Data collection top
Siemens SMART CCD area-detector
diffractometer
7556 independent reflections
Radiation source: fine-focus sealed tube5859 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
ω scansθmax = 26.4°, θmin = 1.6°
Absorption correction: multi-scan
SADABS; Sheldrick, 1997
h = 1414
Tmin = 0.650, Tmax = 0.803k = 1516
17654 measured reflectionsl = 1616
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.127H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0684P)2 + 0.6255P]
where P = (Fo2 + 2Fc2)/3
7556 reflections(Δ/σ)max = 0.001
545 parametersΔρmax = 0.95 e Å3
140 restraintsΔρmin = 1.23 e Å3
Crystal data top
[CuFe4(C5H5)4(C13H9O2)2]γ = 76.987 (1)°
Mr = 941.70V = 1892.49 (4) Å3
Triclinic, P1Z = 2
a = 11.9182 (2) ÅMo Kα radiation
b = 12.8881 (1) ŵ = 2.10 mm1
c = 12.9097 (1) ÅT = 200 K
α = 89.670 (1)°0.16 × 0.14 × 0.1 mm
β = 78.617 (1)°
Data collection top
Siemens SMART CCD area-detector
diffractometer
7556 independent reflections
Absorption correction: multi-scan
SADABS; Sheldrick, 1997
5859 reflections with I > 2σ(I)
Tmin = 0.650, Tmax = 0.803Rint = 0.038
17654 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.048140 restraints
wR(F2) = 0.127H-atom parameters constrained
S = 1.07Δρmax = 0.95 e Å3
7556 reflectionsΔρmin = 1.23 e Å3
545 parameters
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. One disordered ferrocene refined with a two site model atoms, C6/C10 (occupancy 0.6254) and C47/C51 (0.3746). Anisotropic Thermal parameters for these atoms were constrained using the SHELX SIMU and DELU keywords.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C10.1670 (3)0.1357 (3)0.1482 (3)0.0231 (8)
C20.0875 (3)0.2004 (3)0.1882 (3)0.0250 (8)
C30.1535 (3)0.3059 (3)0.1970 (3)0.0239 (8)
C40.2739 (3)0.3077 (3)0.1630 (3)0.0216 (8)
C50.2833 (3)0.2016 (3)0.1318 (3)0.0183 (8)
C60.2178 (13)0.2593 (8)0.4331 (7)0.035 (3)0.674 (18)
C70.1135 (9)0.1800 (11)0.4420 (8)0.031 (3)0.674 (18)
C80.1434 (10)0.0833 (10)0.4074 (12)0.030 (3)0.674 (18)
C90.2679 (12)0.1057 (10)0.3795 (8)0.035 (3)0.674 (18)
C100.3120 (8)0.2141 (12)0.3943 (8)0.036 (3)0.674 (18)
C110.7189 (3)0.2881 (3)0.0658 (3)0.0218 (8)
C120.7300 (3)0.3994 (3)0.0896 (3)0.0209 (8)
C130.8481 (3)0.4432 (3)0.0972 (3)0.0228 (8)
C140.9111 (3)0.3611 (3)0.0801 (3)0.0203 (8)
C150.8313 (3)0.2646 (3)0.0611 (3)0.0198 (8)
C160.6480 (4)0.3225 (3)0.3400 (3)0.0313 (9)
C170.7615 (4)0.3797 (3)0.3539 (3)0.0294 (9)
C180.8362 (4)0.3069 (3)0.3403 (3)0.0291 (9)
C190.7693 (4)0.2054 (3)0.3186 (3)0.0299 (9)
C200.6531 (4)0.2149 (3)0.3185 (3)0.0314 (10)
C210.2073 (4)0.1949 (3)0.4044 (3)0.0332 (10)
C220.1520 (4)0.1751 (3)0.3214 (3)0.0290 (9)
C230.2385 (4)0.1544 (3)0.2266 (3)0.0297 (9)
C240.3464 (4)0.1619 (3)0.2506 (4)0.0358 (10)
C250.3278 (4)0.1865 (3)0.3609 (4)0.0379 (11)
C260.1568 (3)0.4155 (3)0.1907 (3)0.0250 (9)
C270.0926 (3)0.4391 (3)0.2958 (3)0.0260 (9)
C280.1722 (3)0.4540 (3)0.3616 (3)0.0238 (8)
C290.2865 (3)0.4388 (3)0.2950 (3)0.0207 (8)
C300.2769 (3)0.4143 (3)0.1892 (3)0.0225 (8)
C310.8545 (4)0.0258 (3)0.1587 (4)0.0374 (11)
C320.7322 (5)0.0586 (3)0.1701 (4)0.0442 (13)
C330.6841 (4)0.0964 (4)0.2757 (4)0.0424 (12)
C340.7783 (5)0.0855 (3)0.3299 (4)0.0375 (11)
C350.8835 (4)0.0416 (3)0.2575 (4)0.0366 (11)
C360.7423 (3)0.3106 (3)0.1191 (3)0.0225 (8)
C370.8657 (4)0.2676 (3)0.0829 (3)0.0251 (9)
C380.9230 (3)0.2727 (3)0.1681 (3)0.0242 (8)
C390.8375 (3)0.3192 (3)0.2585 (3)0.0219 (8)
C400.7239 (3)0.3436 (3)0.2286 (3)0.0202 (8)
C410.6127 (3)0.3921 (3)0.3008 (3)0.0193 (8)
C420.5056 (3)0.4008 (3)0.2685 (3)0.0236 (8)
C430.3948 (3)0.4418 (3)0.3338 (3)0.0198 (8)
C440.6096 (3)0.2083 (3)0.0577 (3)0.0190 (8)
C450.5013 (3)0.2356 (3)0.0884 (3)0.0237 (8)
C460.3924 (3)0.1652 (3)0.0908 (3)0.0192 (8)
C470.151 (3)0.243 (2)0.4415 (14)0.034 (5)0.326 (18)
C480.0938 (19)0.139 (2)0.4245 (17)0.028 (5)0.326 (18)
C490.191 (3)0.0859 (18)0.395 (2)0.034 (5)0.326 (18)
C500.299 (2)0.159 (3)0.3811 (19)0.041 (6)0.326 (18)
C510.274 (3)0.262 (2)0.410 (2)0.043 (6)0.326 (18)
Cu10.50000.50000.50000.01900 (16)
Cu20.50000.00000.00000.01808 (16)
Fe10.20172 (5)0.19969 (4)0.28757 (4)0.02069 (14)
Fe20.77108 (5)0.31812 (4)0.20619 (4)0.01940 (14)
Fe30.22549 (5)0.30393 (4)0.28993 (4)0.02114 (14)
Fe40.80038 (5)0.18324 (4)0.20588 (4)0.01956 (14)
O10.6235 (2)0.4237 (2)0.3913 (2)0.0231 (6)
O20.3790 (2)0.4832 (2)0.4273 (2)0.0231 (6)
O30.6232 (2)0.11743 (19)0.0237 (2)0.0229 (6)
O40.3774 (2)0.06927 (19)0.0592 (2)0.0222 (6)
H10.14700.06350.13500.028*
H20.00610.17780.20570.030*
H30.12250.36370.22110.029*
H40.33600.36660.16100.026*
H60.22270.33010.45040.041*0.674 (18)
H70.03780.18930.46640.038*0.674 (18)
H80.09170.01810.40360.036*0.674 (18)
H90.31280.05670.35550.042*0.674 (18)
H100.39090.24940.38040.043*0.674 (18)
H120.67000.43580.09830.025*
H130.87910.51360.11110.027*
H140.99030.36860.08090.024*
H150.84970.19870.04810.024*
H160.58210.35080.34430.038*
H170.78250.45120.36900.035*
H180.91510.32260.34470.035*
H190.79720.14370.30670.036*
H200.59140.16070.30650.038*
H210.17080.21060.47490.040*
H220.07280.17560.32790.035*
H230.22600.13860.16020.036*
H240.41760.15250.20270.043*
H250.38480.19540.39780.045*
H260.12570.40290.13250.030*
H270.01240.44420.31830.031*
H280.15310.47040.43390.029*
H300.33810.40010.13030.027*
H310.90740.00160.09680.045*
H320.68990.05600.11720.053*
H330.60500.12350.30450.051*
H340.77190.10410.40070.045*
H350.95870.02580.27220.044*
H360.68460.31630.07900.027*
H370.90200.24080.01490.030*
H381.00330.24950.16550.029*
H390.85200.33170.32500.026*
H420.50770.37820.19970.028*
H450.50150.30500.10860.028*
H470.11160.29380.47070.041*0.326 (18)
H480.01380.11040.43030.033*0.326 (18)
H490.18230.01290.38750.041*0.326 (18)
H500.37240.14530.35750.049*0.326 (18)
H510.32760.32690.40810.052*0.326 (18)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.019 (2)0.023 (2)0.028 (2)0.0042 (15)0.0085 (16)0.0017 (16)
