Di-μ₂-carbonyl-octa­carbon­yl[μ₂-η²,η²-N-cyclo­hexyl-N-(2-thienylmethyl­ene)amine]tetra­iron(0)

In the title compound, [Fe₄(C₁₁H₁₄NS)₂(CO)₁₀], the four Fe atoms show a non-linear arrangement with a planar central Fe₂(μ₂-CO)₂ core. The imine ligands are situated on the same side of the transition metal chain with the N atoms in a trans configuration with respect to each other.

Key indicators

• Single-crystal X-ray study
• T = 213 K
• Mean [sigma](C-C) = 0.011 Å
• R factor = 0.066
• wR factor = 0.136
• Data-to-parameter ratio = 16.1

checkCIF/PLATON results

No syntax errors found



Datablock: 3


Alert level B
PLAT220_ALERT_2_B Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       4.07 Ratio

Author Response: Some carbon atoms of the cyclohexyl substituents show quite high temperature factors. Nevertheless, it was not possible to refine them in two statistically disordered conformations.

Alert level C
PLAT026_ALERT_3_C Ratio Observed / Unique Reflections too Low ....         49 Perc.

Author Response: It was a very small crystal and at the time it was measured we did not have a CCD device. The data parameter ratio is not perfect but from my point of view acceptable. Looking at standard deviations the structure seems to be well refined.

PLAT213_ALERT_2_C Atom C20     has ADP max/min Ratio .............       3.50 oblate

Author Response: This is also due to the fact that the cyclohexyl residue obviously is quite flexible although it was not possible to refine this in terms of a diesorder.

PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.27 Ratio

Author Response: This is also due to the fact that the cyclohexyl residue obviously is quite flexible although it was not possible to refine this in terms of a diesorder. The corresponding H atoms have been refined with displacement parameters of 1.5 times the carbon atom they are bound to, so they also are quite high for parts of the cyclohexyl groups.

PLAT320_ALERT_2_C Check Hybridisation of  C27    in Main Residue .          ?
PLAT320_ALERT_2_C Check Hybridisation of  C28    in Main Residue .          ?
PLAT322_ALERT_2_C Check Hybridisation of  S1     in Main Residue .          ?
PLAT322_ALERT_2_C Check Hybridisation of  S2     in Main Residue .          ?
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         11

Author Response: This is also due to the fact that the cyclohexyl residue obviously is quite flexible although it was not possible to refine this in terms of a diesorder.

PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond  C3     -   C4     ...       1.38 Ang.

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   9 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   7 ALERT type 2 Indicator that the structure model may be wrong or deficient
   3 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: SET4 (Boer et al., 1984); data reduction: MolEN (Enraf–Nonius, 1990); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1990); software used to prepare material for publication: SHELXL97.

Di-µ₂-carbonyl-octacarbonyl[µ₂-η²,η²-N-cyclohexyl-N-(2- thienylmethylene)amido]tetrairon

Crystal data

[Fe4(C11H14NS)2(CO)10]	F(000) = 3600
Mr = 888.08	Dx = 1.676 Mg m^−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 25 reflections
a = 21.924 (4) Å	θ = 12.4–21.0°
b = 13.520 (2) Å	µ = 1.79 mm^−1
c = 23.743 (4) Å	T = 213 K
V = 7038 (2) Å^3	Cuboid, red–brown
Z = 8	0.2 × 0.2 × 0.07 mm

Data collection

Enraf–Nonius CAD-4 diffractometer	3568 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.069
Graphite monochromator	θmax = 26.5°, θmin = 2.0°
ω/2θ scans	h = −1→27
Absorption correction: ψ scan (North et al., 1968)	k = −1→16
Tmin = 0.725, Tmax = 0.886	l = −29→1
8715 measured reflections	3 standard reflections every 60 min
7277 independent reflections	intensity decay: 0.5%

