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Acta Crystallogr Sect E Struct Rep Online. 2008 December 1; 64(Pt 12): m1504.
Published online 2008 November 8. doi:  10.1107/S1600536808035253
PMCID: PMC2959963

Di-μ-chlorido-bis­{bis­[3,5-dimethyl­pyrazol-1-yl-κN 2)methane]iron(II)} bis­[tetra­chloridoferrate(III)]

Abstract

In the title complex, [Fe2Cl2(C11H16N4)4][FeCl4]2, the asymmetric unit is composed of one and a half units of [Fe(bdmpm)2Cl]2(FeCl4)2(bdmpm = bis(bis(3,5-dimethyl­pyrazol-1-yl)methane). The three independent FeII atom have a distorted octa­hedral coordination geometry comprising two bridging chloride anions and four N atoms from two bis­(3,5-dimethyl­pyrazol-1-yl)methane ligands. The FeIII atom has a tetra­hedral coordination geometry comprising four chloride anions.

Related literature

For information on the coordination chemistry of poly-(pyrazol­yl)methane ligands, see: Anderson et al. (2000 [triangle]); Edwards et al. (2006 [triangle]); Higgs et al. (1999 [triangle]); Moubaraki et al. (2003 [triangle]); Pettinari & Pettinari (2005 [triangle]); Reger et al. (2004 [triangle]). For information on binuclear complexes, see: Moubaraki et al. (2003 [triangle]); Batten et al. (2004 [triangle]); Gu et al. (2006 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-m1504-scheme1.jpg

Experimental

Crystal data

  • [Fe2Cl2(C11H16N4)4][FeCl4]2
  • M r = 1395.01
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-m1504-efi1.jpg
  • a = 14.100 (3) Å
  • b = 18.244 (4) Å
  • c = 19.969 (4) Å
  • α = 85.58 (3)°
  • β = 71.23 (3)°
  • γ = 68.20 (3)°
  • V = 4511 (2) Å3
  • Z = 3
  • Mo Kα radiation
  • μ = 1.44 mm−1
  • T = 293 (2) K
  • 0.18 × 0.15 × 0.12 mm

Data collection

  • Rigaku Mercury diffractometer
  • Absorption correction: multi-scan (Jacobson, 1998 [triangle]) T min = 0.782, T max = 0.847
  • 44634 measured reflections
  • 16405 independent reflections
  • 10865 reflections with I > 2σ(I)
  • R int = 0.096

Refinement

  • R[F 2 > 2σ(F 2)] = 0.093
  • wR(F 2) = 0.209
  • S = 1.08
  • 16405 reflections
  • 1022 parameters
  • H-atom parameters constrained
  • Δρmax = 0.76 e Å−3
  • Δρmin = −0.95 e Å−3

Data collection: CrystalClear (Rigaku/MSC, 2001 [triangle]); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku/MSC, 2004 [triangle]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808035253/br2084sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808035253/br2084Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

The authors acknowledge Jiangxi Science and Technology Normal University for funding.

supplementary crystallographic information

Comment

The various unsubstituted and methyl-substituted poly-(pyrazolyl)methane ligands have become very important in coordination chemistry (Pettinari, et al., 2005; Reger, et al., 2004; Higgs, et al., 1999; Anderson, et al., 2000; Edwards, et al., 2006). But most of them are coordinated with iron to form single nuclear coordination complexes, only few examples are binuclear coordination complexes (Gu, et al., 2006; Batten, et al., 2004; Moubaraki, et al., 2003). In the crystal of the title complex, the asymmetric unit is composed of one and a half units of [Fe(bdmpm)2Cl]2 2FeCl4 (bdmpm = bis(bis(3,5-dimethylpyrazol-1-yl)methane). One of [Fe(bdmpm)2Cl]2 complexes has a crystallographic center of symmetry, the other has an approximate center of symmetry but it is not crystallographic. The reason for this difference is that the bond length and bond angles around Fe(2) and Fe(3) are slightly different. Each binuclear cations with a pair of bridging chloride ligands and the two bmmpm ligands results in six-coordination about each of the metal atoms; the environments of the complex are octahedron geometry (Fig. 1).

Experimental

The reaction of FeCl2.4H2O (20 mg, 0.1 mmol) with bdmpm (44 mg, 0.22 mmol) in EtOH (15 ml) was carried out at ambient temperature for 20 minutes, the mixture was filtered and the filtrate was then left for crystallization.

Refinement

In this structrue, the C-H distance was constrained to 0.93 Å for C-H, 0.96 Å for C-H3 and 0.97 for C-H2. The ratio of the Uiso values 1.2 for H atoms of C-H and C-H2, 1.5 for H atoms of C-H3.