C20.019 (2)0.027 (2)0.030 (2)0.0038 (16)0.0072 (17)0.0053 (16)
C30.022 (2)0.0214 (19)0.030 (2)0.0074 (15)0.0067 (17)0.0042 (16)
C40.019 (2)0.0212 (19)0.024 (2)0.0033 (15)0.0056 (16)0.0014 (15)
C50.0149 (19)0.0189 (18)0.0201 (19)0.0007 (14)0.0050 (15)0.0034 (14)
C60.047 (8)0.029 (4)0.019 (5)0.006 (6)0.001 (6)0.001 (3)
C70.019 (5)0.049 (8)0.024 (5)0.002 (5)0.005 (3)0.011 (5)
C80.030 (6)0.028 (4)0.028 (5)0.010 (4)0.013 (5)0.006 (3)
C90.039 (6)0.046 (6)0.026 (4)0.021 (6)0.011 (5)0.000 (5)
C100.024 (4)0.051 (7)0.030 (5)0.006 (4)0.017 (3)0.004 (6)
C110.0172 (19)0.0225 (19)0.025 (2)0.0011 (15)0.0059 (16)0.0015 (15)
C120.019 (2)0.0180 (18)0.026 (2)0.0028 (15)0.0056 (16)0.0020 (15)
C130.021 (2)0.0195 (19)0.027 (2)0.0018 (15)0.0090 (16)0.0007 (16)
C140.0135 (19)0.025 (2)0.0204 (19)0.0012 (15)0.0027 (15)0.0034 (15)
C150.0178 (19)0.0219 (19)0.0204 (19)0.0052 (15)0.0050 (15)0.0063 (15)
C160.023 (2)0.040 (2)0.029 (2)0.0065 (18)0.0015 (18)0.0052 (19)
C170.035 (2)0.028 (2)0.025 (2)0.0023 (18)0.0099 (18)0.0064 (17)
C180.026 (2)0.036 (2)0.026 (2)0.0057 (18)0.0099 (18)0.0000 (18)
C190.037 (3)0.025 (2)0.027 (2)0.0101 (18)0.0038 (19)0.0029 (17)
C200.024 (2)0.031 (2)0.032 (2)0.0037 (17)0.0013 (18)0.0048 (18)
C210.051 (3)0.027 (2)0.028 (2)0.013 (2)0.017 (2)0.0093 (18)
C220.036 (2)0.026 (2)0.032 (2)0.0151 (18)0.0147 (19)0.0060 (17)
C230.041 (3)0.022 (2)0.029 (2)0.0066 (18)0.0156 (19)0.0003 (17)
C240.032 (3)0.026 (2)0.048 (3)0.0006 (18)0.012 (2)0.003 (2)
C250.041 (3)0.026 (2)0.055 (3)0.0023 (19)0.033 (2)0.006 (2)
C260.026 (2)0.0216 (19)0.034 (2)0.0059 (16)0.0195 (18)0.0023 (16)
C270.018 (2)0.024 (2)0.040 (2)0.0047 (16)0.0152 (18)0.0036 (17)
C280.019 (2)0.0215 (19)0.031 (2)0.0009 (15)0.0081 (17)0.0033 (16)
C290.0174 (19)0.0202 (18)0.028 (2)0.0050 (15)0.0110 (16)0.0002 (15)
C300.021 (2)0.0239 (19)0.026 (2)0.0068 (16)0.0114 (16)0.0037 (16)
C310.053 (3)0.021 (2)0.036 (3)0.007 (2)0.003 (2)0.0017 (18)
C320.062 (3)0.031 (2)0.060 (3)0.026 (2)0.043 (3)0.015 (2)
C330.024 (2)0.033 (2)0.068 (4)0.0089 (19)0.002 (2)0.014 (2)
C340.059 (3)0.027 (2)0.027 (2)0.012 (2)0.008 (2)0.0046 (18)
C350.034 (3)0.024 (2)0.055 (3)0.0048 (18)0.020 (2)0.010 (2)
C360.023 (2)0.0213 (19)0.025 (2)0.0051 (15)0.0077 (16)0.0023 (15)
C370.023 (2)0.029 (2)0.022 (2)0.0045 (16)0.0043 (16)0.0035 (16)
C380.019 (2)0.0225 (19)0.029 (2)0.0040 (15)0.0022 (16)0.0052 (16)
C390.020 (2)0.0217 (19)0.027 (2)0.0074 (15)0.0103 (16)0.0015 (16)
C400.019 (2)0.0187 (18)0.024 (2)0.0040 (15)0.0092 (16)0.0018 (15)
C410.022 (2)0.0168 (18)0.0216 (19)0.0056 (15)0.0081 (16)0.0029 (15)
C420.020 (2)0.032 (2)0.020 (2)0.0050 (16)0.0081 (16)0.0018 (16)
C430.021 (2)0.0185 (18)0.024 (2)0.0070 (15)0.0104 (16)0.0004 (15)
C440.0175 (19)0.0188 (18)0.0211 (19)0.0031 (14)0.0060 (15)0.0035 (15)
C450.019 (2)0.0181 (19)0.034 (2)0.0023 (15)0.0092 (17)0.0084 (16)
C460.0190 (19)0.0218 (19)0.0188 (19)0.0067 (15)0.0059 (15)0.0014 (15)
C470.050 (12)0.035 (9)0.019 (7)0.013 (10)0.003 (10)0.021 (8)
C480.022 (7)0.045 (12)0.013 (8)0.007 (8)0.010 (6)0.005 (8)
C490.056 (14)0.018 (7)0.031 (10)0.009 (9)0.018 (15)0.003 (7)
C500.026 (9)0.055 (15)0.043 (11)0.012 (10)0.008 (8)0.008 (14)
C510.044 (12)0.032 (9)0.038 (13)0.021 (9)0.008 (11)0.013 (9)
Cu10.0165 (3)0.0219 (3)0.0204 (3)0.0041 (3)0.0081 (3)0.0002 (3)
Cu20.0147 (3)0.0176 (3)0.0230 (3)0.0029 (2)0.0073 (3)0.0051 (2)
Fe10.0179 (3)0.0212 (3)0.0221 (3)0.0019 (2)0.0053 (2)0.0044 (2)
Fe20.0159 (3)0.0195 (3)0.0222 (3)0.0015 (2)0.0053 (2)0.0044 (2)
Fe30.0202 (3)0.0208 (3)0.0253 (3)0.0049 (2)0.0109 (2)0.0017 (2)
Fe40.0181 (3)0.0194 (3)0.0223 (3)0.0036 (2)0.0077 (2)0.0020 (2)
O10.0183 (14)0.0280 (14)0.0242 (14)0.0038 (11)0.0084 (11)0.0007 (11)
O20.0186 (14)0.0275 (14)0.0237 (14)0.0040 (11)0.0071 (11)0.0016 (11)
O30.0179 (14)0.0219 (14)0.0296 (15)0.0042 (11)0.0066 (11)0.0048 (11)
O40.0159 (14)0.0198 (13)0.0315 (15)0.0031 (10)0.0078 (11)0.0084 (11)
Geometric parameters (Å, º) top
C6—C101.386 (14)C14—C151.437 (5)
C6—C71.405 (12)C14—H140.9300
C6—Fe12.053 (9)O4—C461.285 (4)
C6—H60.9300C13—C121.416 (5)
C7—C81.418 (15)C13—H130.9300
C7—Fe12.050 (10)C4—C31.410 (5)
C7—H70.9300C4—C51.446 (5)
C8—C91.419 (12)C4—H40.9300
C8—Fe12.064 (13)C46—C451.402 (5)
C8—H80.9300C46—C51.480 (5)
C9—C101.403 (13)C12—C111.447 (5)
C9—Fe12.078 (10)C12—H120.9300
C9—H90.9300C30—C261.424 (5)
C10—Fe12.065 (9)C30—C291.437 (5)
C10—H100.9300C30—H300.9300
C47—C481.39 (2)C44—C451.396 (5)
C47—C511.40 (3)C44—C111.488 (5)
C47—Fe12.069 (17)C15—C111.430 (5)
C47—H470.9300C15—H150.9300
C48—C491.46 (3)C41—C421.400 (5)
C48—Fe12.01 (2)C41—C401.471 (5)
C48—H480.9300C36—C371.433 (5)
C49—C501.39 (3)C36—C401.439 (5)
C49—Fe11.99 (3)C36—H360.9300
C49—H490.9300C45—H450.9300
C50—C511.45 (3)C5—C11.429 (5)
C50—Fe11.97 (2)C26—C271.418 (6)
C50—H500.9300C26—H260.9300
C51—Fe12.02 (3)C2—C11.421 (5)
C51—H510.9300C2—C31.426 (5)
Cu1—O1i1.911 (3)C2—H20.9300
Cu1—O11.911 (3)C40—C391.447 (5)
Cu1—O2i1.919 (2)C29—C281.433 (5)
Cu1—O21.919 (2)C29—C431.482 (5)
Cu2—O4ii1.912 (2)C3—H30.9300
Cu2—O41.912 (2)C43—C421.408 (5)
Cu2—O31.926 (3)C1—H10.9300
Cu2—O3ii1.926 (3)C19—C201.418 (6)
Fe4—C312.043 (4)C19—C181.427 (6)
Fe4—C382.043 (4)C19—H190.9300
Fe4—C342.044 (4)C39—C381.423 (5)
Fe4—C332.044 (4)C39—H390.9300
Fe4—C372.045 (4)C21—C221.415 (6)
Fe4—C352.047 (4)C21—C251.415 (7)
Fe4—C322.049 (4)C21—H210.9300
Fe4—C362.050 (4)C42—H420.9300
Fe4—C392.052 (4)C34—C351.410 (7)
Fe4—C402.060 (4)C34—C331.416 (7)
Fe2—C122.035 (4)C34—H340.9300
Fe2—C112.037 (4)C38—C371.413 (5)
Fe2—C162.043 (4)C38—H380.9300
Fe2—C152.044 (4)C18—C171.419 (6)
Fe2—C182.050 (4)C18—H180.9300
Fe2—C172.053 (4)C16—C201.425 (6)
Fe2—C192.053 (4)C16—C171.432 (6)
Fe2—C202.055 (4)C16—H160.9300
Fe2—C142.065 (4)C35—C311.413 (6)
Fe2—C132.066 (4)C35—H350.9300
Fe1—C22.048 (4)C22—C231.419 (6)
Fe1—C42.050 (4)C22—H220.9300
Fe1—C52.051 (4)C27—C281.435 (5)
Fe1—C32.051 (4)C27—H270.9300
Fe1—C12.053 (4)C24—C231.404 (6)