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.066	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.136	H-atom parameters constrained
S = 0.99	w = 1/[σ^2(Fo^2) + (0.0291P)^2] where P = (Fo^2 + 2Fc^2)/3
7277 reflections	(Δ/σ)max < 0.001
452 parameters	Δρmax = 0.53 e Å^−3
0 restraints	Δρmin = −0.56 e Å^−3

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.08773 (4)	0.34052 (9)	0.24017 (4)	0.0250 (2)
Fe2	0.11528 (4)	0.34229 (8)	0.34210 (4)	0.0189 (2)
Fe3	0.17301 (4)	0.34180 (8)	0.43594 (4)	0.0190 (2)
Fe4	0.20726 (4)	0.33514 (8)	0.53550 (4)	0.0246 (2)
S2	0.17070 (9)	0.59692 (14)	0.32700 (9)	0.0327 (5)
C1	0.0747 (3)	0.5554 (6)	0.5063 (3)	0.035 (2)
H1	0.0393	0.5903	0.5165	0.053*
C2	0.0924 (3)	0.4723 (6)	0.5319 (3)	0.0345 (19)
H2	0.0698	0.4410	0.5604	0.052*
C3	0.1503 (3)	0.4355 (5)	0.5110 (3)	0.0259 (18)
C4	0.1716 (3)	0.4952 (5)	0.4679 (3)	0.0228 (16)
C5	0.2292 (3)	0.4699 (5)	0.4447 (3)	0.0176 (15)
H5	0.2476	0.5037	0.4146	0.05 (2)*
N1	0.2545 (2)	0.3911 (4)	0.4712 (2)	0.0171 (12)
C6	0.3199 (3)	0.3646 (5)	0.4596 (3)	0.0223 (16)
H6	0.3221	0.2916	0.4572	0.033*
C7	0.3588 (3)	0.3961 (6)	0.5102 (3)	0.0311 (18)
H7A	0.3565	0.4681	0.5146	0.047*
H7B	0.3424	0.3657	0.5445	0.047*
C8	0.4254 (3)	0.3652 (6)	0.5026 (4)	0.046 (2)
H8A	0.4497	0.3912	0.5339	0.069*
H8B	0.4282	0.2929	0.5034	0.069*
C9	0.4511 (3)	0.4033 (7)	0.4475 (4)	0.051 (2)
H9A	0.4927	0.3785	0.4427	0.077*
H9B	0.4528	0.4757	0.4486	0.077*
C10	0.4122 (3)	0.3707 (6)	0.3975 (3)	0.044 (2)
H10A	0.4131	0.2984	0.3945	0.066*
H10B	0.4290	0.3984	0.3627	0.066*
C11	0.3462 (3)	0.4056 (5)	0.4050 (3)	0.0299 (18)
H11A	0.3450	0.4781	0.4059	0.045*
H11B	0.3215	0.3831	0.3731	0.045*
S1	0.12252 (9)	0.59333 (15)	0.45261 (9)	0.0328 (5)
C12	0.2243 (3)	0.5522 (6)	0.2798 (3)	0.038 (2)
H12	0.2616	0.5839	0.2723	0.057*
C13	0.2070 (3)	0.4678 (6)	0.2552 (3)	0.037 (2)
H13	0.2320	0.4336	0.2297	0.055*
C14	0.1477 (3)	0.4333 (5)	0.2705 (3)	0.0221 (16)
C15	0.1228 (3)	0.4982 (5)	0.3108 (3)	0.0242 (17)
C16	0.0641 (3)	0.4742 (5)	0.3302 (3)	0.0244 (16)
H16	0.0444	0.5093	0.3591	0.037*
N2	0.0385 (2)	0.3960 (4)	0.3035 (2)	0.0221 (13)
C17	−0.0267 (3)	0.3778 (5)	0.3189 (3)	0.0284 (18)
H17	−0.0352	0.4139	0.3543	0.043*
C18	−0.0425 (3)	0.2697 (6)	0.3283 (3)	0.036 (2)
H18A	−0.0163	0.2422	0.3578	0.054*
H18B	−0.0354	0.2323	0.2936	0.054*
C19	−0.1101 (3)	0.2596 (7)	0.3459 (4)	0.049 (2)
H19A	−0.1206	0.1897	0.3506	0.074*
