Synthesis and crystal structure of deca­carbon­yl(μ₃-3,7-di­thia­nonane-1,9-di­thiol­ato)bis­(μ₂-propane-1,3-di­thiol­ato)nickel(II)tetra­iron(II) di­chloro­methane disolvate

Synthesis and structural studies of a Ni^IIS₄–2{2Fe2S}model for the H-cluster of [FeFe]-hydrogenase.

Key indicators

• Single-crystal X-ray study
• T = 243 K
• Mean [sigma](C-C) = 0.006 Å
• Disorder in solvent or counterion
• R factor = 0.032
• wR factor = 0.075
• Data-to-parameter ratio = 14.8

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00638 Ang.
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.595         26 Report
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Info

Alert level G
PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...          3 Report
PLAT005_ALERT_5_G No Embedded Refinement Details Found  in the CIF     Please Do !
PLAT154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note)      0.004 Degree
PLAT180_ALERT_4_G Check Cell Rounding: # of Values Ending with 0 =          3 Note
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Fe1      --C2        .        6.0 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Fe2      --C3        .        5.5 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Fe3      --C7        .        5.5 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Fe4      --C8        .        6.5 s.u.
PLAT300_ALERT_4_G Atom Site Occupancy of Cl1        Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of Cl1A       Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C24        Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C24A       Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H24A       Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H24B       Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H24C       Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H24D       Constrained at        0.5 Check
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  2  )        67% Note
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  3  )        33% Note
PLAT431_ALERT_2_G Short Inter HL..A Contact Cl4      ..O10       .       3.12 Ang.
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        121 Do !
            S7  -NI1 -S5  -C23   121.30  0.40   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        124 Do !
            S7  -NI1 -S5  -FE2     6.40  0.40   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        136 Do !
            S8  -NI1 -S6  -C17   123.60  0.40   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        139 Do !
            S8  -NI1 -S6  -FE3     8.90  0.40   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        152 Do !
            S5  -NI1 -S7  -C18    68.00  0.40   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        155 Do !
            S5  -NI1 -S7  -C19   -39.20  0.50   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        157 Do !
            S6  -NI1 -S8  -C22    97.60  0.40   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        160 Do !
            S6  -NI1 -S8  -C21  -156.70  0.40   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        163 Do !
            C4  -FE1 -C1  -O1     15.00  7.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        164 Do !
            C2  -FE1 -C1  -O1    -78.00  7.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        165 Do !
            S2  -FE1 -C1  -O1    103.00  7.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        166 Do !
            S1  -FE1 -C1  -O1   -168.00  7.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        167 Do !
            FE2 -FE1 -C1  -O1    139.00  7.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        168 Do !
            C4  -FE1 -C2  -O2     -3.00 13.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        169 Do !
            C1  -FE1 -C2  -O2     97.00 13.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        170 Do !
            S2  -FE1 -C2  -O2    -85.00 13.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        171 Do !
            S1  -FE1 -C2  -O2   -154.00 13.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        172 Do !
            FE2 -FE1 -C2  -O2    -99.00 13.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        173 Do !
            C5  -FE2 -C3  -O3     71.00  4.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        174 Do !
            S2  -FE2 -C3  -O3    -87.00  4.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        175 Do !
            S1  -FE2 -C3  -O3    -12.00  4.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        176 Do !
            S5  -FE2 -C3  -O3     18.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        177 Do !
            FE1 -FE2 -C3  -O3    -32.00  4.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        178 Do !
            C2  -FE1 -C4  -O4    -90.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        179 Do !
            C1  -FE1 -C4  -O4    172.00  8.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        180 Do !
            S2  -FE1 -C4  -O4     70.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        181 Do !
            S1  -FE1 -C4  -O4     -2.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        182 Do !
            FE2 -FE1 -C4  -O4     14.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        183 Do !
            C3  -FE2 -C5  -O5    -88.00  5.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        184 Do !
            S2  -FE2 -C5  -O5      1.00  6.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        185 Do !
            S1  -FE2 -C5  -O5     70.00  5.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        186 Do !
            S5  -FE2 -C5  -O5    169.00  5.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        187 Do !
            FE1 -FE2 -C5  -O5     16.00  5.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        188 Do !
            C7  -FE3 -C6  -O6    -60.00  4.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        189 Do !
            S4  -FE3 -C6  -O6    102.00  4.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        190 Do !
            S3  -FE3 -C6  -O6     23.00  4.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        191 Do !
            S6  -FE3 -C6  -O6   -157.00  4.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        192 Do !
            FE4 -FE3 -C6  -O6     46.00  4.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        193 Do !
            C6  -FE3 -C7  -O7     34.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        194 Do !
            S4  -FE3 -C7  -O7    -49.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        195 Do !
            S3  -FE3 -C7  -O7   -119.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        196 Do !
            S6  -FE3 -C7  -O7    140.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        197 Do !
            FE4 -FE3 -C7  -O7    -65.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        198 Do !
            C10 -FE4 -C8  -O8     18.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        199 Do !
            C9  -FE4 -C8  -O8     75.00  8.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        200 Do !
            S3  -FE4 -C8  -O8    -27.00  8.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        201 Do !
            S4  -FE4 -C8  -O8    -94.00  8.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        202 Do !
            FE3 -FE4 -C8  -O8    -82.00  8.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        203 Do !
            C10 -FE4 -C9  -O9   -122.00 17.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        204 Do !
            C8  -FE4 -C9  -O9    -27.00 17.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        205 Do !
            S3  -FE4 -C9  -O9     61.00 17.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        206 Do !
            S4  -FE4 -C9  -O9    149.00 17.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        207 Do !
            FE3 -FE4 -C9  -O9    105.00 17.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        208 Do !
            C8  -FE4 -C10 -O10    96.00 10.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        209 Do !
            C9  -FE4 -C10 -O10  -165.00 10.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        210 Do !
            S3  -FE4 -C10 -O10     8.00 10.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        211 Do !
            S4  -FE4 -C10 -O10   -63.00 10.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        212 Do !
            FE3 -FE4 -C10 -O10    -8.00 10.00   1.555   1.555   1.555   1.555
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        191 Check
              C24A -CL2  -C24     1.555   1.555   1.555             29.90 Deg.
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        192 Check
              CL3  -C25  -CL3A    1.555   1.555   1.555             17.10 Deg.
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          3 Note
              C H2 Cl2
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............         12 Note
PLAT899_ALERT_4_G SHELXL97   is Deprecated and Succeeded by SHELXL       2017 Note
PLAT909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still        66% Note
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          2 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   3 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  84 ALERT level G = General information/check it is not something unexpected

   1 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
   5 ALERT type 3 Indicator that the structure quality may be low
  73 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

---

Computing details

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008) and Mercury (Macrae et al., 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and publCIF (Westrip, 2010).