Fe3—C292.036 (4)C24—C251.424 (6)
Fe3—C302.036 (4)C24—H240.9300
Fe3—C212.047 (4)C25—H250.9300
Fe3—C222.048 (4)C23—H230.9300
Fe3—C252.052 (4)C32—C311.401 (7)
Fe3—C242.054 (4)C32—C331.414 (7)
Fe3—C282.058 (4)C32—H320.9300
Fe3—C232.059 (4)C20—H200.9300
Fe3—C262.060 (4)C28—H280.9300
Fe3—C272.065 (4)C33—H330.9300
O3—C441.281 (4)C17—H170.9300
O1—C411.279 (4)C37—H370.9300
O2—C431.285 (4)C31—H310.9300
C14—C131.422 (5)
C10—C6—C7108.5 (8)C25—Fe3—C2367.69 (17)
C10—C6—Fe170.8 (5)C24—Fe3—C2339.93 (17)
C7—C6—Fe169.8 (5)C28—Fe3—C23166.91 (16)
C10—C6—H6125.8C29—Fe3—C2668.62 (14)
C7—C6—H6125.8C30—Fe3—C2640.69 (15)
Fe1—C6—H6125.2C21—Fe3—C26151.57 (18)
C6—C7—C8108.4 (8)C22—Fe3—C26118.27 (16)
C6—C7—Fe170.1 (5)C25—Fe3—C26166.65 (19)
C8—C7—Fe170.4 (7)C24—Fe3—C26128.43 (17)
C6—C7—H7125.8C28—Fe3—C2668.43 (15)
C8—C7—H7125.8C23—Fe3—C26108.49 (16)
Fe1—C7—H7125.3C29—Fe3—C2768.51 (15)
C7—C8—C9106.3 (9)C30—Fe3—C2768.43 (16)
C7—C8—Fe169.3 (7)C21—Fe3—C27118.67 (18)
C9—C8—Fe170.5 (7)C22—Fe3—C27108.81 (17)
C7—C8—H8126.9C25—Fe3—C27152.01 (18)
C9—C8—H8126.9C24—Fe3—C27166.18 (17)
Fe1—C8—H8125.0C28—Fe3—C2740.74 (14)
C10—C9—C8108.6 (10)C23—Fe3—C27128.89 (16)
C10—C9—Fe169.7 (6)C26—Fe3—C2740.21 (16)
C8—C9—Fe169.4 (7)C44—O3—Cu2126.0 (2)
C10—C9—H9125.7C41—O1—Cu1126.4 (2)
C8—C9—H9125.7C43—O2—Cu1126.1 (2)
Fe1—C9—H9126.8C13—C14—C15108.3 (3)
C6—C10—C9108.2 (9)C13—C14—Fe269.9 (2)
C6—C10—Fe169.9 (6)C15—C14—Fe268.7 (2)
C9—C10—Fe170.7 (6)C13—C14—H14125.8
C6—C10—H10125.9C15—C14—H14125.8
C9—C10—H10125.9Fe2—C14—H14127.1
Fe1—C10—H10125.1C46—O4—Cu2125.5 (2)
C48—C47—C51113 (2)C12—C13—C14108.3 (3)
C48—C47—Fe167.9 (12)C12—C13—Fe268.6 (2)
C51—C47—Fe168.1 (14)C14—C13—Fe269.8 (2)
C48—C47—H47123.4C12—C13—H13125.9
C51—C47—H47123.4C14—C13—H13125.9
Fe1—C47—H47132.9Fe2—C13—H13127.3
C47—C48—C49102.7 (19)C3—C4—C5107.7 (3)
C47—C48—Fe172.2 (12)C3—C4—Fe169.9 (2)
C49—C48—Fe167.9 (14)C5—C4—Fe169.4 (2)
C47—C48—H48128.7C3—C4—H4126.1
C49—C48—H48128.7C5—C4—H4126.1
Fe1—C48—H48123.1Fe1—C4—H4126.1
C50—C49—C48110.8 (18)O4—C46—C45125.5 (3)
C50—C49—Fe168.6 (14)O4—C46—C5115.4 (3)
C48—C49—Fe169.4 (13)C45—C46—C5119.1 (3)
C50—C49—H49124.6C13—C12—C11108.3 (3)
C48—C49—H49124.6C13—C12—Fe271.0 (2)
Fe1—C49—H49129.1C11—C12—Fe269.3 (2)
C49—C50—C51107.0 (18)C13—C12—H12125.9
C49—C50—Fe170.3 (15)C11—C12—H12125.9
C51—C50—Fe170.6 (14)Fe2—C12—H12125.5
C49—C50—H50126.5C26—C30—C29107.6 (3)
C51—C50—H50126.5C26—C30—Fe370.5 (2)
Fe1—C50—H50124.2C29—C30—Fe369.3 (2)
C47—C51—C50105.4 (19)C26—C30—H30126.2
C47—C51—Fe171.8 (14)C29—C30—H30126.2
C50—C51—Fe166.9 (13)Fe3—C30—H30125.5
C47—C51—H51127.3O3—C44—C45124.8 (3)
C50—C51—H51127.3O3—C44—C11116.2 (3)
Fe1—C51—H51125.6C45—C44—C11119.0 (3)
O1i—Cu1—O1180C11—C15—C14107.7 (3)
O1i—Cu1—O2i93.32 (11)C11—C15—Fe269.2 (2)
O1—Cu1—O2i86.68 (11)C14—C15—Fe270.3 (2)
O1i—Cu1—O286.68 (11)C11—C15—H15126.1
O1—Cu1—O293.32 (11)C14—C15—H15126.1
O2i—Cu1—O2180Fe2—C15—H15125.9
O4ii—Cu2—O4180O1—C41—C42124.9 (3)
O4ii—Cu2—O386.38 (10)O1—C41—C40114.9 (3)
O4—Cu2—O393.62 (10)C42—C41—C40120.1 (3)
O4ii—Cu2—O3ii93.62 (10)C37—C36—C40107.7 (3)
O4—Cu2—O3ii86.38 (10)C37—C36—Fe469.3 (2)
O3—Cu2—O3ii180C40—C36—Fe469.9 (2)
C31—Fe4—C38116.09 (18)C37—C36—H36126.2
C31—Fe4—C3467.92 (18)C40—C36—H36126.2
C38—Fe4—C34128.48 (18)Fe4—C36—H36126.2
C31—Fe4—C3367.86 (19)C44—C45—C46124.2 (3)
C38—Fe4—C33167.69 (19)C44—C45—H45117.9
C34—Fe4—C3340.54 (19)C46—C45—H45117.9
C31—Fe4—C37106.92 (18)C1—C5—C4107.8 (3)
C38—Fe4—C3740.45 (15)C1—C5—C46125.1 (3)
C34—Fe4—C37165.71 (19)C4—C5—C46127.2 (3)
C33—Fe4—C37151.51 (19)C1—C5—Fe169.7 (2)
C31—Fe4—C3540.42 (18)C4—C5—Fe169.3 (2)
C38—Fe4—C35106.93 (17)C46—C5—Fe1126.1 (3)
C34—Fe4—C3540.34 (19)C27—C26—C30108.5 (3)
C33—Fe4—C3567.94 (19)C27—C26—Fe370.1 (2)
C37—Fe4—C35127.28 (18)C30—C26—Fe368.8 (2)
C31—Fe4—C3240.05 (19)C27—C26—H26125.8
C38—Fe4—C32149.5 (2)C30—C26—H26125.8
C34—Fe4—C3267.87 (19)Fe3—C26—H26127.0
C33—Fe4—C3240.4 (2)C1—C2—C3108.5 (3)
C37—Fe4—C32117.43 (18)C1—C2—Fe169.9 (2)
C35—Fe4—C3267.64 (18)C3—C2—Fe169.8 (2)
C31—Fe4—C36128.25 (17)C1—C2—H2125.7
C38—Fe4—C3668.72 (15)C3—C2—H2125.7
C34—Fe4—C36152.53 (18)Fe1—C2—H2126.2
C33—Fe4—C36118.95 (18)C36—C40—C39107.3 (3)
C37—Fe4—C3640.96 (15)C36—C40—C41128.4 (3)
C35—Fe4—C36165.92 (18)C39—C40—C41124.3 (3)
C32—Fe4—C36108.86 (17)C36—C40—Fe469.2 (2)
C31—Fe4—C39149.52 (18)C39—C40—Fe469.1 (2)
C38—Fe4—C3940.66 (15)C41—C40—Fe4126.4 (3)
C34—Fe4—C39108.77 (17)C28—C29—C30108.2 (3)
C33—Fe4—C39130.47 (18)C28—C29—C43124.1 (3)
C37—Fe4—C3968.46 (16)C30—C29—C43127.5 (3)
C35—Fe4—C39117.02 (17)C28—C29—Fe370.3 (2)
C32—Fe4—C39169.17 (19)C30—C29—Fe369.3 (2)
C36—Fe4—C3969.04 (15)C43—C29—Fe3123.0 (3)
C31—Fe4—C40167.48 (17)C4—C3—C2108.4 (3)
C38—Fe4—C4068.84 (15)C4—C3—Fe169.8 (2)
C34—Fe4—C40119.04 (17)C2—C3—Fe169.5 (2)
C33—Fe4—C40109.92 (17)C4—C3—H3125.8
C37—Fe4—C4068.79 (15)C2—C3—H3125.8
C35—Fe4—C40151.42 (17)Fe1—C3—H3126.4
C32—Fe4—C40130.41 (18)C15—C11—C12107.4 (3)
C36—Fe4—C4040.99 (14)C15—C11—C44124.9 (3)
C39—Fe4—C4041.21 (14)C12—C11—C44127.4 (3)
C12—Fe2—C1141.63 (14)C15—C11—Fe269.8 (2)
C12—Fe2—C16106.95 (17)C12—C11—Fe269.1 (2)
C11—Fe2—C16119.39 (16)C44—C11—Fe2122.1 (3)
C12—Fe2—C1569.26 (15)O2—C43—C42124.6 (3)
C11—Fe2—C1541.01 (15)O2—C43—C29115.7 (3)
C16—Fe2—C15154.54 (16)C42—C43—C29119.7 (3)
C12—Fe2—C18153.86 (16)C2—C1—C5107.6 (3)
C11—Fe2—C18163.50 (16)C2—C1—Fe169.5 (2)
C16—Fe2—C1868.27 (17)C5—C1—Fe169.6 (2)
C15—Fe2—C18126.24 (16)C2—C1—H1126.2
C12—Fe2—C17118.98 (16)C5—C1—H1126.2
C11—Fe2—C17154.38 (16)Fe1—C1—H1126.3
C16—Fe2—C1740.92 (16)C20—C19—C18108.3 (4)
C15—Fe2—C17163.23 (16)C20—C19—Fe269.9 (2)
C18—Fe2—C1740.47 (16)C18—C19—Fe269.5 (2)
C12—Fe2—C19163.50 (16)C20—C19—H19125.9
C11—Fe2—C19125.75 (16)C18—C19—H19125.9
C16—Fe2—C1968.12 (17)Fe2—C19—H19126.3
C15—Fe2—C19107.99 (16)C38—C39—C40107.8 (3)
C18—Fe2—C1940.70 (16)C38—C39—Fe469.3 (2)
C17—Fe2—C1968.37 (17)C40—C39—Fe469.7 (2)
C12—Fe2—C20125.78 (16)C38—C39—H39126.1
C11—Fe2—C20107.12 (16)C40—C39—H39126.1