H19B	−0.1169	0.2934	0.3819	0.074*
C20	−0.1496 (3)	0.3059 (8)	0.3002 (4)	0.066 (3)
H20A	−0.1450	0.2677	0.2655	0.099*
H20B	−0.1925	0.3019	0.3118	0.099*
C21	−0.1340 (3)	0.4114 (8)	0.2886 (5)	0.072 (3)
H21A	−0.1428	0.4514	0.3220	0.108*
H21B	−0.1592	0.4359	0.2576	0.108*
C22	−0.0664 (3)	0.4223 (7)	0.2731 (4)	0.050 (3)
H22A	−0.0584	0.3886	0.2372	0.076*
H22B	−0.0564	0.4924	0.2684	0.076*
C23	0.2556 (3)	0.2279 (6)	0.5475 (3)	0.0298 (18)
O1	0.2823 (2)	0.1567 (4)	0.5588 (2)	0.0471 (15)
C24	0.1456 (4)	0.2753 (6)	0.5690 (3)	0.036 (2)
O2	0.1030 (3)	0.2399 (5)	0.5884 (2)	0.0599 (19)
C25	0.2337 (3)	0.4096 (6)	0.5923 (3)	0.0313 (18)
O3	0.2492 (3)	0.4596 (5)	0.6282 (2)	0.0593 (18)
C26	0.1726 (3)	0.2166 (6)	0.4509 (3)	0.0333 (19)
O4	0.1711 (3)	0.1325 (4)	0.4580 (2)	0.0530 (18)
C27	0.0868 (3)	0.3329 (5)	0.4177 (3)	0.0227 (15)
O5	0.0409 (2)	0.3243 (4)	0.4426 (2)	0.0391 (14)
C28	0.1988 (3)	0.3110 (5)	0.3607 (3)	0.0237 (17)
O6	0.2426 (2)	0.2811 (4)	0.3376 (2)	0.0376 (14)
C29	0.1062 (3)	0.2143 (6)	0.3306 (3)	0.0300 (18)
O7	0.1011 (3)	0.1303 (4)	0.3270 (2)	0.0486 (17)
C30	0.1496 (3)	0.2739 (6)	0.2113 (3)	0.036 (2)
O8	0.1909 (3)	0.2302 (5)	0.1951 (3)	0.0599 (19)
C31	0.0364 (4)	0.2447 (6)	0.2158 (3)	0.036 (2)
O9	0.0088 (3)	0.1845 (4)	0.1937 (3)	0.0568 (18)
C32	0.0743 (4)	0.4257 (6)	0.1839 (3)	0.041 (2)
O10	0.0675 (3)	0.4819 (5)	0.1493 (3)	0.068 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.0194 (5)	0.0353 (6)	0.0203 (5)	0.0009 (6)	−0.0013 (4)	−0.0033 (6)
Fe2	0.0144 (5)	0.0241 (5)	0.0184 (5)	0.0009 (5)	−0.0013 (4)	−0.0016 (5)
Fe3	0.0181 (5)	0.0222 (5)	0.0167 (5)	0.0015 (5)	−0.0008 (4)	−0.0021 (5)
Fe4	0.0221 (5)	0.0347 (6)	0.0169 (5)	−0.0014 (6)	0.0006 (4)	−0.0001 (5)
S2	0.0310 (10)	0.0275 (11)	0.0397 (12)	−0.0087 (9)	−0.0040 (9)	0.0016 (10)
C1	0.023 (4)	0.037 (5)	0.046 (5)	0.007 (4)	0.001 (4)	−0.016 (4)
C2	0.020 (4)	0.047 (5)	0.036 (5)	0.000 (4)	0.000 (4)	−0.019 (4)
C3	0.016 (3)	0.040 (5)	0.022 (4)	0.008 (3)	0.006 (3)	−0.011 (4)
C4	0.021 (3)	0.028 (4)	0.019 (4)	0.000 (3)	−0.006 (3)	−0.006 (3)
C5	0.016 (3)	0.014 (3)	0.023 (4)	−0.003 (3)	−0.001 (3)	0.000 (3)
N1	0.016 (3)	0.020 (3)	0.015 (3)	0.001 (3)	0.001 (2)	−0.003 (2)
C6	0.012 (3)	0.025 (4)	0.029 (4)	0.007 (3)	−0.001 (3)	−0.004 (3)
C7	0.026 (4)	0.036 (5)	0.032 (4)	0.001 (4)	−0.002 (3)	0.006 (4)
C8	0.022 (4)	0.051 (6)	0.065 (6)	−0.001 (4)	−0.001 (4)	0.002 (5)