Decacarbonyl(µ₃-3,7-dithianonane-1,9-dithiolato)bis(µ₂-propane-1,3-dithiolato)nickel(II)tetrairon(II) dichloromethane disolvate

Crystal data

[Fe4Ni(C3H6S2)2(C7H14S4)(CO)10]·2CH2Cl2	Z = 2
Mr = 1170.88	F(000) = 1176
Triclinic, P1	Dx = 1.858 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 12.4340 (8) Å	Cell parameters from 6326 reflections
b = 13.9981 (10) Å	θ = 1.9–25.0°
c = 14.4912 (9) Å	µ = 2.50 mm^−1
α = 77.860 (4)°	T = 243 K
β = 67.570 (4)°	Block, red
γ = 64.036 (4)°	0.40 × 0.30 × 0.20 mm
V = 2093.3 (2) Å^3

Data collection

Bruker APEXII area detector diffractometer	7352 independent reflections
Radiation source: fine-focus sealed tube	5928 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.034
phi and ω scans	θmax = 25.0°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Bruker, 2007)	h = −14→14
Tmin = 0.435, Tmax = 0.635	k = −16→16
20488 measured reflections	l = −17→17

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)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.075	H-atom parameters constrained
S = 1.01	w = 1/[σ^2(Fo^2) + (0.0322P)^2 + 1.0504P] where P = (Fo^2 + 2Fc^2)/3
7352 reflections	(Δ/σ)max = 0.002
497 parameters	Δρmax = 0.94 e Å^−3
12 restraints	Δρmin = −0.59 e Å^−3