Figures

Fig. 1.
The molecular structure with displacement ellipsoids drawn at the 50% probability level. Atoms labeled with the suffix A are related by the (1 - x, 1 - y, 1 - z) symmetry operator.

Crystal data

[Fe2Cl2(C11H16N4)4][FeCl4]2Z = 3
Mr = 1395.01F000 = 2142
Triclinic, P1Dx = 1.541 Mg m3
Hall symbol: -P 1Mo Kα radiation λ = 0.71073 Å
a = 14.100 (3) ÅCell parameters from 12389 reflections
b = 18.244 (4) Åθ = 3.1–25.4º
c = 19.969 (4) ŵ = 1.44 mm1
α = 85.58 (3)ºT = 293 (2) K
β = 71.23 (3)ºPrism, yellow
γ = 68.20 (3)º0.18 × 0.15 × 0.12 mm
V = 4511 (2) Å3

Data collection

Rigaku Mercury diffractometer16405 independent reflections
Radiation source: fine-focus sealed tube10865 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.096
T = 293(2) Kθmax = 25.4º
ω scansθmin = 3.1º
Absorption correction: multi-scan(Jacobson, 1998)h = −14→16
Tmin = 0.782, Tmax = 0.847k = −21→21
44634 measured reflectionsl = −22→24

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.093H-atom parameters constrained
wR(F2) = 0.209  w = 1/[σ2(Fo2) + (0.0667P)2 + 17.766P] where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.001
16405 reflectionsΔρmax = 0.76 e Å3
1022 parametersΔρmin = −0.95 e Å3
Primary atom site location: structure-invariant direct methodsExtinction correction: none

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 (Å2)