C9	0.022 (4)	0.063 (6)	0.068 (7)	−0.001 (5)	0.012 (4)	−0.005 (5)
C10	0.031 (4)	0.044 (5)	0.057 (6)	−0.001 (4)	0.020 (4)	−0.011 (4)
C11	0.025 (4)	0.030 (4)	0.034 (5)	−0.005 (4)	0.006 (3)	−0.004 (4)
S1	0.0276 (10)	0.0279 (10)	0.0431 (12)	0.0086 (9)	−0.0052 (9)	−0.0087 (10)
C12	0.022 (4)	0.048 (5)	0.043 (5)	−0.007 (4)	0.005 (4)	0.012 (4)
C13	0.030 (4)	0.052 (5)	0.029 (4)	0.004 (4)	0.009 (4)	0.001 (4)
C14	0.010 (3)	0.037 (4)	0.019 (4)	0.000 (3)	−0.003 (3)	0.003 (3)
C15	0.019 (4)	0.028 (4)	0.026 (4)	−0.005 (3)	0.001 (3)	0.005 (3)
C16	0.019 (4)	0.030 (4)	0.023 (4)	0.007 (3)	−0.006 (3)	−0.005 (4)
N2	0.015 (3)	0.028 (3)	0.024 (3)	0.003 (3)	−0.003 (3)	0.001 (3)
C17	0.009 (3)	0.039 (4)	0.037 (5)	0.002 (3)	0.000 (3)	−0.004 (4)
C18	0.017 (4)	0.043 (5)	0.047 (5)	0.001 (4)	0.007 (4)	−0.001 (4)
C19	0.018 (4)	0.066 (6)	0.065 (6)	−0.019 (4)	0.005 (4)	0.000 (5)
C20	0.012 (4)	0.093 (8)	0.093 (8)	−0.018 (5)	0.001 (5)	0.004 (7)
C21	0.013 (4)	0.100 (9)	0.103 (9)	0.000 (5)	−0.003 (5)	0.013 (8)
C22	0.014 (4)	0.067 (7)	0.071 (7)	0.006 (4)	−0.005 (4)	0.023 (6)
C23	0.032 (4)	0.037 (5)	0.021 (4)	−0.007 (4)	0.000 (3)	−0.005 (4)
O1	0.052 (4)	0.046 (4)	0.043 (3)	0.014 (3)	−0.010 (3)	0.002 (3)
C24	0.039 (5)	0.044 (5)	0.024 (4)	−0.002 (4)	−0.006 (4)	0.013 (4)
O2	0.038 (4)	0.101 (6)	0.041 (4)	−0.017 (4)	0.011 (3)	0.017 (4)
C25	0.031 (4)	0.038 (5)	0.025 (4)	−0.002 (4)	−0.002 (3)	0.001 (4)
O3	0.069 (4)	0.071 (5)	0.038 (4)	0.001 (4)	−0.015 (3)	−0.023 (3)
C26	0.032 (5)	0.039 (5)	0.028 (5)	0.000 (4)	−0.007 (4)	−0.005 (4)
O4	0.083 (5)	0.026 (3)	0.050 (4)	0.002 (3)	−0.021 (4)	0.000 (3)
C27	0.020 (3)	0.028 (4)	0.020 (3)	−0.003 (4)	−0.002 (3)	0.000 (4)
O5	0.019 (2)	0.066 (4)	0.032 (3)	−0.011 (3)	0.008 (2)	−0.008 (3)
C28	0.025 (4)	0.029 (4)	0.017 (4)	0.003 (3)	−0.005 (3)	−0.007 (3)
O6	0.023 (3)	0.056 (4)	0.033 (3)	0.013 (3)	0.004 (2)	−0.016 (3)
C29	0.030 (4)	0.036 (5)	0.023 (4)	0.011 (4)	−0.007 (4)	−0.001 (4)
O7	0.062 (4)	0.031 (3)	0.053 (4)	−0.004 (3)	−0.009 (3)	−0.007 (3)
C30	0.028 (4)	0.052 (5)	0.029 (5)	0.001 (4)	0.001 (4)	−0.011 (4)
O8	0.040 (4)	0.090 (5)	0.049 (4)	0.025 (4)	−0.006 (3)	−0.028 (4)
C31	0.031 (4)	0.044 (5)	0.031 (5)	0.004 (4)	−0.003 (4)	−0.011 (4)
O9	0.055 (4)	0.061 (4)	0.054 (4)	−0.018 (3)	−0.001 (3)	−0.024 (3)
C32	0.038 (5)	0.050 (6)	0.034 (5)	−0.002 (4)	−0.015 (4)	0.003 (4)
O10	0.086 (5)	0.070 (5)	0.048 (4)	−0.013 (4)	−0.023 (4)	0.028 (4)