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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	Occ. (<1)
Fe1	0.63313 (4)	0.79098 (4)	0.59106 (3)	0.02955 (12)
Fe2	0.71720 (4)	0.66176 (3)	0.45877 (3)	0.02572 (11)
Fe3	0.81044 (4)	0.79149 (3)	0.02362 (3)	0.02590 (11)
Fe4	0.88790 (4)	0.91380 (4)	−0.11165 (4)	0.03041 (12)
Ni1	0.75218 (3)	0.60567 (3)	0.21998 (3)	0.02502 (10)
S1	0.84093 (8)	0.68240 (7)	0.52818 (7)	0.0376 (2)
S2	0.64699 (8)	0.84026 (7)	0.42929 (7)	0.0373 (2)
S3	0.90803 (7)	0.88819 (7)	0.04133 (7)	0.0320 (2)
S4	0.67953 (7)	0.94975 (7)	−0.02773 (6)	0.03083 (19)
S5	0.85931 (7)	0.62317 (6)	0.29938 (6)	0.02740 (18)
S6	0.68591 (7)	0.77643 (6)	0.18533 (6)	0.02789 (18)
S7	0.62939 (8)	0.59262 (7)	0.15145 (6)	0.0325 (2)
S8	0.83260 (8)	0.43272 (6)	0.24203 (6)	0.03208 (19)
O1	0.6078 (2)	0.9814 (2)	0.6672 (2)	0.0544 (7)
O2	0.6228 (3)	0.6580 (3)	0.7763 (2)	0.0759 (10)
O3	0.4837 (2)	0.6692 (2)	0.4504 (2)	0.0603 (8)
O4	0.3661 (2)	0.8440 (2)	0.6263 (2)	0.0582 (8)
O5	0.7473 (3)	0.4637 (2)	0.5800 (2)	0.0745 (10)
O6	0.7703 (3)	0.6795 (2)	−0.0997 (2)	0.0656 (8)
O7	1.0350 (2)	0.5987 (2)	0.0248 (2)	0.0556 (7)
O8	1.1618 (2)	0.7912 (2)	−0.1818 (2)	0.0583 (8)
O9	0.8921 (3)	1.1258 (2)	−0.1749 (2)	0.0697 (9)
O10	0.8462 (3)	0.8648 (2)	−0.2789 (2)	0.0589 (8)
C1	0.6208 (3)	0.9071 (3)	0.6366 (3)	0.0370 (8)
C2	0.6287 (4)	0.7096 (3)	0.7035 (3)	0.0453 (9)
C3	0.5787 (3)	0.6654 (3)	0.4492 (3)	0.0376 (8)
C4	0.4700 (3)	0.8252 (3)	0.6137 (3)	0.0396 (9)
C5	0.7381 (3)	0.5402 (3)	0.5288 (3)	0.0418 (9)
C6	0.7805 (3)	0.7242 (3)	−0.0477 (3)	0.0387 (8)
C7	0.9462 (3)	0.6750 (3)	0.0261 (3)	0.0359 (8)
C8	1.0549 (3)	0.8382 (3)	−0.1562 (3)	0.0383 (8)
C9	0.8892 (3)	1.0439 (3)	−0.1504 (3)	0.0422 (9)
C10	0.8630 (3)	0.8853 (3)	−0.2144 (3)	0.0408 (9)
C11	0.9377 (4)	0.7519 (4)	0.4431 (3)	0.0619 (13)
H11A	0.9970	0.7488	0.4729	0.074*
H11B	0.9867	0.7140	0.3819	0.074*
C12	0.8670 (4)	0.8653 (4)	0.4168 (3)	0.0689 (15)
H12A	0.9276	0.8961	0.3757	0.083*
H12B	0.8182	0.9036	0.4777	0.083*
C13	0.7789 (4)	0.8813 (3)	0.3618 (3)	0.0578 (12)
H13A	0.8285	0.8426	0.3011	0.069*
H13B	0.7442	0.9562	0.3419	0.069*
C14	0.6123 (3)	1.0571 (3)	0.0566 (3)	0.0460 (9)
H14A	0.6164	1.1208	0.0158	0.055*
H14B	0.5233	1.0706	0.0901	0.055*
C15	0.6679 (4)	1.0435 (3)	0.1332 (3)	0.0607 (11)
H15A	0.6275	1.1110	0.1645	0.073*
H15B	0.6428	0.9928	0.1839	0.073*
C16	0.8032 (3)	1.0094 (3)	0.1091 (3)	0.0498 (10)
H16A	0.8201	0.9999	0.1712	0.060*
H16B	0.8265	1.0669	0.0700	0.060*
C17	0.5253 (3)	0.8050 (3)	0.1922 (3)	0.0358 (8)
H17A	0.4742	0.8006	0.2616	0.043*
H17B	0.4885	0.8772	0.1659	0.043*
C18	0.5215 (3)	0.7290 (3)	0.1343 (3)	0.0389 (9)
H18A	0.5443	0.7507	0.0637	0.047*
H18B	0.4359	0.7323	0.1563	0.047*
C19	0.5269 (3)	0.5391 (3)	0.2543 (3)	0.0384 (8)
H19A	0.4915	0.5806	0.3124	0.046*
H19B	0.4574	0.5444	0.2356	0.046*
C20	0.6004 (3)	0.4242 (3)	0.2799 (3)	0.0406 (9)
H20A	0.6433	0.3859	0.2190	0.049*
H20B	0.5402	0.3944	0.3244	0.049*
C21	0.6982 (3)	0.4026 (3)	0.3286 (3)	0.0373 (8)
H21A	0.7284	0.3284	0.3518	0.045*
H21B	0.6586	0.4456	0.3862	0.045*
C22	0.9260 (3)	0.4059 (3)	0.3229 (3)	0.0390 (9)
H22A	0.8729	0.4082	0.3925	0.047*
H22B	0.9939	0.3356	0.3121	0.047*
C23	0.9805 (3)	0.4890 (3)	0.2984 (3)	0.0380 (9)
H23A	1.0450	0.4776	0.2329	0.046*
H23B	1.0204	0.4815	0.3469	0.046*
C24	0.2347 (12)	0.6444 (8)	1.0636 (13)	0.084 (5)	0.50
H24A	0.2297	0.5877	1.0390	0.101*	0.50
H24B	0.1599	0.7081	1.0624	0.101*	0.50
Cl1	0.3634 (8)	0.6661 (6)	0.9840 (8)	0.099 (2)	0.50
C24A	0.2888 (15)	0.5782 (14)	1.0674 (11)	0.111 (5)	0.50
H24C	0.2191	0.6039	1.0415	0.133*	0.50
H24D	0.3270	0.5013	1.0658	0.133*	0.50
Cl1A	0.4044 (7)	0.6293 (7)	0.9861 (7)	0.106 (2)	0.50
Cl2	0.23047 (12)	0.61093 (11)	1.18636 (13)	0.0906 (4)
C25	0.7905 (4)	1.1147 (4)	−0.4497 (3)	0.0579 (11)
H25A	0.7078	1.1437	−0.4576	0.069*
H25B	0.8105	1.0404	−0.4274	0.069*
Cl3	0.7839 (13)	1.1824 (16)	−0.3584 (7)	0.077 (2)	0.77 (6)
Cl3A	0.7681 (19)	1.215 (3)	−0.382 (4)	0.070 (7)	0.23 (6)
Cl4	0.90311 (11)	1.12301 (10)	−0.56564 (9)	0.0686 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.0318 (2)	0.0291 (3)	0.0275 (3)	−0.0109 (2)	−0.0094 (2)	−0.0046 (2)