C16—Fe2—C2040.70 (17)Fe4—C39—H39126.4
C15—Fe2—C20119.90 (16)C22—C21—C25107.8 (4)
C18—Fe2—C2068.35 (17)C22—C21—Fe369.8 (2)
C17—Fe2—C2068.70 (16)C25—C21—Fe370.0 (2)
C19—Fe2—C2040.38 (17)C22—C21—H21126.1
C12—Fe2—C1468.23 (15)C25—C21—H21126.1
C11—Fe2—C1468.72 (15)Fe3—C21—H21125.7
C16—Fe2—C14162.86 (16)C41—C42—C43124.0 (3)
C15—Fe2—C1440.95 (14)C41—C42—H42118.0
C18—Fe2—C14108.36 (16)C43—C42—H42118.0
C17—Fe2—C14125.69 (16)C35—C34—C33107.9 (4)
C19—Fe2—C14121.07 (16)C35—C34—Fe470.0 (3)
C20—Fe2—C14155.33 (16)C33—C34—Fe469.7 (3)
C12—Fe2—C1340.38 (14)C35—C34—H34126.0
C11—Fe2—C1368.85 (15)C33—C34—H34126.0
C16—Fe2—C13125.63 (17)Fe4—C34—H34125.9
C15—Fe2—C1368.66 (15)C37—C38—C39108.7 (3)
C18—Fe2—C13120.15 (16)C37—C38—Fe469.8 (2)
C17—Fe2—C13107.35 (16)C39—C38—Fe470.0 (2)
C19—Fe2—C13155.19 (16)C37—C38—H38125.7
C20—Fe2—C13162.96 (17)C39—C38—H38125.7
C14—Fe2—C1340.26 (15)Fe4—C38—H38126.1
C50—Fe1—C4941.1 (9)C17—C18—C19108.3 (4)
C50—Fe1—C4872.1 (9)C17—C18—Fe269.9 (2)
C49—Fe1—C4842.7 (9)C19—C18—Fe269.8 (2)
C50—Fe1—C5142.6 (9)C17—C18—H18125.8
C49—Fe1—C5169.3 (10)C19—C18—H18125.8
C48—Fe1—C5170.8 (8)Fe2—C18—H18126.1
C50—Fe1—C2165.4 (10)C20—C16—C17108.5 (4)
C49—Fe1—C2126.5 (9)C20—C16—Fe270.1 (2)
C48—Fe1—C2102.8 (6)C17—C16—Fe269.9 (2)
C51—Fe1—C2149.8 (11)C20—C16—H16125.8
C50—Fe1—C768.5 (7)C17—C16—H16125.8
C49—Fe1—C750.4 (9)Fe2—C16—H16125.8
C48—Fe1—C716.7 (5)C34—C35—C31107.9 (4)
C51—Fe1—C756.5 (7)C34—C35—Fe469.7 (2)
C2—Fe1—C7110.6 (3)C31—C35—Fe469.6 (2)
C50—Fe1—C4121.5 (8)C34—C35—H35126.0
C49—Fe1—C4158.9 (10)C31—C35—H35126.0
C48—Fe1—C4156.9 (9)Fe4—C35—H35126.2
C51—Fe1—C4105.7 (6)C21—C22—C23108.2 (4)
C2—Fe1—C468.27 (15)C21—C22—Fe369.8 (2)
C7—Fe1—C4144.7 (4)C23—C22—Fe370.2 (2)
C50—Fe1—C5110.9 (7)C21—C22—H22125.9
C49—Fe1—C5124.8 (8)C23—C22—H22125.9
C48—Fe1—C5157.0 (7)Fe3—C22—H22125.7
C51—Fe1—C5127.7 (8)C26—C27—C28108.5 (3)
C2—Fe1—C568.26 (15)C26—C27—Fe369.7 (2)
C7—Fe1—C5173.6 (4)C28—C27—Fe369.4 (2)
C4—Fe1—C541.28 (14)C26—C27—H27125.7
C50—Fe1—C3153.7 (10)C28—C27—H27125.7
C49—Fe1—C3160.8 (10)Fe3—C27—H27126.7
C48—Fe1—C3119.4 (8)C23—C24—C25108.1 (4)
C51—Fe1—C3115.5 (9)C23—C24—Fe370.2 (2)
C2—Fe1—C340.70 (15)C25—C24—Fe369.7 (2)
C7—Fe1—C3115.1 (3)C23—C24—H24125.9
C4—Fe1—C340.21 (15)C25—C24—H24125.9
C5—Fe1—C368.41 (15)Fe3—C24—H24125.8
C50—Fe1—C1129.3 (9)C21—C25—C24107.9 (4)
C49—Fe1—C1111.2 (8)C21—C25—Fe369.6 (2)
C48—Fe1—C1118.9 (6)C24—C25—Fe369.8 (2)
C51—Fe1—C1167.1 (10)C21—C25—H25126.1
C2—Fe1—C140.56 (15)C24—C25—H25126.1
C7—Fe1—C1134.4 (4)Fe3—C25—H25126.1
C4—Fe1—C168.95 (15)C24—C23—C22108.0 (4)
C5—Fe1—C140.76 (14)C24—C23—Fe369.8 (2)
C3—Fe1—C168.55 (15)C22—C23—Fe369.4 (2)
C50—Fe1—C653.9 (8)C24—C23—H23126.0
C49—Fe1—C667.5 (8)C22—C23—H23126.0
C48—Fe1—C655.9 (6)Fe3—C23—H23126.4
C51—Fe1—C618.8 (7)C31—C32—C33108.3 (4)
C2—Fe1—C6135.1 (4)C31—C32—Fe469.7 (2)
C7—Fe1—C640.1 (3)C33—C32—Fe469.6 (2)
C4—Fe1—C6114.5 (3)C31—C32—H32125.9
C5—Fe1—C6145.0 (4)C33—C32—H32125.9
C3—Fe1—C6110.6 (3)Fe4—C32—H32126.4
C1—Fe1—C6174.0 (4)C19—C20—C16107.6 (4)
C50—Fe1—C854.6 (8)C19—C20—Fe269.7 (2)
C49—Fe1—C815.5 (8)C16—C20—Fe269.2 (2)
C48—Fe1—C829.0 (8)C19—C20—H20126.2
C51—Fe1—C874.6 (7)C16—C20—H20126.2
C2—Fe1—C8114.6 (4)Fe2—C20—H20126.4
C7—Fe1—C840.3 (4)C29—C28—C27107.2 (3)
C4—Fe1—C8174.0 (4)C29—C28—Fe368.7 (2)
C5—Fe1—C8133.9 (4)C27—C28—Fe369.9 (2)
C3—Fe1—C8145.3 (4)C29—C28—H28126.4
C1—Fe1—C8109.5 (4)C27—C28—H28126.4
C6—Fe1—C867.6 (4)Fe3—C28—H28126.6
C29—Fe3—C3041.31 (14)C32—C33—C34107.7 (4)
C29—Fe3—C21128.52 (16)C32—C33—Fe470.0 (3)
C30—Fe3—C21166.86 (17)C34—C33—Fe469.7 (2)
C29—Fe3—C22166.85 (16)C32—C33—H33126.2
C30—Fe3—C22150.96 (15)C34—C33—H33126.2
C21—Fe3—C2240.42 (16)Fe4—C33—H33125.7
C29—Fe3—C25108.13 (16)C18—C17—C16107.3 (4)
C30—Fe3—C25128.46 (18)C18—C17—Fe269.6 (2)
C21—Fe3—C2540.39 (19)C16—C17—Fe269.2 (2)
C22—Fe3—C2567.79 (18)C18—C17—H17126.3
C29—Fe3—C24118.00 (17)C16—C17—H17126.3
C30—Fe3—C24107.70 (18)Fe2—C17—H17126.4
C21—Fe3—C2468.05 (19)C38—C37—C36108.5 (3)
C22—Fe3—C2467.70 (18)C38—C37—Fe469.7 (2)
C25—Fe3—C2440.58 (18)C36—C37—Fe469.7 (2)
C29—Fe3—C2840.97 (15)C38—C37—H37125.7
C30—Fe3—C2869.19 (16)C36—C37—H37125.7
C21—Fe3—C28108.30 (17)Fe4—C37—H37126.4
C22—Fe3—C28128.73 (17)C32—C31—C35108.2 (4)
C25—Fe3—C28118.23 (17)C32—C31—Fe470.2 (2)
C24—Fe3—C28151.79 (17)C35—C31—Fe470.0 (2)
C29—Fe3—C23151.10 (17)C32—C31—H31125.9
C30—Fe3—C23117.39 (16)C35—C31—H31125.9
C21—Fe3—C2367.95 (17)Fe4—C31—H31125.5
C22—Fe3—C2340.43 (17)
C10—C6—C7—C80.3 (13)C5—Fe1—C3—C281.3 (2)
Fe1—C6—C7—C860.2 (9)C1—Fe1—C3—C237.4 (2)
C10—C6—C7—Fe160.5 (7)C6—Fe1—C3—C2136.3 (5)
C6—C7—C8—C91.1 (14)C8—Fe1—C3—C256.2 (7)
Fe1—C7—C8—C961.2 (9)C14—C15—C11—C120.9 (4)
C6—C7—C8—Fe160.0 (7)Fe2—C15—C11—C1259.1 (3)
C7—C8—C9—C101.6 (15)C14—C15—C11—C44175.7 (3)
Fe1—C8—C9—C1058.8 (9)Fe2—C15—C11—C44115.6 (4)
C7—C8—C9—Fe160.4 (9)C14—C15—C11—Fe260.0 (3)
C7—C6—C10—C90.7 (12)C13—C12—C11—C151.1 (4)
Fe1—C6—C10—C960.6 (8)Fe2—C12—C11—C1559.5 (3)
C7—C6—C10—Fe159.9 (7)C13—C12—C11—C44175.6 (3)
C8—C9—C10—C61.4 (14)Fe2—C12—C11—C44115.1 (4)
Fe1—C9—C10—C660.1 (7)C13—C12—C11—Fe260.5 (3)
C8—C9—C10—Fe158.7 (9)O3—C44—C11—C1514.2 (5)
C51—C47—C48—C499 (3)C45—C44—C11—C15164.7 (4)
Fe1—C47—C48—C4961.5 (16)O3—C44—C11—C12172.1 (3)
C51—C47—C48—Fe152 (2)C45—C44—C11—C128.9 (6)
C47—C48—C49—C509 (3)O3—C44—C11—Fe2100.8 (4)
Fe1—C48—C49—C5056 (2)C45—C44—C11—Fe278.2 (4)
C47—C48—C49—Fe164.5 (15)C12—Fe2—C11—C15118.8 (3)
C48—C49—C50—C515 (3)C16—Fe2—C11—C15158.7 (2)
Fe1—C49—C50—C5161.4 (17)C18—Fe2—C11—C1544.8 (6)
C48—C49—C50—Fe156.4 (19)C17—Fe2—C11—C15167.5 (3)
C48—C47—C51—C507 (3)C19—Fe2—C11—C1575.6 (3)
Fe1—C47—C51—C5058.7 (17)C20—Fe2—C11—C15116.1 (2)
C48—C47—C51—Fe152.1 (19)C14—Fe2—C11—C1538.1 (2)
C49—C50—C51—C471 (3)C13—Fe2—C11—C1581.4 (2)
Fe1—C50—C51—C4761.9 (18)C16—Fe2—C11—C1282.5 (3)
C49—C50—C51—Fe161.2 (19)C15—Fe2—C11—C12118.8 (3)
C51—C50—Fe1—C49117.1 (19)C18—Fe2—C11—C12163.6 (5)
C49—C50—Fe1—C4836.4 (13)C17—Fe2—C11—C1248.7 (4)
C51—C50—Fe1—C4880.7 (13)C19—Fe2—C11—C12165.6 (2)