Geometric parameters (Å, º)

Fe1—C30	1.766 (8)	C8—H8A	0.9800
Fe1—C32	1.788 (8)	C8—H8B	0.9800
Fe1—C31	1.810 (8)	C9—C10	1.526 (10)
Fe1—C14	1.955 (7)	C9—H9A	0.9800
Fe1—N2	1.998 (5)	C9—H9B	0.9800
Fe1—Fe2	2.4945 (14)	C10—C11	1.533 (9)
Fe2—C29	1.764 (8)	C10—H10A	0.9800
Fe2—C27	1.904 (6)	C10—H10B	0.9800
Fe2—C28	1.931 (7)	C11—H11A	0.9800
Fe2—N2	2.050 (5)	C11—H11B	0.9800
Fe2—C16	2.126 (7)	C12—C13	1.338 (10)
Fe2—C14	2.216 (7)	C12—H12	0.9400
Fe2—C15	2.241 (7)	C13—C14	1.427 (9)
Fe2—Fe3	2.5625 (13)	C13—H13	0.9400
Fe3—C26	1.729 (9)	C14—C15	1.410 (9)
Fe3—C28	1.919 (7)	C15—C16	1.404 (9)
Fe3—C27	1.942 (6)	C16—N2	1.355 (8)
Fe3—N1	2.083 (5)	C16—H16	0.9400
Fe3—C5	2.135 (6)	N2—C17	1.495 (8)
Fe3—C4	2.209 (7)	C17—C18	1.519 (10)
Fe3—C3	2.242 (7)	C17—C22	1.516 (9)
Fe3—Fe4	2.4819 (13)	C17—H17	0.9900
Fe4—C24	1.764 (8)	C18—C19	1.545 (9)
Fe4—C25	1.780 (8)	C18—H18A	0.9800
Fe4—C23	1.819 (8)	C18—H18B	0.9800
Fe4—C3	1.934 (7)	C19—C20	1.523 (11)
Fe4—N1	1.994 (5)	C19—H19A	0.9800
S2—C12	1.733 (8)	C19—H19B	0.9800
S2—C15	1.741 (7)	C20—C21	1.492 (13)
C1—C2	1.336 (10)	C20—H20A	0.9800
C1—S1	1.728 (8)	C20—H20B	0.9800
C1—H1	0.9400	C21—C22	1.534 (10)
C2—C3	1.451 (9)	C21—H21A	0.9800
C2—H2	0.9400	C21—H21B	0.9800
C3—C4	1.383 (9)	C22—H22A	0.9800
C4—C5	1.420 (8)	C22—H22B	0.9800
C4—S1	1.746 (7)	C23—O1	1.158 (8)
C5—N1	1.356 (7)	C24—O2	1.146 (8)
C5—H5	0.9400	C25—O3	1.140 (8)
N1—C6	1.503 (7)	C26—O4	1.150 (9)
C6—C11	1.522 (9)	C27—O5	1.174 (7)
C6—C7	1.534 (9)	C28—O6	1.178 (7)
C6—H6	0.9900	C29—O7	1.144 (8)
C7—C8	1.530 (9)	C30—O8	1.148 (8)
C7—H7A	0.9800	C31—O9	1.143 (8)
C7—H7B	0.9800	C32—O10	1.130 (9)
C8—C9	1.514 (10)
C30—Fe1—C32	99.5 (4)	C4—C5—H5	124.0
C30—Fe1—C31	89.3 (4)	Fe3—C5—H5	124.6