Fe2	0.0280 (2)	0.0249 (2)	0.0249 (3)	−0.01072 (19)	−0.00932 (19)	−0.00100 (19)
Fe3	0.0287 (2)	0.0246 (2)	0.0253 (3)	−0.01209 (19)	−0.00882 (19)	0.00017 (19)
Fe4	0.0321 (2)	0.0322 (3)	0.0283 (3)	−0.0166 (2)	−0.0092 (2)	0.0031 (2)
Ni1	0.0291 (2)	0.0233 (2)	0.0248 (2)	−0.01258 (17)	−0.00913 (17)	0.00011 (17)
S1	0.0312 (4)	0.0456 (5)	0.0374 (5)	−0.0104 (4)	−0.0159 (4)	−0.0070 (4)
S2	0.0453 (5)	0.0255 (5)	0.0313 (5)	−0.0049 (4)	−0.0147 (4)	0.0011 (4)
S3	0.0328 (4)	0.0336 (5)	0.0357 (5)	−0.0150 (4)	−0.0157 (4)	−0.0015 (4)
S4	0.0295 (4)	0.0324 (5)	0.0315 (5)	−0.0116 (3)	−0.0138 (4)	0.0020 (4)
S5	0.0296 (4)	0.0275 (4)	0.0267 (4)	−0.0118 (3)	−0.0101 (3)	−0.0017 (3)
S6	0.0342 (4)	0.0249 (4)	0.0256 (4)	−0.0141 (3)	−0.0098 (3)	0.0021 (3)
S7	0.0377 (4)	0.0347 (5)	0.0326 (5)	−0.0199 (4)	−0.0139 (4)	0.0008 (4)
S8	0.0383 (4)	0.0248 (4)	0.0320 (5)	−0.0123 (4)	−0.0096 (4)	−0.0033 (4)
O1	0.0494 (15)	0.0471 (17)	0.072 (2)	−0.0168 (13)	−0.0161 (14)	−0.0250 (15)
O2	0.101 (2)	0.079 (2)	0.046 (2)	−0.038 (2)	−0.0312 (19)	0.0208 (17)
O3	0.0382 (14)	0.097 (2)	0.0568 (19)	−0.0337 (15)	−0.0072 (13)	−0.0268 (17)
O4	0.0315 (14)	0.0600 (19)	0.079 (2)	−0.0138 (13)	−0.0101 (13)	−0.0212 (16)
O5	0.108 (2)	0.0373 (17)	0.0499 (19)	−0.0269 (17)	−0.0060 (18)	0.0124 (14)
O6	0.092 (2)	0.075 (2)	0.0529 (19)	−0.0474 (18)	−0.0224 (17)	−0.0175 (16)
O7	0.0447 (15)	0.0417 (17)	0.0584 (19)	−0.0022 (13)	−0.0121 (14)	−0.0021 (14)
O8	0.0347 (15)	0.0520 (17)	0.083 (2)	−0.0141 (13)	−0.0042 (14)	−0.0303 (16)
O9	0.105 (2)	0.0460 (19)	0.072 (2)	−0.0437 (18)	−0.0391 (19)	0.0189 (16)
O10	0.0622 (17)	0.080 (2)	0.0408 (17)	−0.0291 (16)	−0.0211 (14)	−0.0068 (15)
C1	0.0333 (18)	0.041 (2)	0.036 (2)	−0.0129 (16)	−0.0103 (16)	−0.0072 (17)
C2	0.050 (2)	0.050 (2)	0.036 (2)	−0.0194 (19)	−0.0140 (19)	−0.005 (2)
C3	0.0376 (19)	0.046 (2)	0.030 (2)	−0.0165 (17)	−0.0061 (16)	−0.0129 (17)
C4	0.041 (2)	0.034 (2)	0.042 (2)	−0.0118 (16)	−0.0118 (17)	−0.0096 (17)
C5	0.050 (2)	0.032 (2)	0.033 (2)	−0.0151 (17)	−0.0038 (17)	−0.0047 (17)
C6	0.048 (2)	0.038 (2)	0.034 (2)	−0.0223 (17)	−0.0109 (17)	−0.0021 (17)
C7	0.0370 (19)	0.037 (2)	0.030 (2)	−0.0158 (17)	−0.0059 (16)	−0.0019 (16)
C8	0.044 (2)	0.041 (2)	0.039 (2)	−0.0256 (18)	−0.0107 (17)	−0.0049 (17)
C9	0.050 (2)	0.043 (2)	0.036 (2)	−0.0220 (19)	−0.0148 (18)	0.0044 (18)
C10	0.0358 (19)	0.050 (2)	0.034 (2)	−0.0178 (17)	−0.0104 (17)	0.0029 (18)
C11	0.047 (2)	0.087 (4)	0.065 (3)	−0.041 (2)	−0.005 (2)	−0.022 (3)
C12	0.073 (3)	0.077 (3)	0.064 (3)	−0.060 (3)	0.020 (2)	−0.031 (3)
C13	0.082 (3)	0.032 (2)	0.045 (3)	−0.031 (2)	0.003 (2)	0.0018 (18)
C14	0.0418 (18)	0.0329 (19)	0.056 (2)	−0.0040 (15)	−0.0186 (17)	−0.0082 (17)
C15	0.058 (2)	0.053 (2)	0.067 (2)	−0.0070 (18)	−0.0216 (19)	−0.0259 (19)
C16	0.055 (2)	0.045 (2)	0.057 (2)	−0.0145 (17)	−0.0242 (19)	−0.0190 (19)
C17	0.0304 (17)	0.036 (2)	0.036 (2)	−0.0127 (15)	−0.0085 (15)	0.0046 (16)
C18	0.0354 (18)	0.044 (2)	0.043 (2)	−0.0199 (16)	−0.0191 (17)	0.0078 (17)
C19	0.0392 (19)	0.042 (2)	0.041 (2)	−0.0240 (17)	−0.0126 (17)	0.0006 (17)
C20	0.046 (2)	0.035 (2)	0.045 (2)	−0.0268 (17)	−0.0076 (18)	−0.0004 (17)
C21	0.047 (2)	0.0281 (19)	0.034 (2)	−0.0196 (16)	−0.0077 (17)	0.0048 (15)
C22	0.0445 (19)	0.0256 (19)	0.041 (2)	−0.0052 (16)	−0.0180 (17)	−0.0022 (16)
C23	0.0303 (17)	0.035 (2)	0.044 (2)	−0.0039 (15)	−0.0128 (16)	−0.0100 (17)
C24	0.079 (8)	0.035 (6)	0.177 (14)	−0.002 (5)	−0.098 (9)	−0.021 (7)
Cl1	0.130 (5)	0.091 (4)	0.092 (3)	−0.040 (3)	−0.057 (3)	−0.006 (3)
C24A	0.139 (14)	0.157 (15)	0.095 (10)	−0.107 (12)	−0.033 (10)	−0.025 (12)
Cl1A	0.114 (5)	0.147 (7)	0.088 (3)	−0.087 (5)	−0.039 (3)	0.021 (4)
Cl2	0.0710 (8)	0.0752 (9)	0.1187 (13)	−0.0267 (7)	−0.0299 (8)	0.0007 (8)
C25	0.050 (2)	0.060 (3)	0.061 (3)	−0.026 (2)	−0.012 (2)	−0.002 (2)
Cl3	0.052 (3)	0.130 (5)	0.061 (2)	−0.049 (3)	−0.0078 (15)	−0.021 (3)
Cl3A	0.041 (4)	0.086 (12)	0.090 (14)	−0.015 (6)	−0.021 (6)	−0.038 (8)
Cl4	0.0661 (7)	0.0681 (8)	0.0531 (7)	−0.0241 (6)	−0.0090 (6)	0.0070 (6)