C49—C50—Fe1—C51117.1 (19)C20—Fe2—C11—C12125.1 (2)
C49—C50—Fe1—C236 (4)C14—Fe2—C11—C1280.7 (2)
C51—C50—Fe1—C2153 (3)C13—Fe2—C11—C1237.4 (2)
C49—C50—Fe1—C753.7 (14)C12—Fe2—C11—C44121.9 (4)
C51—C50—Fe1—C763.4 (11)C16—Fe2—C11—C4439.4 (4)
C49—C50—Fe1—C4164.3 (13)C15—Fe2—C11—C44119.3 (4)
C51—C50—Fe1—C478.6 (13)C18—Fe2—C11—C4474.5 (7)
C49—C50—Fe1—C5119.5 (15)C17—Fe2—C11—C4473.2 (5)
C51—C50—Fe1—C5123.4 (12)C19—Fe2—C11—C4443.6 (4)
C49—C50—Fe1—C3157.2 (15)C20—Fe2—C11—C443.1 (3)
C51—C50—Fe1—C340 (2)C14—Fe2—C11—C44157.4 (3)
C49—C50—Fe1—C176.8 (16)C13—Fe2—C11—C44159.3 (3)
C51—C50—Fe1—C1166.1 (10)Cu1—O2—C43—C420.4 (5)
C49—C50—Fe1—C696.7 (15)Cu1—O2—C43—C29179.5 (2)
C51—C50—Fe1—C620.4 (9)C28—C29—C43—O215.6 (5)
C49—C50—Fe1—C810.2 (15)C30—C29—C43—O2168.7 (3)
C51—C50—Fe1—C8106.9 (14)Fe3—C29—C43—O2103.1 (3)
C48—C49—Fe1—C50123.7 (19)C28—C29—C43—C42164.5 (4)
C50—C49—Fe1—C48123.7 (19)C30—C29—C43—C4211.2 (6)
C50—C49—Fe1—C5140.1 (14)Fe3—C29—C43—C4277.0 (4)
C48—C49—Fe1—C5183.6 (13)C3—C2—C1—C50.1 (4)
C50—C49—Fe1—C2169.5 (14)Fe1—C2—C1—C559.4 (3)
C48—C49—Fe1—C266.8 (15)C3—C2—C1—Fe159.3 (3)
C50—C49—Fe1—C7103.1 (16)C4—C5—C1—C20.3 (4)
C48—C49—Fe1—C720.6 (8)C46—C5—C1—C2179.9 (3)
C50—C49—Fe1—C440 (3)Fe1—C5—C1—C259.4 (3)
C48—C49—Fe1—C4163.6 (15)C4—C5—C1—Fe159.1 (3)
C50—C49—Fe1—C582.1 (16)C46—C5—C1—Fe1120.5 (4)
C48—C49—Fe1—C5154.2 (10)C50—Fe1—C1—C2165.2 (10)
C50—C49—Fe1—C3148 (2)C49—Fe1—C1—C2121.9 (11)
C48—C49—Fe1—C325 (3)C48—Fe1—C1—C275.2 (10)
C50—C49—Fe1—C1126.1 (15)C51—Fe1—C1—C2148 (4)
C48—C49—Fe1—C1110.2 (12)C7—Fe1—C1—C267.2 (5)
C50—C49—Fe1—C660.2 (14)C4—Fe1—C1—C280.8 (2)
C48—C49—Fe1—C663.5 (11)C5—Fe1—C1—C2118.9 (3)
C50—C49—Fe1—C8147 (5)C3—Fe1—C1—C237.5 (2)
C48—C49—Fe1—C824 (3)C8—Fe1—C1—C2105.4 (5)
C47—C48—Fe1—C5077.3 (15)C50—Fe1—C1—C575.9 (10)
C49—C48—Fe1—C5035.0 (13)C49—Fe1—C1—C5119.3 (11)
C47—C48—Fe1—C49112 (2)C48—Fe1—C1—C5165.9 (10)
C47—C48—Fe1—C5132.3 (15)C51—Fe1—C1—C529 (4)
C49—C48—Fe1—C5180.1 (15)C2—Fe1—C1—C5118.9 (3)
C47—C48—Fe1—C2117.0 (14)C7—Fe1—C1—C5174.0 (5)
C49—C48—Fe1—C2130.7 (14)C4—Fe1—C1—C538.1 (2)
C47—C48—Fe1—C73 (2)C3—Fe1—C1—C581.4 (2)
C49—C48—Fe1—C7110 (3)C8—Fe1—C1—C5135.7 (5)
C47—C48—Fe1—C453 (2)C12—Fe2—C19—C2037.7 (7)
C49—C48—Fe1—C4165.0 (13)C11—Fe2—C19—C2073.3 (3)
C47—C48—Fe1—C5178.9 (12)C16—Fe2—C19—C2037.9 (2)
C49—C48—Fe1—C567 (2)C15—Fe2—C19—C20115.3 (2)
C47—C48—Fe1—C376.8 (15)C18—Fe2—C19—C20119.6 (3)
C49—C48—Fe1—C3170.9 (13)C17—Fe2—C19—C2082.1 (3)
C47—C48—Fe1—C1157.1 (12)C14—Fe2—C19—C20158.3 (2)
C49—C48—Fe1—C190.6 (15)C13—Fe2—C19—C20166.8 (3)
C47—C48—Fe1—C619.3 (11)C12—Fe2—C19—C18157.2 (5)
C49—C48—Fe1—C693.0 (15)C11—Fe2—C19—C18167.1 (2)
C47—C48—Fe1—C8125 (2)C16—Fe2—C19—C1881.7 (3)
C49—C48—Fe1—C812.7 (17)C15—Fe2—C19—C18125.1 (2)
C47—C51—Fe1—C50116.4 (19)C17—Fe2—C19—C1837.4 (2)
C47—C51—Fe1—C4977.7 (15)C20—Fe2—C19—C18119.6 (3)
C50—C51—Fe1—C4938.7 (13)C14—Fe2—C19—C1882.1 (3)
C47—C51—Fe1—C4832.1 (15)C13—Fe2—C19—C1847.2 (5)
C50—C51—Fe1—C4884.2 (14)C36—C40—C39—C380.3 (4)
C47—C51—Fe1—C250 (2)C41—C40—C39—C38179.6 (3)
C50—C51—Fe1—C2166.7 (12)Fe4—C40—C39—C3859.1 (3)
C47—C51—Fe1—C722.3 (12)C36—C40—C39—Fe458.8 (2)
C50—C51—Fe1—C794.1 (13)C41—C40—C39—Fe4120.5 (4)
C47—C51—Fe1—C4123.9 (15)C31—Fe4—C39—C3849.6 (4)
C50—C51—Fe1—C4119.7 (13)C34—Fe4—C39—C38127.8 (3)
C47—C51—Fe1—C5163.6 (12)C33—Fe4—C39—C38167.9 (3)
C50—C51—Fe1—C580.0 (14)C37—Fe4—C39—C3837.3 (2)
C47—C51—Fe1—C382.1 (16)C35—Fe4—C39—C3884.7 (3)
C50—C51—Fe1—C3161.6 (12)C32—Fe4—C39—C38162.1 (8)
C47—C51—Fe1—C1172 (2)C36—Fe4—C39—C3881.4 (2)
C50—C51—Fe1—C156 (4)C40—Fe4—C39—C38119.2 (3)
C47—C51—Fe1—C63.1 (19)C31—Fe4—C39—C40168.9 (3)
C50—C51—Fe1—C6119 (3)C38—Fe4—C39—C40119.2 (3)
C47—C51—Fe1—C862.3 (14)C34—Fe4—C39—C40113.0 (2)
C50—C51—Fe1—C854.1 (12)C33—Fe4—C39—C4072.9 (3)
C6—C7—Fe1—C5058.9 (11)C37—Fe4—C39—C4082.0 (2)
C8—C7—Fe1—C5060.2 (10)C35—Fe4—C39—C40156.0 (2)
C6—C7—Fe1—C49102.3 (13)C32—Fe4—C39—C4042.9 (10)
C8—C7—Fe1—C4916.7 (12)C36—Fe4—C39—C4037.9 (2)
C6—C7—Fe1—C48158 (3)C29—Fe3—C21—C22170.0 (2)
C8—C7—Fe1—C4839 (3)C30—Fe3—C21—C22154.4 (7)
C6—C7—Fe1—C5112.4 (13)C25—Fe3—C21—C22118.7 (4)
C8—C7—Fe1—C51106.6 (12)C24—Fe3—C21—C2280.9 (3)
C6—C7—Fe1—C2136.8 (6)C28—Fe3—C21—C22128.9 (3)
C8—C7—Fe1—C2104.2 (7)C23—Fe3—C21—C2237.7 (3)
C6—C7—Fe1—C455.6 (8)C26—Fe3—C21—C2250.6 (5)
C8—C7—Fe1—C4174.7 (6)C27—Fe3—C21—C2285.7 (3)
C6—C7—Fe1—C392.7 (7)C29—Fe3—C21—C2571.2 (3)
C8—C7—Fe1—C3148.3 (6)C30—Fe3—C21—C2535.6 (8)
C6—C7—Fe1—C1176.6 (6)C22—Fe3—C21—C25118.7 (4)
C8—C7—Fe1—C164.4 (8)C24—Fe3—C21—C2537.8 (3)
C8—C7—Fe1—C6119.0 (9)C28—Fe3—C21—C25112.3 (3)
C6—C7—Fe1—C8119.0 (9)C23—Fe3—C21—C2581.0 (3)
C10—C6—Fe1—C5019.6 (9)C26—Fe3—C21—C25169.3 (3)
C7—C6—Fe1—C5099.4 (11)C27—Fe3—C21—C25155.6 (2)
C10—C6—Fe1—C4964.5 (10)O1—C41—C42—C432.9 (6)
C7—C6—Fe1—C4954.5 (11)C40—C41—C42—C43177.1 (3)
C10—C6—Fe1—C48111.6 (11)O2—C43—C42—C415.5 (6)
C7—C6—Fe1—C487.4 (12)C29—C43—C42—C41174.6 (3)
C10—C6—Fe1—C5127 (3)C31—Fe4—C34—C3537.7 (3)
C7—C6—Fe1—C51146 (3)C38—Fe4—C34—C3568.8 (3)
C10—C6—Fe1—C2175.7 (6)C33—Fe4—C34—C35119.0 (4)
C7—C6—Fe1—C265.2 (7)C37—Fe4—C34—C3533.6 (8)
C10—C6—Fe1—C7119.0 (8)C32—Fe4—C34—C3581.1 (3)
C10—C6—Fe1—C492.6 (7)C36—Fe4—C34—C35169.6 (3)
C7—C6—Fe1—C4148.4 (6)C39—Fe4—C34—C35109.9 (3)
C10—C6—Fe1—C554.6 (8)C40—Fe4—C34—C35153.9 (2)
C7—C6—Fe1—C5173.7 (5)C31—Fe4—C34—C3381.3 (3)
C10—C6—Fe1—C3136.1 (6)C38—Fe4—C34—C33172.2 (3)
C7—C6—Fe1—C3104.9 (6)C37—Fe4—C34—C33152.6 (6)
C10—C6—Fe1—C881.3 (6)C35—Fe4—C34—C33119.0 (4)
C7—C6—Fe1—C837.7 (6)C32—Fe4—C34—C3337.9 (3)
C7—C8—Fe1—C5098.2 (12)C36—Fe4—C34—C3350.6 (5)
C9—C8—Fe1—C5018.7 (11)C39—Fe4—C34—C33131.1 (3)
C7—C8—Fe1—C49124 (4)C40—Fe4—C34—C3387.2 (3)
C9—C8—Fe1—C497 (3)C40—C39—C38—C370.0 (4)
C7—C8—Fe1—C4822.0 (11)Fe4—C39—C38—C3759.3 (3)
C9—C8—Fe1—C48138.9 (16)C40—C39—C38—Fe459.3 (2)
C7—C8—Fe1—C5156.0 (10)C31—Fe4—C38—C3785.7 (3)
C9—C8—Fe1—C5160.9 (11)C34—Fe4—C38—C37167.3 (2)
C7—C8—Fe1—C293.3 (7)C33—Fe4—C38—C37168.3 (7)
C9—C8—Fe1—C2149.8 (6)C35—Fe4—C38—C37128.2 (3)