C32—Fe1—C31	96.8 (4)	C5—N1—C6	119.6 (5)
C30—Fe1—C14	87.3 (3)	C5—N1—Fe4	116.1 (4)
C32—Fe1—C14	88.5 (3)	C6—N1—Fe4	123.1 (4)
C31—Fe1—C14	174.1 (3)	C5—N1—Fe3	73.3 (3)
C30—Fe1—N2	154.0 (3)	C6—N1—Fe3	131.9 (4)
C32—Fe1—N2	103.4 (3)	Fe4—N1—Fe3	74.96 (18)
C31—Fe1—N2	100.0 (3)	N1—C6—C11	115.5 (5)
C14—Fe1—N2	81.1 (3)	N1—C6—C7	108.7 (5)
C30—Fe1—Fe2	101.3 (3)	C11—C6—C7	110.8 (6)
C32—Fe1—Fe2	139.3 (3)	N1—C6—H6	107.2
C31—Fe1—Fe2	117.9 (3)	C11—C6—H6	107.2
C14—Fe1—Fe2	58.2 (2)	C7—C6—H6	107.2
N2—Fe1—Fe2	52.90 (15)	C8—C7—C6	111.3 (6)
C29—Fe2—C27	92.5 (3)	C8—C7—H7A	109.4
C29—Fe2—C28	85.9 (3)	C6—C7—H7A	109.4
C27—Fe2—C28	94.6 (3)	C8—C7—H7B	109.4
C29—Fe2—N2	100.7 (3)	C6—C7—H7B	109.4
C27—Fe2—N2	100.1 (2)	H7A—C7—H7B	108.0
C28—Fe2—N2	163.6 (3)	C9—C8—C7	111.3 (7)
C29—Fe2—C16	138.0 (3)	C9—C8—H8A	109.4
C27—Fe2—C16	90.5 (3)	C7—C8—H8A	109.4
C28—Fe2—C16	135.6 (3)	C9—C8—H8B	109.4
N2—Fe2—C16	37.8 (2)	C7—C8—H8B	109.4
C29—Fe2—C14	117.5 (3)	H8A—C8—H8B	108.0
C27—Fe2—C14	149.9 (3)	C8—C9—C10	111.5 (6)
C28—Fe2—C14	89.6 (3)	C8—C9—H9A	109.3
N2—Fe2—C14	74.0 (2)	C10—C9—H9A	109.3
C16—Fe2—C14	66.5 (2)	C8—C9—H9B	109.3
C29—Fe2—C15	151.7 (3)	C10—C9—H9B	109.3
C27—Fe2—C15	113.5 (3)	H9A—C9—H9B	108.0
C28—Fe2—C15	102.2 (3)	C9—C10—C11	110.4 (6)
N2—Fe2—C15	65.1 (2)	C9—C10—H10A	109.6
C16—Fe2—C15	37.4 (2)	C11—C10—H10A	109.6
C14—Fe2—C15	36.9 (2)	C9—C10—H10B	109.6
C29—Fe2—Fe1	79.2 (2)	C11—C10—H10B	109.6
C27—Fe2—Fe1	146.55 (19)	H10A—C10—H10B	108.1
C28—Fe2—Fe1	116.7 (2)	C6—C11—C10	110.1 (6)
N2—Fe2—Fe1	51.03 (15)	C6—C11—H11A	109.6
C16—Fe2—Fe1	75.60 (19)	C10—C11—H11A	109.6
C14—Fe2—Fe1	48.60 (17)	C6—C11—H11B	109.6
C15—Fe2—Fe1	72.88 (18)	C10—C11—H11B	109.6
C29—Fe2—Fe3	100.8 (2)	H11A—C11—H11B	108.2