Geometric parameters (Å, º)

Fe1—C4	1.778 (4)	C11—H11A	0.9700
Fe1—C2	1.779 (4)	C11—H11B	0.9700
Fe1—C1	1.805 (4)	C12—C13	1.504 (6)
Fe1—S2	2.2620 (10)	C12—H12A	0.9700
Fe1—S1	2.2724 (9)	C12—H12B	0.9700
Fe1—Fe2	2.5126 (6)	C13—H13A	0.9700
Fe2—C5	1.755 (4)	C13—H13B	0.9700
Fe2—C3	1.759 (3)	C14—C15	1.460 (5)
Fe2—S2	2.2613 (10)	C14—H14A	0.9700
Fe2—S1	2.2703 (9)	C14—H14B	0.9700
Fe2—S5	2.3073 (9)	C15—C16	1.449 (5)
Fe3—C6	1.761 (4)	C15—H15A	0.9700
Fe3—C7	1.767 (4)	C15—H15B	0.9700
Fe3—S4	2.2769 (9)	C16—H16A	0.9700
Fe3—S3	2.2787 (9)	C16—H16B	0.9700
Fe3—S6	2.2897 (9)	C17—C18	1.513 (5)
Fe3—Fe4	2.5086 (7)	C17—H17A	0.9700
Fe4—C10	1.783 (4)	C17—H17B	0.9700
Fe4—C8	1.786 (4)	C18—H18A	0.9700
Fe4—C9	1.794 (4)	C18—H18B	0.9700
Fe4—S3	2.2619 (10)	C19—C20	1.510 (5)
Fe4—S4	2.2708 (9)	C19—H19A	0.9700
Ni1—S6	2.1750 (9)	C19—H19B	0.9700
Ni1—S5	2.1754 (9)	C20—C21	1.520 (5)
Ni1—S8	2.1822 (9)	C20—H20A	0.9700
Ni1—S7	2.1974 (9)	C20—H20B	0.9700
S1—C11	1.817 (4)	C21—H21A	0.9700
S2—C13	1.828 (4)	C21—H21B	0.9700
S3—C16	1.825 (3)	C22—C23	1.507 (5)
S4—C14	1.828 (4)	C22—H22A	0.9700
S5—C23	1.820 (3)	C22—H22B	0.9700
S6—C17	1.823 (3)	C23—H23A	0.9700
S7—C18	1.822 (3)	C23—H23B	0.9700
S7—C19	1.823 (3)	C24—Cl1	1.689 (19)
S8—C22	1.826 (4)	C24—Cl2	1.728 (16)
S8—C21	1.827 (3)	C24—H24A	0.9700
O1—C1	1.139 (4)	C24—H24B	0.9700
O2—C2	1.142 (5)	C24A—Cl2	1.671 (14)
O3—C3	1.152 (4)	C24A—Cl1A	1.794 (17)
O4—C4	1.147 (4)	C24A—H24C	0.9700
O5—C5	1.155 (4)	C24A—H24D	0.9700
O6—C6	1.148 (4)	C25—Cl3	1.741 (9)
O7—C7	1.149 (4)	C25—Cl3A	1.75 (2)
O8—C8	1.139 (4)	C25—Cl4	1.750 (4)
O9—C9	1.139 (4)	C25—H25A	0.9700
O10—C10	1.147 (4)	C25—H25B	0.9700
C11—C12	1.489 (6)
C4—Fe1—C2	91.51 (17)	C12—C11—H11A	108.4
C4—Fe1—C1	99.37 (15)	S1—C11—H11A	108.4
C2—Fe1—C1	97.89 (17)	C12—C11—H11B	108.4
C4—Fe1—S2	85.96 (13)	S1—C11—H11B	108.4
C2—Fe1—S2	159.36 (12)	H11A—C11—H11B	107.4
C1—Fe1—S2	102.74 (12)	C11—C12—C13	114.2 (3)
C4—Fe1—S1	151.33 (11)	C11—C12—H12A	108.7
C2—Fe1—S1	87.50 (12)	C13—C12—H12A	108.7
C1—Fe1—S1	109.15 (11)	C11—C12—H12B	108.7
S2—Fe1—S1	85.04 (4)	C13—C12—H12B	108.7
C4—Fe1—Fe2	96.33 (11)	H12A—C12—H12B	107.6
C2—Fe1—Fe2	103.85 (12)	C12—C13—S2	116.7 (3)
C1—Fe1—Fe2	152.74 (12)	C12—C13—H13A	108.1
S2—Fe1—Fe2	56.24 (3)	S2—C13—H13A	108.1
S1—Fe1—Fe2	56.38 (3)	C12—C13—H13B	108.1
C5—Fe2—C3	90.13 (18)	S2—C13—H13B	108.1
C5—Fe2—S2	157.67 (12)	H13A—C13—H13B	107.3
C3—Fe2—S2	89.49 (12)	C15—C14—S4	118.8 (3)
C5—Fe2—S1	86.92 (13)	C15—C14—H14A	107.6
C3—Fe2—S1	157.92 (11)	S4—C14—H14A	107.6
S2—Fe2—S1	85.10 (4)	C15—C14—H14B	107.6
C5—Fe2—S5	106.91 (11)	S4—C14—H14B	107.6
C3—Fe2—S5	102.64 (11)	H14A—C14—H14B	107.0
S2—Fe2—S5	94.94 (3)	C16—C15—C14	121.5 (4)
S1—Fe2—S5	99.15 (3)	C16—C15—H15A	107.0
C5—Fe2—Fe1	102.21 (12)	C14—C15—H15A	107.0
C3—Fe2—Fe1	103.06 (10)	C16—C15—H15B	107.0
S2—Fe2—Fe1	56.27 (3)	C14—C15—H15B	107.0
S1—Fe2—Fe1	56.46 (3)	H15A—C15—H15B	106.7
S5—Fe2—Fe1	140.73 (3)	C15—C16—S3	118.0 (3)
C6—Fe3—C7	87.86 (16)	C15—C16—H16A	107.8
C6—Fe3—S4	89.82 (12)	S3—C16—H16A	107.8
C7—Fe3—S4	161.61 (12)	C15—C16—H16B	107.8
C6—Fe3—S3	152.86 (12)	S3—C16—H16B	107.8