C9—C8—Fe1—C7116.9 (10)C32—Fe4—C38—C3753.7 (4)
C7—C8—Fe1—C5176.1 (5)C36—Fe4—C38—C3737.6 (2)
C9—C8—Fe1—C567.0 (9)C39—Fe4—C38—C37119.8 (3)
C7—C8—Fe1—C356.7 (10)C40—Fe4—C38—C3781.7 (2)
C9—C8—Fe1—C3173.6 (5)C31—Fe4—C38—C39154.5 (2)
C7—C8—Fe1—C1136.9 (6)C34—Fe4—C38—C3972.9 (3)
C9—C8—Fe1—C1106.2 (7)C33—Fe4—C38—C3948.5 (9)
C7—C8—Fe1—C637.5 (6)C37—Fe4—C38—C39119.8 (3)
C9—C8—Fe1—C679.4 (7)C35—Fe4—C38—C39112.0 (2)
O4ii—Cu2—O3—C44173.8 (3)C32—Fe4—C38—C39173.5 (3)
O4—Cu2—O3—C446.2 (3)C36—Fe4—C38—C3982.2 (2)
O2i—Cu1—O1—C41171.8 (3)C40—Fe4—C38—C3938.1 (2)
O2—Cu1—O1—C418.2 (3)C20—C19—C18—C170.1 (5)
O1i—Cu1—O2—C43174.2 (3)Fe2—C19—C18—C1759.5 (3)
O1—Cu1—O2—C435.8 (3)C20—C19—C18—Fe259.3 (3)
C12—Fe2—C14—C1337.1 (2)C12—Fe2—C18—C1746.1 (5)
C11—Fe2—C14—C1382.0 (2)C11—Fe2—C18—C17159.1 (5)
C16—Fe2—C14—C1339.6 (6)C16—Fe2—C18—C1738.2 (2)
C15—Fe2—C14—C13120.1 (3)C15—Fe2—C18—C17165.9 (2)
C18—Fe2—C14—C13115.3 (2)C19—Fe2—C18—C17119.5 (4)
C17—Fe2—C14—C1373.7 (3)C20—Fe2—C18—C1782.1 (3)
C19—Fe2—C14—C13158.2 (2)C14—Fe2—C18—C17123.9 (2)
C20—Fe2—C14—C13166.8 (4)C13—Fe2—C18—C1781.4 (3)
C12—Fe2—C14—C1583.0 (2)C12—Fe2—C18—C19165.5 (3)
C11—Fe2—C14—C1538.1 (2)C11—Fe2—C18—C1939.7 (7)
C16—Fe2—C14—C15159.7 (5)C16—Fe2—C18—C1981.3 (3)
C18—Fe2—C14—C15124.6 (2)C15—Fe2—C18—C1974.6 (3)
C17—Fe2—C14—C15166.1 (2)C17—Fe2—C18—C19119.5 (4)
C19—Fe2—C14—C1581.7 (3)C20—Fe2—C18—C1937.3 (2)
C20—Fe2—C14—C1546.7 (5)C14—Fe2—C18—C19116.6 (2)
C13—Fe2—C14—C15120.1 (3)C13—Fe2—C18—C19159.1 (2)
O3—Cu2—O4—C464.9 (3)C12—Fe2—C16—C20125.7 (3)
O3ii—Cu2—O4—C46175.1 (3)C11—Fe2—C16—C2082.1 (3)
C15—C14—C13—C120.2 (4)C15—Fe2—C16—C2048.4 (5)
Fe2—C14—C13—C1258.0 (3)C18—Fe2—C16—C2081.6 (3)
C15—C14—C13—Fe258.1 (3)C17—Fe2—C16—C20119.4 (4)
C11—Fe2—C13—C1238.5 (2)C19—Fe2—C16—C2037.6 (3)
C16—Fe2—C13—C1273.2 (3)C14—Fe2—C16—C20163.5 (5)
C15—Fe2—C13—C1282.7 (2)C13—Fe2—C16—C20166.1 (2)
C18—Fe2—C13—C12156.8 (2)C12—Fe2—C16—C17114.9 (2)
C17—Fe2—C13—C12114.6 (2)C11—Fe2—C16—C17158.5 (2)
C19—Fe2—C13—C12169.5 (3)C15—Fe2—C16—C17167.8 (3)
C20—Fe2—C13—C1240.8 (6)C18—Fe2—C16—C1737.8 (2)
C14—Fe2—C13—C12120.2 (3)C19—Fe2—C16—C1781.8 (3)
C12—Fe2—C13—C14120.2 (3)C20—Fe2—C16—C17119.4 (4)
C11—Fe2—C13—C1481.6 (2)C14—Fe2—C16—C1744.1 (7)
C16—Fe2—C13—C14166.6 (2)C13—Fe2—C16—C1774.5 (3)
C15—Fe2—C13—C1437.5 (2)C33—C34—C35—C310.3 (5)
C18—Fe2—C13—C1483.0 (3)Fe4—C34—C35—C3159.4 (3)
C17—Fe2—C13—C14125.2 (2)C33—C34—C35—Fe459.6 (3)
C19—Fe2—C13—C1449.4 (5)C31—Fe4—C35—C34119.1 (4)
C20—Fe2—C13—C14161.0 (5)C38—Fe4—C35—C34130.3 (3)
C50—Fe1—C4—C3154.7 (11)C33—Fe4—C35—C3437.8 (3)
C49—Fe1—C4—C3176 (2)C37—Fe4—C35—C34170.1 (3)
C48—Fe1—C4—C333.5 (15)C32—Fe4—C35—C3481.7 (3)
C51—Fe1—C4—C3111.1 (12)C36—Fe4—C35—C34159.9 (6)
C2—Fe1—C4—C337.6 (2)C39—Fe4—C35—C3487.6 (3)
C7—Fe1—C4—C357.7 (6)C40—Fe4—C35—C3453.6 (5)
C5—Fe1—C4—C3118.9 (3)C38—Fe4—C35—C31110.6 (3)
C1—Fe1—C4—C381.3 (2)C34—Fe4—C35—C31119.1 (4)
C50—Fe1—C4—C586.4 (11)C33—Fe4—C35—C3181.3 (3)
C49—Fe1—C4—C557 (2)C37—Fe4—C35—C3170.8 (3)
C48—Fe1—C4—C5152.4 (15)C32—Fe4—C35—C3137.5 (3)
C51—Fe1—C4—C5129.9 (12)C36—Fe4—C35—C3140.8 (8)
C2—Fe1—C4—C581.4 (2)C39—Fe4—C35—C31153.3 (3)
C7—Fe1—C4—C5176.6 (6)C40—Fe4—C35—C31172.7 (3)
C3—Fe1—C4—C5118.9 (3)C25—C21—C22—C230.0 (5)
C1—Fe1—C4—C537.6 (2)Fe3—C21—C22—C2360.0 (3)
C6—Fe1—C4—C5147.7 (5)C25—C21—C22—Fe359.9 (3)
Cu2—O4—C46—C450.6 (5)C29—Fe3—C22—C2136.5 (8)
Cu2—O4—C46—C5178.8 (2)C30—Fe3—C22—C21168.3 (3)
C14—C13—C12—C110.7 (4)C25—Fe3—C22—C2137.9 (3)
Fe2—C13—C12—C1159.5 (3)C24—Fe3—C22—C2181.9 (3)
C14—C13—C12—Fe258.7 (3)C28—Fe3—C22—C2171.3 (3)
C11—Fe2—C12—C13119.0 (3)C23—Fe3—C22—C21119.0 (4)
C16—Fe2—C12—C13125.6 (2)C26—Fe3—C22—C21155.3 (3)
C15—Fe2—C12—C1381.1 (2)C27—Fe3—C22—C21112.4 (3)
C18—Fe2—C12—C1350.5 (4)C29—Fe3—C22—C23155.5 (6)
C17—Fe2—C12—C1382.8 (3)C30—Fe3—C22—C2349.3 (4)
C19—Fe2—C12—C13164.5 (5)C21—Fe3—C22—C23119.0 (4)
C20—Fe2—C12—C13166.3 (2)C25—Fe3—C22—C2381.2 (3)
C14—Fe2—C12—C1337.0 (2)C24—Fe3—C22—C2337.2 (3)
C16—Fe2—C12—C11115.4 (2)C28—Fe3—C22—C23169.7 (2)
C15—Fe2—C12—C1137.9 (2)C26—Fe3—C22—C2385.6 (3)
C18—Fe2—C12—C11169.5 (3)C27—Fe3—C22—C23128.5 (2)
C17—Fe2—C12—C11158.2 (2)C30—C26—C27—C280.5 (4)
C19—Fe2—C12—C1145.5 (6)Fe3—C26—C27—C2858.7 (3)
C20—Fe2—C12—C1174.7 (3)C30—C26—C27—Fe358.2 (3)
C14—Fe2—C12—C1182.0 (2)C29—Fe3—C27—C2681.9 (2)
C13—Fe2—C12—C11119.0 (3)C30—Fe3—C27—C2637.3 (2)
C29—Fe3—C30—C26118.4 (3)C21—Fe3—C27—C26154.9 (2)
C21—Fe3—C30—C26162.0 (7)C22—Fe3—C27—C26111.8 (2)
C22—Fe3—C30—C2653.3 (4)C25—Fe3—C27—C26170.3 (3)
C25—Fe3—C30—C26169.1 (2)C24—Fe3—C27—C2638.9 (8)
C24—Fe3—C30—C26129.0 (2)C28—Fe3—C27—C26120.0 (3)
C28—Fe3—C30—C2680.7 (2)C23—Fe3—C27—C2671.2 (3)
C23—Fe3—C30—C2686.9 (3)C29—Fe3—C27—C2838.2 (2)
C27—Fe3—C30—C2636.9 (2)C30—Fe3—C27—C2882.7 (2)
C21—Fe3—C30—C2943.6 (8)C21—Fe3—C27—C2885.0 (3)
C22—Fe3—C30—C29171.7 (3)C22—Fe3—C27—C28128.1 (2)
C25—Fe3—C30—C2972.4 (3)C25—Fe3—C27—C2850.2 (4)
C24—Fe3—C30—C29112.5 (2)C24—Fe3—C27—C28158.9 (7)
C28—Fe3—C30—C2937.7 (2)C23—Fe3—C27—C28168.8 (2)
C23—Fe3—C30—C29154.7 (2)C26—Fe3—C27—C28120.0 (3)
C26—Fe3—C30—C29118.4 (3)C29—Fe3—C24—C23155.5 (2)
C27—Fe3—C30—C2981.6 (2)C30—Fe3—C24—C23111.8 (3)
Cu2—O3—C44—C453.3 (5)C21—Fe3—C24—C2381.4 (3)
Cu2—O3—C44—C11177.8 (2)C22—Fe3—C24—C2337.6 (3)
C13—C14—C15—C110.5 (4)C25—Fe3—C24—C23119.1 (4)
Fe2—C14—C15—C1159.4 (3)C28—Fe3—C24—C23169.4 (3)
C13—C14—C15—Fe258.9 (3)C26—Fe3—C24—C2371.5 (3)
C12—Fe2—C15—C1138.5 (2)C27—Fe3—C24—C2340.3 (8)
C16—Fe2—C15—C1147.5 (5)C29—Fe3—C24—C2585.5 (3)
C18—Fe2—C15—C11165.6 (2)C30—Fe3—C24—C25129.1 (3)
C17—Fe2—C15—C11161.1 (5)C21—Fe3—C24—C2537.6 (3)
C19—Fe2—C15—C11124.2 (2)C22—Fe3—C24—C2581.4 (3)
C20—Fe2—C15—C1181.7 (3)C28—Fe3—C24—C2550.3 (5)
C14—Fe2—C15—C11118.8 (3)C23—Fe3—C24—C25119.1 (4)
C13—Fe2—C15—C1181.9 (2)C26—Fe3—C24—C25169.4 (3)
C12—Fe2—C15—C1480.3 (2)C27—Fe3—C24—C25159.4 (7)
C11—Fe2—C15—C14118.8 (3)C22—C21—C25—C240.3 (5)
C16—Fe2—C15—C14166.3 (4)Fe3—C21—C25—C2459.5 (3)
C18—Fe2—C15—C1475.6 (3)C22—C21—C25—Fe359.8 (3)