xyzUiso*/Ueq
Fe10.62332 (8)0.51099 (6)0.50914 (5)0.0247 (2)
Fe20.74539 (9)0.16729 (6)0.16291 (5)0.0257 (3)
Fe30.99665 (9)0.17009 (6)0.18208 (5)0.0282 (3)
Fe40.63770 (10)0.63582 (7)0.06660 (6)0.0422 (3)
Fe50.99828 (10)0.69688 (7)0.26964 (6)0.0370 (3)
Fe61.32478 (10)−0.03970 (7)0.40487 (6)0.0354 (3)
Cl10.57354 (17)0.41434 (12)0.46044 (11)0.0410 (5)
Cl20.80653 (18)0.25535 (13)0.21295 (12)0.0477 (5)
Cl30.93390 (19)0.08437 (14)0.13036 (12)0.0514 (6)
Cl40.7281 (2)0.52573 (14)0.10930 (12)0.0573 (6)
Cl50.7239 (2)0.64291 (16)−0.04497 (12)0.0610 (7)
Cl60.6167 (2)0.73748 (16)0.12761 (16)0.0754 (8)
Cl70.4792 (2)0.63502 (19)0.07611 (13)0.0707 (8)
Cl81.0250 (2)0.80953 (13)0.24793 (12)0.0587 (7)
Cl90.8800 (2)0.70590 (15)0.37419 (12)0.0602 (7)
Cl101.1519 (2)0.60330 (17)0.26359 (17)0.0781 (8)
Cl110.9354 (3)0.67382 (17)0.19135 (15)0.0774 (9)
Cl121.31887 (19)−0.15580 (13)0.44282 (12)0.0499 (6)
Cl131.18150 (19)0.05457 (13)0.46825 (13)0.0533 (6)
Cl141.3308 (2)−0.03182 (17)0.29382 (12)0.0652 (7)
Cl151.46816 (19)−0.03050 (15)0.41644 (14)0.0567 (6)
N10.7937 (5)0.4304 (3)0.4892 (3)0.0261 (14)
N20.8140 (5)0.3594 (3)0.5215 (3)0.0293 (14)
N30.6535 (5)0.3821 (3)0.6202 (3)0.0312 (15)
N40.5976 (5)0.4607 (3)0.6133 (3)0.0275 (14)
N50.6583 (5)0.6072 (3)0.5454 (3)0.0268 (14)
N60.6305 (5)0.6792 (3)0.5136 (3)0.0276 (14)
N70.6583 (5)0.5625 (3)0.4070 (3)0.0260 (13)
N80.6266 (5)0.6434 (3)0.4021 (3)0.0284 (14)
N90.5806 (5)0.2555 (3)0.1851 (3)0.0302 (15)
N100.5666 (5)0.3242 (3)0.1493 (3)0.0300 (14)
N110.7731 (5)0.2163 (3)0.0589 (3)0.0285 (14)
N120.7309 (5)0.2976 (3)0.0525 (3)0.0289 (14)
N130.6936 (5)0.0789 (4)0.1283 (3)0.0326 (15)
N140.7025 (5)0.0118 (4)0.1674 (3)0.0352 (16)
N150.7092 (5)0.1155 (3)0.2663 (3)0.0262 (14)
N160.7415 (5)0.0349 (3)0.2707 (3)0.0314 (15)
N171.0463 (5)0.2590 (4)0.2160 (3)0.0335 (15)
N181.0214 (5)0.3315 (3)0.1877 (3)0.0354 (16)
N191.0364 (5)0.2189 (3)0.0794 (3)0.0331 (15)
N201.0169 (6)0.2978 (4)0.0749 (3)0.0395 (17)
N211.1602 (5)0.0799 (3)0.1588 (3)0.0306 (14)
N221.1697 (5)0.0043 (3)0.1781 (3)0.0304 (14)
N230.9701 (5)0.1183 (3)0.2847 (3)0.0286 (14)
N241.0253 (5)0.0387 (3)0.2891 (3)0.0310 (15)
C10.9188 (7)0.3241 (4)0.5144 (4)0.037 (2)
C20.9694 (7)0.3718 (5)0.4769 (4)0.041 (2)
H2A1.04260.36230.46360.049*
C30.8891 (6)0.4383 (4)0.4623 (4)0.0307 (17)
C40.9045 (6)0.5082 (5)0.4232 (4)0.0370 (19)
H4A0.93010.49580.37310.055*
H4B0.95620.52160.43610.055*
H4C0.83710.55220.43500.055*
C50.9646 (8)0.2436 (5)0.5413 (5)0.059 (3)
H5A0.93690.24600.59200.088*
H5B1.04170.22650.52650.088*
H5C0.94440.20680.52240.088*
C60.7271 (7)0.3339 (4)0.5571 (4)0.037 (2)
H6A0.75610.27960.56990.045*
H6B0.68760.33510.52490.045*
C70.6286 (7)0.3620 (4)0.6881 (4)0.039 (2)
C80.5552 (7)0.4292 (5)0.7274 (4)0.039 (2)
H8A0.52240.43360.77620.047*
C90.5391 (6)0.4899 (4)0.6802 (4)0.0303 (17)
C100.6762 (9)0.2811 (5)0.7122 (5)0.060 (3)
H10A0.66380.24380.68800.090*
H10B0.64320.28000.76230.090*
H10C0.75230.26730.70190.090*
C110.4729 (7)0.5744 (5)0.6969 (4)0.041 (2)