C7—Fe3—S3	88.74 (11)	H16A—C16—H16B	107.1
S4—Fe3—S3	85.04 (3)	C18—C17—S6	112.5 (2)
C6—Fe3—S6	106.05 (12)	C18—C17—H17A	109.1
C7—Fe3—S6	97.86 (11)	S6—C17—H17A	109.1
S4—Fe3—S6	100.31 (3)	C18—C17—H17B	109.1
S3—Fe3—S6	101.09 (3)	S6—C17—H17B	109.1
C6—Fe3—Fe4	99.19 (12)	H17A—C17—H17B	107.8
C7—Fe3—Fe4	106.02 (11)	C17—C18—S7	111.7 (2)
S4—Fe3—Fe4	56.41 (3)	C17—C18—H18A	109.3
S3—Fe3—Fe4	56.14 (3)	S7—C18—H18A	109.3
S6—Fe3—Fe4	145.71 (3)	C17—C18—H18B	109.3
C10—Fe4—C8	93.52 (16)	S7—C18—H18B	109.3
C10—Fe4—C9	100.99 (17)	H18A—C18—H18B	107.9
C8—Fe4—C9	98.17 (16)	C20—C19—S7	110.6 (2)
C10—Fe4—S3	156.81 (13)	C20—C19—H19A	109.5
C8—Fe4—S3	86.09 (12)	S7—C19—H19A	109.5
C9—Fe4—S3	102.02 (12)	C20—C19—H19B	109.5
C10—Fe4—S4	86.56 (11)	S7—C19—H19B	109.5
C8—Fe4—S4	158.66 (12)	H19A—C19—H19B	108.1
C9—Fe4—S4	102.77 (12)	C19—C20—C21	116.8 (3)
S3—Fe4—S4	85.57 (3)	C19—C20—H20A	108.1
C10—Fe4—Fe3	100.97 (12)	C21—C20—H20A	108.1
C8—Fe4—Fe3	102.60 (12)	C19—C20—H20B	108.1
C9—Fe4—Fe3	148.60 (12)	C21—C20—H20B	108.1
S3—Fe4—Fe3	56.78 (3)	H20A—C20—H20B	107.3
S4—Fe4—Fe3	56.64 (3)	C20—C21—S8	111.9 (2)
S6—Ni1—S5	88.17 (3)	C20—C21—H21A	109.2
S6—Ni1—S8	174.85 (4)	S8—C21—H21A	109.2
S5—Ni1—S8	92.01 (3)	C20—C21—H21B	109.2
S6—Ni1—S7	91.05 (3)	S8—C21—H21B	109.2
S5—Ni1—S7	175.01 (4)	H21A—C21—H21B	107.9
S8—Ni1—S7	89.22 (3)	C23—C22—S8	108.5 (2)
C11—S1—Fe2	112.33 (15)	C23—C22—H22A	110.0
C11—S1—Fe1	113.21 (15)	S8—C22—H22A	110.0
Fe2—S1—Fe1	67.16 (3)	C23—C22—H22B	110.0
C13—S2—Fe2	111.11 (14)	S8—C22—H22B	110.0
C13—S2—Fe1	112.09 (15)	H22A—C22—H22B	108.4
Fe2—S2—Fe1	67.49 (3)	C22—C23—S5	111.9 (2)
C16—S3—Fe4	108.98 (14)	C22—C23—H23A	109.2
C16—S3—Fe3	115.56 (13)	S5—C23—H23A	109.2
Fe4—S3—Fe3	67.07 (3)	C22—C23—H23B	109.2
C14—S4—Fe4	110.26 (13)	S5—C23—H23B	109.2
C14—S4—Fe3	114.30 (13)	H23A—C23—H23B	107.9
Fe4—S4—Fe3	66.96 (3)	Cl1—C24—Cl2	116.0 (6)
C23—S5—Ni1	101.59 (11)	Cl1—C24—H24A	108.3
C23—S5—Fe2	110.57 (13)	Cl2—C24—H24A	108.3
Ni1—S5—Fe2	103.94 (3)	Cl1—C24—H24B	108.3
C17—S6—Ni1	99.83 (11)	Cl2—C24—H24B	108.3
C17—S6—Fe3	111.08 (12)	H24A—C24—H24B	107.4
Ni1—S6—Fe3	103.81 (3)	Cl2—C24A—Cl1A	115.0 (8)
C18—S7—C19	102.54 (16)	Cl2—C24A—H24C	108.5
C18—S7—Ni1	105.10 (11)	Cl1A—C24A—H24C	108.5
C19—S7—Ni1	103.26 (12)	Cl2—C24A—H24D	108.5
C22—S8—C21	101.18 (17)	Cl1A—C24A—H24D	108.5
C22—S8—Ni1	104.79 (11)	H24C—C24A—H24D	107.5
C21—S8—Ni1	103.69 (11)	C24A—Cl2—C24	29.9 (6)
O1—C1—Fe1	177.2 (3)	Cl3—C25—Cl3A	17.1 (14)
O2—C2—Fe1	178.3 (4)	Cl3—C25—Cl4	113.1 (3)
O3—C3—Fe2	174.9 (3)	Cl3A—C25—Cl4	105.2 (17)
O4—C4—Fe1	177.4 (3)	Cl3—C25—H25A	109.0
O5—C5—Fe2	175.9 (3)	Cl3A—C25—H25A	98.9
O6—C6—Fe3	174.5 (3)	Cl4—C25—H25A	109.0
O7—C7—Fe3	177.9 (3)	Cl3—C25—H25B	109.0
O8—C8—Fe4	177.5 (3)	Cl3A—C25—H25B	126.0
O9—C9—Fe4	178.7 (4)	Cl4—C25—H25B	109.0
O10—C10—Fe4	178.1 (4)	H25A—C25—H25B	107.8
C12—C11—S1	115.6 (3)
C4—Fe1—Fe2—C5	−92.64 (18)	S6—Ni1—S5—Fe2	87.40 (4)
C2—Fe1—Fe2—C5	0.50 (18)	S8—Ni1—S5—Fe2	−97.75 (4)
C1—Fe1—Fe2—C5	142.4 (3)	S7—Ni1—S5—Fe2	6.4 (4)
S2—Fe1—Fe2—C5	−173.46 (13)	C5—Fe2—S5—C23	−16.11 (18)
S1—Fe1—Fe2—C5	77.91 (13)	C3—Fe2—S5—C23	−110.16 (17)
C4—Fe1—Fe2—C3	0.38 (18)	S2—Fe2—S5—C23	159.25 (12)