C17—Fe2—C15—C1442.4 (6)C23—C24—C25—C210.5 (5)
C19—Fe2—C15—C14117.0 (2)Fe3—C24—C25—C2159.4 (3)
C20—Fe2—C15—C14159.5 (2)C23—C24—C25—Fe359.9 (3)
C13—Fe2—C15—C1436.9 (2)C29—Fe3—C25—C21128.8 (2)
Cu1—O1—C41—C425.3 (5)C30—Fe3—C25—C21170.3 (2)
Cu1—O1—C41—C40174.7 (2)C22—Fe3—C25—C2137.9 (2)
C31—Fe4—C36—C3770.0 (3)C24—Fe3—C25—C21119.1 (4)
C38—Fe4—C36—C3737.1 (2)C28—Fe3—C25—C2185.3 (3)
C34—Fe4—C36—C37171.5 (3)C23—Fe3—C25—C2181.7 (3)
C33—Fe4—C36—C37153.5 (3)C26—Fe3—C25—C21157.6 (6)
C35—Fe4—C36—C3737.3 (8)C27—Fe3—C25—C2150.6 (4)
C32—Fe4—C36—C37110.4 (3)C29—Fe3—C25—C24112.2 (3)
C39—Fe4—C36—C3780.9 (2)C30—Fe3—C25—C2470.7 (3)
C40—Fe4—C36—C37118.9 (3)C21—Fe3—C25—C24119.1 (4)
C31—Fe4—C36—C40171.1 (2)C22—Fe3—C25—C2481.2 (3)
C38—Fe4—C36—C4081.8 (2)C28—Fe3—C25—C24155.6 (3)
C34—Fe4—C36—C4052.5 (4)C23—Fe3—C25—C2437.3 (3)
C33—Fe4—C36—C4087.5 (3)C26—Fe3—C25—C2438.5 (8)
C37—Fe4—C36—C40118.9 (3)C27—Fe3—C25—C24169.7 (3)
C35—Fe4—C36—C40156.3 (6)C25—C24—C23—C220.5 (5)
C32—Fe4—C36—C40130.6 (3)Fe3—C24—C23—C2259.0 (3)
C39—Fe4—C36—C4038.1 (2)C25—C24—C23—Fe359.6 (3)
O3—C44—C45—C463.2 (6)C21—C22—C23—C240.4 (5)
C11—C44—C45—C46175.7 (4)Fe3—C22—C23—C2459.3 (3)
O4—C46—C45—C444.7 (6)C21—C22—C23—Fe359.7 (3)
C5—C46—C45—C44175.9 (3)C29—Fe3—C23—C2449.4 (4)
C3—C4—C5—C10.4 (4)C30—Fe3—C23—C2485.1 (3)
Fe1—C4—C5—C159.3 (3)C21—Fe3—C23—C2481.7 (3)
C3—C4—C5—C46179.9 (3)C22—Fe3—C23—C24119.4 (4)
Fe1—C4—C5—C46120.3 (4)C25—Fe3—C23—C2437.9 (3)
C3—C4—C5—Fe159.7 (3)C28—Fe3—C23—C24157.4 (7)
O4—C46—C5—C16.8 (5)C26—Fe3—C23—C24128.4 (3)
C45—C46—C5—C1173.8 (4)C27—Fe3—C23—C24168.5 (3)
O4—C46—C5—C4173.7 (3)C29—Fe3—C23—C22168.7 (3)
C45—C46—C5—C45.7 (6)C30—Fe3—C23—C22155.5 (2)
O4—C46—C5—Fe196.0 (4)C21—Fe3—C23—C2237.7 (3)
C45—C46—C5—Fe184.5 (4)C25—Fe3—C23—C2281.5 (3)
C50—Fe1—C5—C1126.5 (11)C24—Fe3—C23—C22119.4 (4)
C49—Fe1—C5—C182.4 (11)C28—Fe3—C23—C2238.0 (8)
C48—Fe1—C5—C133.1 (19)C26—Fe3—C23—C22112.2 (3)
C51—Fe1—C5—C1172.0 (13)C27—Fe3—C23—C2272.1 (3)
C2—Fe1—C5—C137.8 (2)C38—Fe4—C32—C3147.7 (5)
C4—Fe1—C5—C1119.2 (3)C34—Fe4—C32—C3181.6 (3)
C3—Fe1—C5—C181.8 (2)C33—Fe4—C32—C31119.6 (4)
C6—Fe1—C5—C1177.2 (6)C37—Fe4—C32—C3183.8 (3)
C8—Fe1—C5—C166.0 (5)C35—Fe4—C32—C3137.8 (3)
C50—Fe1—C5—C4114.3 (11)C36—Fe4—C32—C31127.6 (3)
C49—Fe1—C5—C4158.5 (11)C39—Fe4—C32—C31155.5 (8)
C48—Fe1—C5—C4152.3 (19)C40—Fe4—C32—C31168.4 (3)
C51—Fe1—C5—C468.8 (13)C31—Fe4—C32—C33119.6 (4)
C2—Fe1—C5—C481.4 (2)C38—Fe4—C32—C33167.3 (3)
C3—Fe1—C5—C437.4 (2)C34—Fe4—C32—C3338.0 (3)
C1—Fe1—C5—C4119.2 (3)C37—Fe4—C32—C33156.6 (3)
C6—Fe1—C5—C458.0 (6)C35—Fe4—C32—C3381.8 (3)
C8—Fe1—C5—C4174.8 (5)C36—Fe4—C32—C33112.8 (3)
C50—Fe1—C5—C467.3 (11)C39—Fe4—C32—C3335.9 (10)
C49—Fe1—C5—C4636.9 (12)C40—Fe4—C32—C3372.0 (3)
C48—Fe1—C5—C4686.1 (19)C18—C19—C20—C160.0 (5)
C51—Fe1—C5—C4652.8 (13)Fe2—C19—C20—C1659.1 (3)
C2—Fe1—C5—C46157.0 (3)C18—C19—C20—Fe259.1 (3)
C4—Fe1—C5—C46121.6 (4)C17—C16—C20—C190.2 (5)
C3—Fe1—C5—C46159.0 (3)Fe2—C16—C20—C1959.4 (3)
C1—Fe1—C5—C46119.2 (4)C17—C16—C20—Fe259.6 (3)
C6—Fe1—C5—C4663.6 (7)C12—Fe2—C20—C19167.6 (2)
C8—Fe1—C5—C4653.2 (6)C11—Fe2—C20—C19125.6 (2)
C29—C30—C26—C270.7 (4)C16—Fe2—C20—C19119.0 (4)
Fe3—C30—C26—C2759.0 (3)C15—Fe2—C20—C1982.8 (3)
C29—C30—C26—Fe359.7 (3)C18—Fe2—C20—C1937.6 (2)
C29—Fe3—C26—C2781.6 (2)C17—Fe2—C20—C1981.2 (3)
C30—Fe3—C26—C27120.2 (3)C14—Fe2—C20—C1949.4 (5)
C21—Fe3—C26—C2751.4 (4)C13—Fe2—C20—C19160.9 (5)
C22—Fe3—C26—C2786.1 (3)C12—Fe2—C20—C1673.3 (3)
C25—Fe3—C26—C27159.9 (6)C11—Fe2—C20—C16115.4 (3)
C24—Fe3—C26—C27169.0 (2)C15—Fe2—C20—C16158.2 (2)
C28—Fe3—C26—C2737.4 (2)C18—Fe2—C20—C1681.4 (3)
C23—Fe3—C26—C27129.0 (2)C17—Fe2—C20—C1637.8 (3)
C29—Fe3—C26—C3038.6 (2)C19—Fe2—C20—C16119.0 (4)
C21—Fe3—C26—C30171.5 (3)C14—Fe2—C20—C16168.4 (3)
C22—Fe3—C26—C30153.8 (2)C13—Fe2—C20—C1641.9 (7)
C25—Fe3—C26—C3039.8 (8)C30—C29—C28—C270.3 (4)
C24—Fe3—C26—C3070.9 (3)C43—C29—C28—C27176.7 (3)
C28—Fe3—C26—C3082.7 (2)Fe3—C29—C28—C2759.5 (3)
C23—Fe3—C26—C30110.8 (2)C30—C29—C28—Fe359.2 (3)
C27—Fe3—C26—C30120.2 (3)C43—C29—C28—Fe3117.2 (4)
C50—Fe1—C2—C152 (3)C26—C27—C28—C290.1 (4)
C49—Fe1—C2—C180.0 (11)Fe3—C27—C28—C2958.8 (3)
C48—Fe1—C2—C1119.8 (9)C26—C27—C28—Fe358.9 (3)
C51—Fe1—C2—C1166.5 (13)C30—Fe3—C28—C2938.0 (2)
C7—Fe1—C2—C1135.3 (5)C21—Fe3—C28—C29128.3 (2)
C4—Fe1—C2—C182.6 (2)C22—Fe3—C28—C29168.6 (2)
C5—Fe1—C2—C138.0 (2)C25—Fe3—C28—C2985.4 (3)
C3—Fe1—C2—C1119.7 (3)C24—Fe3—C28—C2950.8 (5)
C6—Fe1—C2—C1173.9 (5)C23—Fe3—C28—C29160.6 (6)
C8—Fe1—C2—C191.7 (5)C26—Fe3—C28—C2981.8 (2)
C50—Fe1—C2—C3171 (3)C27—Fe3—C28—C29118.7 (3)
C49—Fe1—C2—C3160.2 (11)C29—Fe3—C28—C27118.7 (3)
C48—Fe1—C2—C3120.5 (9)C30—Fe3—C28—C2780.7 (2)
C51—Fe1—C2—C346.8 (13)C21—Fe3—C28—C27113.0 (3)
C7—Fe1—C2—C3105.0 (5)C22—Fe3—C28—C2772.7 (3)
C4—Fe1—C2—C337.1 (2)C25—Fe3—C28—C27155.8 (3)
C5—Fe1—C2—C381.7 (2)C24—Fe3—C28—C27169.5 (4)
C1—Fe1—C2—C3119.7 (3)C23—Fe3—C28—C2741.9 (8)
C6—Fe1—C2—C366.3 (5)C26—Fe3—C28—C2736.9 (2)
C8—Fe1—C2—C3148.6 (5)C31—C32—C33—C340.6 (5)
C37—C36—C40—C390.4 (4)Fe4—C32—C33—C3459.8 (3)
Fe4—C36—C40—C3958.8 (2)C31—C32—C33—Fe459.2 (3)
C37—C36—C40—C41179.7 (3)C35—C34—C33—C320.2 (5)
Fe4—C36—C40—C41120.5 (4)Fe4—C34—C33—C3259.9 (3)
C37—C36—C40—Fe459.2 (3)C35—C34—C33—Fe459.8 (3)
O1—C41—C40—C36173.0 (3)C31—Fe4—C33—C3237.2 (3)
C42—C41—C40—C367.0 (6)C38—Fe4—C33—C32148.4 (7)
O1—C41—C40—C397.8 (5)C34—Fe4—C33—C32118.6 (4)
C42—C41—C40—C39172.2 (4)C37—Fe4—C33—C3247.6 (5)
O1—C41—C40—Fe495.9 (4)C35—Fe4—C33—C3280.9 (3)
C42—C41—C40—Fe484.1 (4)C36—Fe4—C33—C3285.4 (3)
C31—Fe4—C40—C3634.1 (9)C39—Fe4—C33—C32171.7 (2)
C38—Fe4—C40—C3681.5 (2)C40—Fe4—C33—C32129.6 (3)
C34—Fe4—C40—C36155.2 (2)C31—Fe4—C33—C3481.4 (3)
C33—Fe4—C40—C36111.6 (3)C38—Fe4—C33—C3429.8 (9)
C37—Fe4—C40—C3638.0 (2)C37—Fe4—C33—C34166.2 (3)
C35—Fe4—C40—C36168.2 (3)C35—Fe4—C33—C3437.7 (3)
C32—Fe4—C40—C3670.6 (3)C32—Fe4—C33—C34118.6 (4)
C39—Fe4—C40—C36119.1 (3)C36—Fe4—C33—C34156.0 (2)
C31—Fe4—C40—C39153.2 (7)C39—Fe4—C33—C3469.7 (3)