H11A0.51040.59920.71420.062*
H11B0.40570.57990.73260.062*
H11C0.45950.59920.65500.062*
C120.6665 (6)0.7291 (4)0.5355 (4)0.0317 (18)
C130.7196 (6)0.6896 (4)0.5815 (4)0.0314 (18)
H13A0.75320.70870.60530.038*
C140.7132 (6)0.6144 (4)0.5854 (4)0.0285 (17)
C150.6445 (8)0.8130 (4)0.5129 (5)0.048 (2)
H15A0.66930.81310.46210.072*
H15B0.68180.83640.53200.072*
H15C0.56860.84290.53020.072*
C160.7610 (7)0.5477 (5)0.6277 (4)0.0364 (19)
H16A0.71770.55760.67660.055*
H16B0.83280.54340.62310.055*
H16C0.76320.49920.61050.055*
C170.5678 (6)0.6935 (4)0.4663 (4)0.0299 (17)
H17A0.54790.74850.45400.036*
H17B0.50210.68390.49010.036*
C180.6542 (7)0.6650 (5)0.3351 (4)0.0335 (18)
C190.7084 (6)0.5961 (4)0.2934 (4)0.0325 (18)
H19A0.73780.59160.24430.039*
C200.7103 (6)0.5347 (4)0.3391 (4)0.0302 (17)
C210.6302 (8)0.7493 (5)0.3150 (5)0.051 (2)
H21A0.59050.78370.35670.077*
H21B0.58810.76090.28330.077*
H21C0.69640.75740.29180.077*
C220.7658 (7)0.4472 (4)0.3209 (4)0.038 (2)
H22A0.75330.41860.36320.057*
H22B0.84180.43470.29940.057*
H22C0.73770.43250.28830.057*
C230.4612 (7)0.3631 (5)0.1552 (4)0.040 (2)
C240.4075 (7)0.3191 (5)0.1935 (4)0.044 (2)
H24A0.33390.33040.20530.053*
C250.4811 (7)0.2538 (5)0.2124 (4)0.0358 (19)
C260.4232 (8)0.4413 (5)0.1214 (5)0.057 (3)
H26A0.34630.46020.13250.086*
H26B0.45630.43410.07100.086*
H26C0.44290.47900.13920.086*
C270.4616 (7)0.1858 (5)0.2536 (5)0.047 (2)
H27A0.43060.16120.23020.070*
H27B0.41310.20460.30040.070*
H27C0.52860.14790.25680.070*
C280.6579 (7)0.3472 (4)0.1162 (4)0.0356 (19)
H28A0.69660.34300.14950.043*
H28B0.63280.40200.10370.043*
C290.7608 (7)0.3186 (5)−0.0149 (4)0.0341 (18)
C300.8243 (7)0.2482 (5)−0.0549 (4)0.038 (2)
H30A0.85820.2428−0.10360.045*
C310.8275 (6)0.1868 (4)−0.0076 (4)0.0283 (17)
C320.7313 (8)0.4014 (5)−0.0373 (4)0.049 (2)
H32A0.65440.4259−0.02500.073*
H32B0.76310.4017−0.08770.073*
H32C0.75740.4301−0.01390.073*
C330.8799 (6)0.1007 (5)−0.0257 (4)0.0366 (19)
H33A0.89650.07340.01460.055*
H33B0.94500.0905−0.06470.055*
H33C0.83200.0826−0.03850.055*
C340.6352 (7)−0.0221 (5)0.1630 (5)0.044 (2)
C350.5815 (8)0.0232 (5)0.1197 (4)0.046 (2)
H35A0.52870.01480.10650.055*
C360.6196 (7)0.0847 (5)0.0986 (4)0.042 (2)
C370.6298 (9)−0.0956 (6)0.2013 (5)0.065 (3)
H37A0.6991−0.13750.18580.097*
H37B0.5775−0.11100.19120.097*
H37C0.6092−0.08520.25140.097*
C380.5838 (7)0.1494 (5)0.0528 (4)0.042 (2)
H38A0.51100.18320.07660.063*
H38B0.58740.12770.00940.063*
H38C0.62970.17940.04270.063*
C390.7792 (7)−0.0124 (4)0.2052 (4)0.037 (2)
H39A0.8461−0.00800.17520.045*
H39B0.7938−0.06740.21620.045*
C400.7230 (6)0.0123 (5)0.3382 (4)0.0361 (19)
C410.6764 (6)0.0800 (5)0.3797 (4)0.0340 (18)
H41A0.65460.08390.42890.041*
C420.6674 (6)0.1431 (4)0.3340 (4)0.0289 (17)
C430.7498 (7)−0.0714 (5)0.3587 (5)0.046 (2)
H43A0.7126−0.09560.34040.069*
H43B0.7280−0.07310.40940.069*
H43C0.8260−0.09960.33950.069*
C440.6167 (7)0.2287 (4)0.3534 (4)0.039 (2)
H44A0.64810.25700.31590.059*
H44B0.62830.23850.39610.059*
H44C0.54080.24610.36080.059*