C2—Fe1—Fe2—C3	93.52 (18)	S1—Fe2—S5—C23	73.44 (12)
C1—Fe1—Fe2—C3	−124.6 (3)	Fe1—Fe2—S5—C23	120.04 (12)
S2—Fe1—Fe2—C3	−80.44 (13)	C5—Fe2—S5—Ni1	92.21 (14)
S1—Fe1—Fe2—C3	170.93 (13)	C3—Fe2—S5—Ni1	−1.84 (13)
C4—Fe1—Fe2—S2	80.83 (13)	S2—Fe2—S5—Ni1	−92.43 (4)
C2—Fe1—Fe2—S2	173.96 (13)	S1—Fe2—S5—Ni1	−178.24 (4)
C1—Fe1—Fe2—S2	−44.1 (2)	Fe1—Fe2—S5—Ni1	−131.64 (4)
S1—Fe1—Fe2—S2	−108.63 (4)	S5—Ni1—S6—C17	−144.38 (12)
C4—Fe1—Fe2—S1	−170.55 (13)	S8—Ni1—S6—C17	123.6 (4)
C2—Fe1—Fe2—S1	−77.41 (13)	S7—Ni1—S6—C17	30.69 (12)
C1—Fe1—Fe2—S1	64.5 (2)	S5—Ni1—S6—Fe3	100.88 (4)
S2—Fe1—Fe2—S1	108.63 (4)	S8—Ni1—S6—Fe3	8.9 (4)
C4—Fe1—Fe2—S5	130.07 (13)	S7—Ni1—S6—Fe3	−84.05 (4)
C2—Fe1—Fe2—S5	−136.80 (13)	C6—Fe3—S6—C17	−45.78 (17)
C1—Fe1—Fe2—S5	5.1 (2)	C7—Fe3—S6—C17	−135.81 (16)
S2—Fe1—Fe2—S5	49.24 (5)	S4—Fe3—S6—C17	47.03 (12)
S1—Fe1—Fe2—S5	−59.39 (5)	S3—Fe3—S6—C17	133.94 (12)
C6—Fe3—Fe4—C10	5.20 (16)	Fe4—Fe3—S6—C17	90.02 (13)
C7—Fe3—Fe4—C10	95.60 (16)	C6—Fe3—S6—Ni1	60.67 (13)
S4—Fe3—Fe4—C10	−78.42 (12)	C7—Fe3—S6—Ni1	−29.36 (12)
S3—Fe3—Fe4—C10	172.88 (12)	S4—Fe3—S6—Ni1	153.48 (3)
S6—Fe3—Fe4—C10	−132.06 (12)	S3—Fe3—S6—Ni1	−119.61 (4)
C6—Fe3—Fe4—C8	−90.97 (16)	Fe4—Fe3—S6—Ni1	−163.53 (4)
C7—Fe3—Fe4—C8	−0.57 (16)	S6—Ni1—S7—C18	−12.91 (13)
S4—Fe3—Fe4—C8	−174.59 (11)	S5—Ni1—S7—C18	68.0 (4)
S3—Fe3—Fe4—C8	76.71 (11)	S8—Ni1—S7—C18	172.23 (13)
S6—Fe3—Fe4—C8	131.77 (12)	S6—Ni1—S7—C19	−120.04 (12)
C6—Fe3—Fe4—C9	138.8 (3)	S5—Ni1—S7—C19	−39.2 (5)
C7—Fe3—Fe4—C9	−130.8 (3)	S8—Ni1—S7—C19	65.10 (12)
S4—Fe3—Fe4—C9	55.2 (2)	S6—Ni1—S8—C22	97.6 (4)
S3—Fe3—Fe4—C9	−53.5 (2)	S5—Ni1—S8—C22	5.75 (13)
S6—Fe3—Fe4—C9	1.6 (2)	S7—Ni1—S8—C22	−169.41 (13)
C6—Fe3—Fe4—S3	−167.68 (12)	S6—Ni1—S8—C21	−156.7 (4)
C7—Fe3—Fe4—S3	−77.28 (12)	S5—Ni1—S8—C21	111.45 (12)
S4—Fe3—Fe4—S3	108.70 (4)	S7—Ni1—S8—C21	−63.71 (12)
S6—Fe3—Fe4—S3	55.06 (6)	C4—Fe1—C1—O1	15 (7)
C6—Fe3—Fe4—S4	83.62 (12)	C2—Fe1—C1—O1	−78 (7)
C7—Fe3—Fe4—S4	174.02 (12)	S2—Fe1—C1—O1	103 (7)
S3—Fe3—Fe4—S4	−108.70 (4)	S1—Fe1—C1—O1	−168 (7)
S6—Fe3—Fe4—S4	−53.64 (6)	Fe2—Fe1—C1—O1	139 (7)
C5—Fe2—S1—C11	146.3 (2)	C4—Fe1—C2—O2	−3 (13)
C3—Fe2—S1—C11	−130.9 (4)	C1—Fe1—C2—O2	97 (13)
S2—Fe2—S1—C11	−54.54 (16)	S2—Fe1—C2—O2	−85 (13)
S5—Fe2—S1—C11	39.69 (16)	S1—Fe1—C2—O2	−154 (13)
Fe1—Fe2—S1—C11	−106.82 (16)	Fe2—Fe1—C2—O2	−99 (13)
C5—Fe2—S1—Fe1	−106.85 (11)	C5—Fe2—C3—O3	71 (4)
C3—Fe2—S1—Fe1	−24.1 (3)	S2—Fe2—C3—O3	−87 (4)
S2—Fe2—S1—Fe1	52.28 (3)	S1—Fe2—C3—O3	−12 (4)
S5—Fe2—S1—Fe1	146.51 (3)	S5—Fe2—C3—O3	178 (100)
C4—Fe1—S1—C11	125.4 (3)	Fe1—Fe2—C3—O3	−32 (4)
C2—Fe1—S1—C11	−146.0 (2)	C2—Fe1—C4—O4	−90 (9)
C1—Fe1—S1—C11	−48.5 (2)	C1—Fe1—C4—O4	172 (8)
S2—Fe1—S1—C11	53.28 (16)	S2—Fe1—C4—O4	70 (9)
Fe2—Fe1—S1—C11	105.54 (16)	S1—Fe1—C4—O4	−2 (9)
C4—Fe1—S1—Fe2	19.9 (3)	Fe2—Fe1—C4—O4	14 (9)
C2—Fe1—S1—Fe2	108.47 (12)	C3—Fe2—C5—O5	−88 (5)
C1—Fe1—S1—Fe2	−154.04 (13)	S2—Fe2—C5—O5	1 (6)
S2—Fe1—S1—Fe2	−52.26 (3)	S1—Fe2—C5—O5	70 (5)
C5—Fe2—S2—C13	123.1 (4)	S5—Fe2—C5—O5	169 (5)
C3—Fe2—S2—C13	−147.83 (19)	Fe1—Fe2—C5—O5	16 (5)
S1—Fe2—S2—C13	53.60 (16)	C7—Fe3—C6—O6	−60 (4)