C27—Fe2—Fe3	48.87 (19)	C1—S1—C4	89.7 (4)
C28—Fe2—Fe3	48.1 (2)	C13—C12—S2	112.8 (6)
N2—Fe2—Fe3	142.67 (16)	C13—C12—H12	123.6
C16—Fe2—Fe3	112.24 (19)	S2—C12—H12	123.6
C14—Fe2—Fe3	120.67 (17)	C12—C13—C14	115.3 (7)
C15—Fe2—Fe3	104.72 (18)	C12—C13—H13	122.4
Fe1—Fe2—Fe3	164.40 (5)	C14—C13—H13	122.4
C26—Fe3—C28	88.9 (3)	C15—C14—C13	108.8 (6)
C26—Fe3—C27	88.8 (3)	C15—C14—Fe1	112.9 (5)
C28—Fe3—C27	93.8 (3)	C13—C14—Fe1	136.8 (6)
C26—Fe3—N1	103.6 (3)	C15—C14—Fe2	72.5 (4)
C28—Fe3—N1	101.0 (2)	C13—C14—Fe2	132.0 (5)
C27—Fe3—N1	160.8 (2)	Fe1—C14—Fe2	73.2 (2)
C26—Fe3—C5	141.0 (3)	C16—C15—C14	115.7 (6)
C28—Fe3—C5	95.6 (3)	C16—C15—S2	131.1 (6)
C27—Fe3—C5	129.3 (3)	C14—C15—S2	113.2 (5)
N1—Fe3—C5	37.5 (2)	C16—C15—Fe2	66.9 (4)
C26—Fe3—C4	148.0 (3)	C14—C15—Fe2	70.6 (4)
C28—Fe3—C4	121.9 (3)	S2—C15—Fe2	133.8 (4)
C27—Fe3—C4	96.9 (3)	N2—C16—C15	114.1 (6)
N1—Fe3—C4	64.8 (2)	N2—C16—Fe2	68.1 (4)
C5—Fe3—C4	38.1 (2)	C15—C16—Fe2	75.7 (4)
C26—Fe3—C3	112.9 (3)	N2—C16—H16	123.0
C28—Fe3—C3	158.0 (3)	C15—C16—H16	123.0
C27—Fe3—C3	89.8 (3)	Fe2—C16—H16	124.7
N1—Fe3—C3	72.0 (2)	C16—N2—C17	114.3 (6)
C5—Fe3—C3	65.9 (2)	C16—N2—Fe1	114.9 (4)
C4—Fe3—C3	36.2 (2)	C17—N2—Fe1	129.7 (5)
C26—Fe3—Fe4	76.8 (2)	C16—N2—Fe2	74.1 (4)
C28—Fe3—Fe4	142.1 (2)	C17—N2—Fe2	128.2 (4)
C27—Fe3—Fe4	120.32 (19)	Fe1—N2—Fe2	76.08 (18)
N1—Fe3—Fe4	50.90 (14)	N2—C17—C18	114.3 (5)
C5—Fe3—Fe4	76.22 (18)	N2—C17—C22	108.0 (6)
C4—Fe3—Fe4	73.21 (18)	C18—C17—C22	110.9 (6)
C3—Fe3—Fe4	48.00 (18)	N2—C17—H17	107.8
C26—Fe3—Fe2	100.3 (3)	C18—C17—H17	107.8
C28—Fe3—Fe2	48.5 (2)	C22—C17—H17	107.8
C27—Fe3—Fe2	47.58 (19)	C17—C18—C19	110.1 (6)
N1—Fe3—Fe2	140.56 (15)	C17—C18—H18A	109.6