C451.0586 (7)0.3788 (5)0.2121 (4)0.043 (2)
C461.1065 (8)0.3363 (6)0.2584 (5)0.055 (3)
H46A1.13840.35360.28480.065*
C471.1000 (7)0.2623 (5)0.2598 (4)0.038 (2)
C481.0394 (9)0.4629 (5)0.1916 (5)0.062 (3)
H48A1.07130.46390.14140.093*
H48B1.07120.48590.21580.093*
H48C0.96330.49250.20460.093*
C491.1465 (7)0.1917 (5)0.2990 (5)0.048 (2)
H49A1.10560.20030.34840.073*
H49B1.22000.18380.29310.073*
H49C1.14380.14570.28060.073*
C500.9607 (8)0.3492 (4)0.1381 (4)0.044 (2)
H50A0.89190.34370.16110.052*
H50B0.94670.40360.12500.052*
C511.0533 (7)0.3169 (5)0.0074 (4)0.0365 (19)
C521.0996 (7)0.2488 (5)−0.0330 (4)0.039 (2)
H52A1.13170.2436−0.08190.047*
C531.0903 (6)0.1880 (4)0.0121 (4)0.0314 (17)
C541.0374 (9)0.4006 (5)−0.0139 (5)0.055 (3)
H54A0.96180.4311−0.00290.082*
H54B1.07230.4007−0.06380.082*
H54C1.06800.42330.01150.082*
C551.1312 (7)0.1023 (4)−0.0065 (4)0.043 (2)
H55A1.10410.07540.03400.064*
H55B1.20850.0817−0.02120.064*
H55C1.10760.0943−0.04450.064*
C561.2710 (7)−0.0487 (4)0.1468 (4)0.0361 (19)
C571.3278 (6)−0.0050 (4)0.1076 (4)0.0355 (19)
H57A1.3997−0.02450.07950.043*
C581.2595 (6)0.0729 (5)0.1173 (4)0.0331 (18)
C591.3022 (7)−0.1345 (4)0.1588 (4)0.044 (2)
H59A1.2889−0.14260.20850.067*
H59B1.3774−0.16120.13400.067*
H59C1.2605−0.15530.14170.067*
C601.2860 (7)0.1434 (5)0.0887 (5)0.045 (2)
H60A1.22160.18990.10130.068*
H60B1.31640.13690.03810.068*
H60C1.33710.14870.10840.068*
C611.0760 (6)−0.0108 (4)0.2252 (4)0.0312 (18)
H61A1.0241−0.00180.20040.037*
H61B1.0983−0.06570.23740.037*
C621.0109 (6)0.0187 (5)0.3568 (4)0.0337 (18)
C630.9459 (7)0.0861 (5)0.3978 (4)0.0380 (19)
H63A0.92160.09040.44700.046*
C640.9228 (6)0.1473 (5)0.3524 (4)0.0314 (18)
C651.0595 (7)−0.0641 (5)0.3771 (5)0.047 (2)
H65A1.0305−0.09730.36160.071*
H65B1.0431−0.06520.42760.071*
H65C1.1362−0.08320.35510.071*
C660.8590 (7)0.2325 (5)0.3715 (4)0.042 (2)
H66A0.90270.25670.38220.062*
H66B0.79720.23810.41220.062*
H66C0.83590.25770.33250.062*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Fe10.0325 (6)0.0166 (5)0.0198 (5)−0.0057 (5)−0.0057 (4)0.0023 (4)
Fe20.0330 (6)0.0174 (5)0.0225 (5)−0.0082 (5)−0.0053 (5)0.0036 (4)
Fe30.0371 (7)0.0172 (5)0.0250 (6)−0.0074 (5)−0.0066 (5)0.0036 (4)
Fe40.0518 (8)0.0402 (7)0.0364 (7)−0.0215 (6)−0.0093 (6)−0.0052 (5)
Fe50.0518 (8)0.0269 (6)0.0343 (6)−0.0156 (6)−0.0157 (6)0.0054 (5)
Fe60.0405 (7)0.0314 (7)0.0330 (6)−0.0088 (5)−0.0145 (5)−0.0018 (5)
Cl10.0454 (12)0.0432 (12)0.0421 (11)−0.0224 (10)−0.0191 (10)0.0132 (9)
Cl20.0463 (13)0.0519 (14)0.0517 (13)−0.0225 (11)−0.0226 (11)0.0182 (10)
Cl30.0502 (14)0.0557 (15)0.0560 (14)−0.0252 (12)−0.0239 (11)0.0191 (11)
Cl40.0776 (18)0.0479 (14)0.0466 (13)−0.0239 (13)−0.0195 (12)0.0035 (10)
Cl50.0685 (17)0.0799 (19)0.0388 (13)−0.0368 (15)−0.0125 (12)0.0089 (12)
Cl60.083 (2)0.0571 (17)0.090 (2)−0.0209 (15)−0.0305 (16)−0.0304 (15)
Cl70.0692 (18)0.113 (2)0.0486 (14)−0.0567 (18)−0.0141 (13)−0.0005 (14)
Cl80.0803 (18)0.0387 (13)0.0496 (14)−0.0338 (13)0.0047 (12)−0.0043 (10)