S5—Fe2—S2—C13	−45.19 (16)	S4—Fe3—C6—O6	102 (4)
Fe1—Fe2—S2—C13	106.04 (16)	S3—Fe3—C6—O6	23 (4)
C5—Fe2—S2—Fe1	17.0 (3)	S6—Fe3—C6—O6	−157 (4)
C3—Fe2—S2—Fe1	106.13 (11)	Fe4—Fe3—C6—O6	46 (4)
S1—Fe2—S2—Fe1	−52.44 (3)	C6—Fe3—C7—O7	34 (9)
S5—Fe2—S2—Fe1	−151.23 (3)	S4—Fe3—C7—O7	−49 (9)
C4—Fe1—S2—C13	155.00 (18)	S3—Fe3—C7—O7	−119 (9)
C2—Fe1—S2—C13	−121.5 (4)	S6—Fe3—C7—O7	140 (9)
C1—Fe1—S2—C13	56.29 (17)	Fe4—Fe3—C7—O7	−65 (9)
S1—Fe1—S2—C13	−52.24 (14)	C10—Fe4—C8—O8	176 (100)
Fe2—Fe1—S2—C13	−104.63 (14)	C9—Fe4—C8—O8	75 (8)
C4—Fe1—S2—Fe2	−100.38 (11)	S3—Fe4—C8—O8	−27 (8)
C2—Fe1—S2—Fe2	−16.8 (4)	S4—Fe4—C8—O8	−94 (8)
C1—Fe1—S2—Fe2	160.92 (11)	Fe3—Fe4—C8—O8	−82 (8)
S1—Fe1—S2—Fe2	52.38 (3)	C10—Fe4—C9—O9	−122 (17)
C10—Fe4—S3—C16	−128.5 (3)	C8—Fe4—C9—O9	−27 (17)
C8—Fe4—S3—C16	141.69 (18)	S3—Fe4—C9—O9	61 (17)
C9—Fe4—S3—C16	44.16 (18)	S4—Fe4—C9—O9	149 (17)
S4—Fe4—S3—C16	−57.98 (14)	Fe3—Fe4—C9—O9	105 (17)
Fe3—Fe4—S3—C16	−110.49 (14)	C8—Fe4—C10—O10	96 (10)
C10—Fe4—S3—Fe3	−18.0 (3)	C9—Fe4—C10—O10	−165 (10)
C8—Fe4—S3—Fe3	−107.82 (11)	S3—Fe4—C10—O10	8 (10)
C9—Fe4—S3—Fe3	154.65 (12)	S4—Fe4—C10—O10	−63 (10)
S4—Fe4—S3—Fe3	52.51 (3)	Fe3—Fe4—C10—O10	−8 (10)
C6—Fe3—S3—C16	128.4 (3)	Fe2—S1—C11—C12	66.6 (3)
C7—Fe3—S3—C16	−148.79 (19)	Fe1—S1—C11—C12	−7.1 (4)
S4—Fe3—S3—C16	48.53 (16)	S1—C11—C12—C13	−63.0 (4)
S6—Fe3—S3—C16	−51.03 (16)	C11—C12—C13—S2	63.8 (4)
Fe4—Fe3—S3—C16	100.90 (16)	Fe2—S2—C13—C12	−66.6 (3)
C6—Fe3—S3—Fe4	27.5 (3)	Fe1—S2—C13—C12	6.8 (3)
C7—Fe3—S3—Fe4	110.31 (11)	Fe4—S4—C14—C15	−58.3 (4)
S4—Fe3—S3—Fe4	−52.37 (3)	Fe3—S4—C14—C15	14.7 (4)
S6—Fe3—S3—Fe4	−151.92 (3)	S4—C14—C15—C16	49.9 (6)
C10—Fe4—S4—C14	−145.83 (19)	C14—C15—C16—S3	−53.0 (6)
C8—Fe4—S4—C14	123.3 (3)	Fe4—S3—C16—C15	64.1 (4)
C9—Fe4—S4—C14	−45.33 (18)	Fe3—S3—C16—C15	−8.9 (4)
S3—Fe4—S4—C14	56.01 (14)	Ni1—S6—C17—C18	−48.1 (3)
Fe3—Fe4—S4—C14	108.64 (14)	Fe3—S6—C17—C18	60.9 (3)
C10—Fe4—S4—Fe3	105.53 (12)	S6—C17—C18—S7	41.3 (3)
C8—Fe4—S4—Fe3	14.6 (3)	C19—S7—C18—C17	94.0 (3)
C9—Fe4—S4—Fe3	−153.97 (12)	Ni1—S7—C18—C17	−13.7 (3)
S3—Fe4—S4—Fe3	−52.63 (3)	C18—S7—C19—C20	179.8 (2)
C6—Fe3—S4—C14	156.07 (18)	Ni1—S7—C19—C20	−71.2 (2)
C7—Fe3—S4—C14	−121.3 (4)	S7—C19—C20—C21	69.7 (4)
S3—Fe3—S4—C14	−50.61 (14)	C19—C20—C21—S8	−68.6 (4)
S6—Fe3—S4—C14	49.78 (15)	C22—S8—C21—C20	177.2 (2)
Fe4—Fe3—S4—C14	−102.76 (14)	Ni1—S8—C21—C20	68.8 (2)
C6—Fe3—S4—Fe4	−101.17 (12)	C21—S8—C22—C23	−140.8 (2)
C7—Fe3—S4—Fe4	−18.5 (4)	Ni1—S8—C22—C23	−33.2 (2)
S3—Fe3—S4—Fe4	52.14 (3)	S8—C22—C23—S5	51.1 (3)
S6—Fe3—S4—Fe4	152.54 (3)	Ni1—S5—C23—C22	−43.7 (3)
S6—Ni1—S5—C23	−157.74 (13)	Fe2—S5—C23—C22	66.2 (3)
S8—Ni1—S5—C23	17.11 (13)	Cl1A—C24A—Cl2—C24	77.7 (16)
S7—Ni1—S5—C23	121.3 (4)	Cl1—C24—Cl2—C24A	−74.2 (14)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C19—H19A···O3	0.97	2.52	3.440 (5)	159
C15—H15B···S6	0.97	2.83	3.578 (4)	134
C13—H13B···O4^i	0.97	2.57	3.470 (5)	154
C20—H20A···O8^ii	0.97	2.57	3.263 (5)	128
C24—H24A···O7^iii	0.97	2.44	3.08 (2)	123
C24A—H24C···O7^iii	0.97	2.42	3.32 (2)	154

Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x+2, −y+1, −z; (iii) x−1, y, z+1.