C38—Fe4—C40—C3937.6 (2)C40—Fe4—C33—C34111.8 (3)
C34—Fe4—C40—C3985.7 (3)C19—C18—C17—C160.3 (5)
C33—Fe4—C40—C39129.3 (3)Fe2—C18—C17—C1659.1 (3)
C37—Fe4—C40—C3981.1 (2)C19—C18—C17—Fe259.4 (3)
C35—Fe4—C40—C3949.1 (4)C20—C16—C17—C180.3 (5)
C32—Fe4—C40—C39170.3 (3)Fe2—C16—C17—C1859.4 (3)
C36—Fe4—C40—C39119.1 (3)C20—C16—C17—Fe259.7 (3)
C31—Fe4—C40—C4188.9 (8)C12—Fe2—C17—C18158.7 (2)
C38—Fe4—C40—C41155.5 (4)C11—Fe2—C17—C18166.5 (3)
C34—Fe4—C40—C4132.2 (4)C16—Fe2—C17—C18118.8 (3)
C33—Fe4—C40—C4111.4 (4)C15—Fe2—C17—C1842.9 (6)
C37—Fe4—C40—C41161.0 (4)C19—Fe2—C17—C1837.7 (2)
C35—Fe4—C40—C4168.8 (5)C20—Fe2—C17—C1881.2 (3)
C32—Fe4—C40—C4152.4 (4)C14—Fe2—C17—C1875.9 (3)
C36—Fe4—C40—C41123.0 (4)C13—Fe2—C17—C18116.4 (2)
C39—Fe4—C40—C41117.9 (4)C12—Fe2—C17—C1682.5 (3)
C26—C30—C29—C280.6 (4)C11—Fe2—C17—C1647.7 (5)
Fe3—C30—C29—C2859.8 (3)C15—Fe2—C17—C16161.7 (5)
C26—C30—C29—C43176.8 (3)C18—Fe2—C17—C16118.8 (3)
Fe3—C30—C29—C43116.4 (4)C19—Fe2—C17—C1681.1 (3)
C26—C30—C29—Fe360.4 (3)C20—Fe2—C17—C1637.6 (2)
C30—Fe3—C29—C28119.3 (3)C14—Fe2—C17—C16165.4 (2)
C21—Fe3—C29—C2872.3 (3)C13—Fe2—C17—C16124.8 (2)
C22—Fe3—C29—C2842.8 (8)C39—C38—C37—C360.3 (4)
C25—Fe3—C29—C28112.5 (3)Fe4—C38—C37—C3659.1 (3)
C24—Fe3—C29—C28155.5 (2)C39—C38—C37—Fe459.4 (3)
C23—Fe3—C29—C28171.0 (3)C40—C36—C37—C380.5 (4)
C26—Fe3—C29—C2881.3 (2)Fe4—C36—C37—C3859.1 (3)
C27—Fe3—C29—C2838.0 (2)C40—C36—C37—Fe459.6 (3)
C21—Fe3—C29—C30168.4 (2)C31—Fe4—C37—C38110.6 (3)
C22—Fe3—C29—C30162.1 (7)C34—Fe4—C37—C3844.0 (7)
C25—Fe3—C29—C30128.2 (2)C33—Fe4—C37—C38174.8 (3)
C24—Fe3—C29—C3085.2 (3)C35—Fe4—C37—C3870.8 (3)
C28—Fe3—C29—C30119.3 (3)C32—Fe4—C37—C38152.6 (3)
C23—Fe3—C29—C3051.7 (4)C36—Fe4—C37—C38119.9 (3)
C26—Fe3—C29—C3038.0 (2)C39—Fe4—C37—C3837.4 (2)
C27—Fe3—C29—C3081.3 (2)C40—Fe4—C37—C3881.9 (2)
C30—Fe3—C29—C43122.1 (4)C31—Fe4—C37—C36129.5 (2)
C21—Fe3—C29—C4346.3 (4)C38—Fe4—C37—C36119.9 (3)
C22—Fe3—C29—C4375.8 (8)C34—Fe4—C37—C36163.9 (6)
C25—Fe3—C29—C436.1 (4)C33—Fe4—C37—C3654.9 (4)
C24—Fe3—C29—C4336.9 (4)C35—Fe4—C37—C36169.3 (2)
C28—Fe3—C29—C43118.6 (4)C32—Fe4—C37—C3687.6 (3)
C23—Fe3—C29—C4370.4 (5)C39—Fe4—C37—C3682.4 (2)
C26—Fe3—C29—C43160.1 (4)C40—Fe4—C37—C3638.0 (2)
C27—Fe3—C29—C43156.5 (4)C33—C32—C31—C350.7 (5)
C5—C4—C3—C20.3 (4)Fe4—C32—C31—C3559.9 (3)
Fe1—C4—C3—C259.0 (3)C33—C32—C31—Fe459.1 (3)
C5—C4—C3—Fe159.3 (3)C34—C35—C31—C320.6 (5)
C1—C2—C3—C40.1 (4)Fe4—C35—C31—C3260.0 (3)
Fe1—C2—C3—C459.2 (3)C34—C35—C31—Fe459.4 (3)
C1—C2—C3—Fe159.4 (3)C38—Fe4—C31—C32155.3 (3)
C50—Fe1—C3—C455.4 (17)C34—Fe4—C31—C3281.4 (3)
C49—Fe1—C3—C4175 (2)C33—Fe4—C31—C3237.5 (3)
C48—Fe1—C3—C4165.6 (8)C37—Fe4—C31—C32112.7 (3)
C51—Fe1—C3—C484.2 (10)C35—Fe4—C31—C32119.0 (4)
C2—Fe1—C3—C4119.7 (3)C36—Fe4—C31—C3272.7 (3)
C7—Fe1—C3—C4147.4 (4)C39—Fe4—C31—C32171.2 (3)
C5—Fe1—C3—C438.4 (2)C40—Fe4—C31—C3244.7 (9)
C1—Fe1—C3—C482.4 (2)C38—Fe4—C31—C3585.7 (3)
C6—Fe1—C3—C4104.0 (5)C34—Fe4—C31—C3537.6 (3)
C8—Fe1—C3—C4175.9 (7)C33—Fe4—C31—C3581.5 (3)
C50—Fe1—C3—C2175.1 (16)C37—Fe4—C31—C35128.3 (3)
C49—Fe1—C3—C256 (2)C32—Fe4—C31—C35119.0 (4)
C48—Fe1—C3—C274.7 (8)C36—Fe4—C31—C35168.3 (3)
C51—Fe1—C3—C2156.0 (10)C39—Fe4—C31—C3552.1 (5)
C7—Fe1—C3—C292.9 (5)C40—Fe4—C31—C35163.8 (7)
C4—Fe1—C3—C2119.7 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C19—H···Cga0.932.773.63154
C49—H···Cgb0.932.843.71155
C9—H···Cgb0.932.983.68134
C34—H···Cgc0.932.633.55170
C21—H···Cgd0.933.153.82130
C17—H···O1e0.932.733.30121
C51—H···O2e0.932.413.26153
C32—H···O4f0.932.553.45163

Experimental details

(I)(II)
Crystal data
Chemical formula[CuFe2(C5H5)2(C9H8O2)2][CuFe4(C5H5)4(C13H9O2)2]
Mr601.73941.70
Crystal system, space groupMonoclinic, C2/cTriclinic, P1
Temperature (K)203200
a, b, c (Å)29.6410 (3), 7.4132 (1), 10.5656 (2)11.9182 (2), 12.8881 (1), 12.9097 (1)
α, β, γ (°)90, 92.109 (1), 9089.670 (1), 78.617 (1), 76.987 (1)
V3)2320.06 (6)1892.49 (4)
Z42
Radiation typeMo KαMo Kα
µ (mm1)2.182.10
Crystal size (mm)0.38 × 0.28 × 0.030.16 × 0.14 × 0.1
Data collection
DiffractometerSiemens SMART CCD area-detector
diffractometer
Siemens SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
SADABS; Sheldrick, 1997
Multi-scan
SADABS; Sheldrick, 1997
Tmin, Tmax0.655, 0.9520.650, 0.803
No. of measured, independent and
observed [I > 2σ(I)] reflections
7126, 2558, 2195 17654, 7556, 5859
Rint0.0210.038
(sin θ/λ)max1)0.6490.625
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.100, 1.21 0.048, 0.127, 1.07
No. of reflections25587556
No. of parameters161545
No. of restraints0140
H-atom treatmentH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.50, 0.690.95, 1.23

Computer programs: SMART (Siemens, 1995), SAINT (Siemens, 1995), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).

Selected geometric parameters (Å, º) for (I) top
Cu—O11.9033 (18)O2—C41.285 (3)
Cu—O21.9182 (16)C2—C31.395 (3)
O1—C21.280 (3)C3—C41.396 (3)
O1—Cu—O293.91 (7)O1—Cu—O2i86.09 (7)
Symmetry code: (i) x+1/2, y+1/2, z+1.
Selected geometric parameters (Å, º) for (II) top
Cu1—O11.911 (3)Cu2—O41.912 (2)
Cu1—O21.919 (2)Cu2—O31.926 (3)
O1i—Cu1—O286.68 (11)O4ii—Cu2—O386.38 (10)
O1—Cu1—O293.32 (11)O4—Cu2—O393.62 (10)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z.
Hydrogen-bond geometry (Å, º) for (II) top
D—H···AD—HH···AD···AD—H···A
C19—H···Cga0.932.773.63154
C49—H···Cgb0.932.843.71155
C9—H···Cgb0.932.983.68134
C34—H···Cgc0.932.633.55170
C21—H···Cgd0.933.153.82130
C17—H···O1e0.932.733.30121
C51—H···O2e0.932.413.26153
C32—H···O4f0.932.553.45163
C—H···O and C—H···π contacts in (II) (Å, °) top
D-H.·AH···AD-H.·AD-H.·AH.·AD-H.·A
C19-H.·Cga2.77154.0C49-H.·Cgb2.84155.2
C9-H.·Cgb2.98133.8C34-H.·Cgc2.63168.6
C21-H.·Cgd3.15130.4C16-H.·O12.92113.7
C17-H.·O12.73121.1C51-H.·O22.41153.0
C6-H.·O22.67140.0C23-H.·O32.65128.0
C32-H.·O42.55163.4
Centroids of the (a) C31–C35, (b) C21–C25, (c) C6–C10 and (d) C16–C20 rings.
 

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