C5—Fe3—Fe2	111.58 (18)	C19—C18—H18A	109.6
C4—Fe3—Fe2	106.81 (18)	C17—C18—H18B	109.6
C3—Fe3—Fe2	125.43 (18)	C19—C18—H18B	109.6
Fe4—Fe3—Fe2	167.87 (5)	H18A—C18—H18B	108.2
C24—Fe4—C25	99.6 (4)	C20—C19—C18	108.5 (7)
C24—Fe4—C23	90.6 (3)	C20—C19—H19A	110.0
C25—Fe4—C23	98.2 (3)	C18—C19—H19A	110.0
C24—Fe4—C3	87.9 (3)	C20—C19—H19B	110.0
C25—Fe4—C3	92.4 (3)	C18—C19—H19B	110.0
C23—Fe4—C3	169.4 (3)	H19A—C19—H19B	108.4
C24—Fe4—N1	156.5 (3)	C21—C20—C19	113.2 (8)
C25—Fe4—N1	101.3 (3)	C21—C20—H20A	108.9
C23—Fe4—N1	96.9 (3)	C19—C20—H20A	108.9
C3—Fe4—N1	80.7 (2)	C21—C20—H20B	108.9
C24—Fe4—Fe3	102.4 (2)	C19—C20—H20B	108.9
C25—Fe4—Fe3	143.1 (3)	H20A—C20—H20B	107.8
C23—Fe4—Fe3	110.8 (2)	C20—C21—C22	111.0 (8)
C3—Fe4—Fe3	59.5 (2)	C20—C21—H21A	109.4
N1—Fe4—Fe3	54.14 (15)	C22—C21—H21A	109.4
C12—S2—C15	90.0 (4)	C20—C21—H21B	109.4
C2—C1—S1	114.1 (6)	C22—C21—H21B	109.4
C2—C1—H1	122.9	H21A—C21—H21B	108.0
S1—C1—H1	122.9	C17—C22—C21	110.1 (7)
C1—C2—C3	112.8 (7)	C17—C22—H22A	109.6
C1—C2—H2	123.6	C21—C22—H22A	109.6
C3—C2—H2	123.6	C17—C22—H22B	109.6
C4—C3—C2	110.3 (7)	C21—C22—H22B	109.6
C4—C3—Fe4	114.5 (5)	H22A—C22—H22B	108.2
C2—C3—Fe4	134.6 (6)	O1—C23—Fe4	173.6 (7)
C4—C3—Fe3	70.6 (4)	O2—C24—Fe4	175.3 (7)
C2—C3—Fe3	131.3 (5)	O3—C25—Fe4	177.7 (7)
Fe4—C3—Fe3	72.5 (2)	O4—C26—Fe3	176.4 (8)
C3—C4—C5	116.4 (6)	O5—C27—Fe2	139.7 (5)
C3—C4—S1	112.9 (5)	O5—C27—Fe3	136.7 (5)
C5—C4—S1	130.6 (6)	Fe2—C27—Fe3	83.6 (3)
C3—C4—Fe3	73.2 (4)	O6—C28—Fe3	138.6 (6)
C5—C4—Fe3	68.1 (4)	O6—C28—Fe2	137.8 (5)
S1—C4—Fe3	130.6 (3)	Fe3—C28—Fe2	83.5 (3)
N1—C5—C4	112.0 (6)	O7—C29—Fe2	175.3 (7)
N1—C5—Fe3	69.2 (3)	O8—C30—Fe1	176.8 (7)
C4—C5—Fe3	73.8 (4)	O9—C31—Fe1	170.5 (7)
N1—C5—H5	124.0	O10—C32—Fe1	177.2 (8)