Cl90.0774 (18)0.0578 (16)0.0436 (13)−0.0367 (14)−0.0048 (12)0.0104 (11)
Cl100.0682 (19)0.0559 (17)0.094 (2)0.0004 (14)−0.0334 (16)0.0099 (15)
Cl110.131 (3)0.0736 (19)0.0648 (17)−0.0565 (19)−0.0611 (18)0.0231 (14)
Cl120.0556 (14)0.0343 (12)0.0626 (14)−0.0162 (11)−0.0227 (12)0.0035 (10)
Cl130.0453 (13)0.0405 (13)0.0596 (14)−0.0010 (11)−0.0122 (11)−0.0106 (10)
Cl140.0726 (18)0.086 (2)0.0361 (12)−0.0237 (15)−0.0222 (12)0.0028 (12)
Cl150.0464 (14)0.0592 (16)0.0727 (17)−0.0207 (12)−0.0265 (12)−0.0040 (12)
N10.039 (4)0.012 (3)0.026 (3)−0.007 (3)−0.012 (3)0.004 (2)
N20.039 (4)0.013 (3)0.029 (3)−0.004 (3)−0.009 (3)0.001 (2)
N30.046 (4)0.015 (3)0.019 (3)−0.001 (3)−0.006 (3)0.003 (2)
N40.040 (4)0.020 (3)0.020 (3)−0.009 (3)−0.007 (3)0.001 (2)
N50.030 (3)0.016 (3)0.028 (3)−0.005 (3)−0.007 (3)0.004 (2)
N60.030 (4)0.017 (3)0.030 (3)−0.005 (3)−0.005 (3)0.001 (2)
N70.030 (3)0.016 (3)0.027 (3)−0.009 (3)−0.003 (3)0.005 (2)
N80.043 (4)0.021 (3)0.019 (3)−0.012 (3)−0.007 (3)0.005 (2)
N90.045 (4)0.023 (3)0.020 (3)−0.011 (3)−0.009 (3)0.001 (2)
N100.042 (4)0.019 (3)0.025 (3)−0.009 (3)−0.008 (3)0.002 (2)
N110.039 (4)0.017 (3)0.023 (3)−0.007 (3)−0.006 (3)0.006 (2)
N120.042 (4)0.020 (3)0.022 (3)−0.007 (3)−0.012 (3)0.003 (2)
N130.042 (4)0.025 (4)0.029 (3)−0.015 (3)−0.005 (3)0.001 (3)
N140.046 (4)0.019 (3)0.036 (4)−0.012 (3)−0.007 (3)0.002 (3)
N150.040 (4)0.014 (3)0.023 (3)−0.011 (3)−0.006 (3)0.001 (2)
N160.041 (4)0.024 (3)0.023 (3)−0.012 (3)−0.002 (3)0.006 (3)
N170.038 (4)0.024 (4)0.037 (4)−0.015 (3)−0.007 (3)0.005 (3)
N180.042 (4)0.018 (3)0.039 (4)−0.009 (3)−0.005 (3)−0.004 (3)
N190.050 (4)0.013 (3)0.029 (3)−0.009 (3)−0.006 (3)0.006 (2)
N200.056 (5)0.021 (3)0.031 (4)−0.013 (3)−0.002 (3)0.005 (3)
N210.034 (4)0.017 (3)0.039 (4)−0.006 (3)−0.013 (3)0.002 (3)
N220.038 (4)0.020 (3)0.026 (3)−0.006 (3)−0.006 (3)0.004 (3)
N230.036 (4)0.019 (3)0.028 (3)−0.005 (3)−0.012 (3)0.006 (2)
N240.044 (4)0.017 (3)0.027 (3)−0.009 (3)−0.008 (3)0.002 (2)
C10.039 (5)0.022 (4)0.042 (5)0.006 (4)−0.022 (4)−0.004 (3)
C20.036 (5)0.034 (5)0.049 (5)−0.006 (4)−0.014 (4)−0.005 (4)
C30.021 (4)0.021 (4)0.038 (4)−0.002 (3)−0.001 (3)0.000 (3)
C40.026 (4)0.040 (5)0.042 (5)−0.013 (4)−0.005 (4)0.003 (4)
C50.068 (7)0.031 (5)0.068 (6)0.007 (5)−0.040 (6)0.005 (4)
C60.059 (6)0.013 (4)0.026 (4)−0.006 (4)−0.003 (4)0.002 (3)
C70.059 (6)0.024 (4)0.029 (4)−0.013 (4)−0.011 (4)0.012 (3)
C80.054 (6)0.043 (5)0.024 (4)−0.025 (5)−0.010 (4)0.008 (4)
C90.026 (4)0.035 (5)0.024 (4)−0.011 (4)−0.002 (3)0.001 (3)
C100.106 (9)0.028 (5)0.036 (5)−0.014 (5)−0.027 (5)0.021 (4)
C110.042 (5)0.033 (5)0.031 (4)0.005 (4)−0.005 (4)−0.015 (4)
C120.040 (5)0.015 (4)0.031 (4)−0.009 (3)0.000 (4)−0.006 (3)
C130.028 (4)0.020 (4)0.039 (4)−0.006 (3)−0.003 (4)−0.008 (3)
C140.027 (4)0.024 (4)0.026 (4)0.000 (3)−0.008 (3)−0.001 (3)
C150.073 (7)0.020 (4)0.049 (5)−0.022 (4)−0.011 (5)0.006 (4)
C160.041 (5)0.035 (5)0.040 (5)−0.015 (4)−0.022 (4)0.003 (4)
C170.045 (5)0.019 (4)0.025 (4)−0.011 (4)−0.012 (4)0.004 (3)
C180.046 (5)0.032 (4)0.030 (4)−0.021 (4)−0.016 (4)0.012 (3)
C190.042 (5)0.033 (4)0.020 (4)−0.018 (4)0.000 (3)−0.004 (3)
C200.036 (4)0.024 (4)0.028 (4)−0.013 (4)−0.002 (3)−0.007 (3)
C210.078 (7)0.039 (5)0.040 (5)−0.027 (5)−0.021 (5)0.018 (4)
C220.050 (5)0.035 (5)0.026 (4)−0.020 (4)−0.001 (4)−0.007 (3)
C230.045 (5)0.030 (5)0.035 (5)0.005 (4)−0.021 (4)−0.005 (4)
C240.040 (5)0.047 (6)0.042 (5)−0.009 (5)−0.014 (4)−0.004 (4)
C250.035 (5)0.037 (5)0.032 (4)−0.009 (4)−0.009 (4)−0.007 (3)
C260.069 (7)0.039 (5)0.050 (6)0.007 (5)−0.029 (5)−0.008 (4)
C270.036 (5)0.052 (6)0.050 (5)−0.019 (4)−0.004 (4)−0.006 (4)
C280.059 (6)0.018 (4)0.024 (4)−0.009 (4)−0.013 (4)0.001 (3)
C290.048 (5)0.033 (5)0.027 (4)−0.020 (4)−0.016 (4)0.014 (3)
C300.049 (5)0.040 (5)0.023 (4)−0.021 (4)−0.005 (4)0.003 (3)
C310.028 (4)0.027 (4)0.026 (4)−0.008 (3)−0.006 (3)0.002 (3)
C320.075 (7)0.038 (5)0.037 (5)−0.025 (5)−0.020 (5)0.012 (4)
C330.035 (5)0.037 (5)0.025 (4)−0.004 (4)−0.002 (3)−0.007 (3)
C340.056 (6)0.024 (4)0.043 (5)−0.021 (4)0.007 (4)−0.011 (4)
C350.063 (6)0.051 (6)0.036 (5)−0.039 (5)−0.007 (4)−0.008 (4)
C360.047 (5)0.036 (5)0.040 (5)−0.008 (4)−0.014 (4)−0.009 (4)
C370.087 (8)0.046 (6)0.055 (6)−0.040 (6)0.008 (6)−0.003 (5)
C380.042 (5)0.045 (5)0.044 (5)−0.017 (4)−0.017 (4)−0.009 (4)
C390.050 (5)0.012 (4)0.028 (4)−0.004 (4)0.005 (4)0.004 (3)
C400.037 (5)0.038 (5)0.032 (4)−0.014 (4)−0.011 (4)0.014 (4)
C410.033 (4)0.049 (5)0.019 (4)−0.017 (4)−0.007 (3)0.010 (3)
C420.030 (4)0.023 (4)0.026 (4)−0.005 (3)−0.005 (3)0.000 (3)
C430.046 (5)0.037 (5)0.048 (5)−0.010 (4)−0.016 (4)0.020 (4)
C440.042 (5)0.031 (5)0.036 (4)−0.009 (4)−0.004 (4)−0.011 (3)
C450.057 (6)0.032 (5)0.033 (5)−0.024 (4)0.006 (4)−0.004 (4)
C460.053 (6)0.057 (6)0.051 (6)−0.032 (5)0.004 (5)−0.019 (5)
C470.034 (5)0.033 (5)0.043 (5)−0.014 (4)−0.004 (4)−0.003 (4)
C480.079 (8)0.030 (5)0.064 (7)−0.028 (5)0.003 (6)−0.003 (4)
C490.046 (6)0.061 (6)0.048 (5)−0.020 (5)−0.026 (4)0.010 (4)
C500.062 (6)0.016 (4)0.037 (5)−0.003 (4)−0.007 (4)0.002 (3)
C510.039 (5)0.032 (5)0.038 (5)−0.017 (4)−0.010 (4)0.013 (4)
C520.052 (5)0.037 (5)0.027 (4)−0.024 (4)−0.003 (4)0.006 (3)
C530.036 (5)0.033 (4)0.023 (4)−0.013 (4)−0.006 (3)0.001 (3)
C540.089 (8)0.040 (5)0.045 (5)−0.034 (5)−0.028 (5)0.024 (4)
C550.050 (5)0.026 (4)0.036 (5)−0.007 (4)−0.002 (4)−0.005 (3)
C560.053 (5)0.020 (4)0.030 (4)−0.002 (4)−0.020 (4)−0.001 (3)
C570.024 (4)0.030 (4)0.049 (5)−0.005 (4)−0.012 (4)−0.002 (4)
C580.023 (4)0.030 (4)0.043 (5)−0.008 (4)−0.010 (4)0.004 (3)
C590.059 (6)0.021 (4)0.041 (5)−0.001 (4)−0.016 (4)0.004 (3)
C600.037 (5)0.029 (5)0.057 (6)−0.012 (4)−0.001 (4)0.005 (4)
C610.042 (5)0.009 (3)0.033 (4)−0.011 (3)0.001 (4)0.002 (3)
C620.041 (5)0.033 (5)0.027 (4)−0.016 (4)−0.011 (4)0.015 (3)
C630.039 (5)0.045 (5)0.031 (4)−0.015 (4)−0.014 (4)0.003 (4)
C640.032 (4)0.041 (5)0.022 (4)−0.015 (4)−0.007 (3)0.002 (3)
C650.053 (6)0.043 (5)0.042 (5)−0.016 (5)−0.015 (4)0.015 (4)
C660.046 (5)0.042 (5)0.034 (4)−0.010 (4)−0.012 (4)−0.010 (4)

Geometric parameters (Å, °)

Fe1—N72.165 (6)C16—H16A0.9600
Fe1—N42.184 (6)C16—H16B0.9600
Fe1—N52.218 (6)C16—H16C0.9600
Fe1—N12.223 (6)C17—H17A0.9700
Fe1—Cl1i2.483 (3)C17—H17B0.9700
Fe1—Cl12.484 (2)C18—C191.378 (10)
Fe1—Fe1i3.777 (2)C18—C211.499 (10)
Fe2—N112.171 (6)C19—C201.386 (10)
Fe2—N152.191 (6)C19—H19A0.9300
Fe2—N92.204 (7)C20—C221.509 (10)
Fe2—N132.233 (6)C21—H21A0.9600
Fe2—Cl32.414 (3)C21—H21B0.9600
Fe2—Cl22.481 (3)C21—H21C0.9600
Fe2—Fe33.7028 (17)C22—H22A0.9600
Fe3—N192.158 (6)C22—H22B0.9600
Fe3—N232.170 (6)C22—H22C0.9600
Fe3—N212.202 (6)C23—C241.337 (12)
Fe3—N172.213 (6)C23—C261.514 (11)
Fe3—Cl22.444 (3)C24—C251.380 (11)
Fe3—Cl32.482 (3)C24—H24A0.9300
Fe4—Cl62.173 (3)C25—C271.498 (11)
Fe4—Cl72.187 (3)C26—H26A0.9600
Fe4—Cl52.188 (3)C26—H26B0.9600
Fe4—Cl42.218 (3)C26—H26C0.9600
Fe5—Cl112.163 (3)C27—H27A0.9600
Fe5—Cl102.177 (3)C27—H27B0.9600
Fe5—Cl92.186 (3)C27—H27C0.9600
Fe5—Cl82.210 (2)C28—H28A0.9700
Fe6—Cl152.174 (3)C28—H28B0.9700
Fe6—Cl132.180 (3)C29—C301.390 (11)
Fe6—Cl142.187 (3)C29—C321.485 (10)
Fe6—Cl122.216 (3)C30—C311.406 (10)
Cl1—Fe1i2.483 (3)C30—H30A0.9300
N1—C31.336 (9)C31—C331.482 (10)
N1—N21.376 (8)C32—H32A0.9600
N2—C11.339 (10)C32—H32B0.9600
N2—C61.427 (10)C32—H32C0.9600
N3—C71.344 (9)C33—H33A0.9600
N3—N41.377 (8)C33—H33B0.9600
N3—C61.446 (9)C33—H33C0.9600
N4—C91.349 (9)C34—C351.360 (13)
N5—C141.321 (9)C34—C371.507 (12)
N5—N61.389 (8)C35—C361.398 (12)
N6—C121.352 (9)C35—H35A0.9300
N6—C171.440 (9)C36—C381.473 (12)
N7—C201.350 (9)C37—H37A0.9600
N7—N81.380 (8)C37—H37B0.9600
N8—C181.339 (9)C37—H37C0.9600
N8—C171.448 (9)C38—H38A0.9600
N9—C251.343 (10)C38—H38B0.9600
N9—N101.374 (8)C38—H38C0.9600
N10—C231.358 (10)C39—H39A0.9700
N10—C281.444 (10)C39—H39B0.9700
N11—C311.338 (9)C40—C411.362 (11)
N11—N121.392 (8)C40—C431.489 (11)
N12—C291.346 (9)C41—C421.407 (10)
N12—C281.462 (9)C41—H41A0.9300
N13—C361.325 (10)C42—C441.478 (10)
N13—N141.388 (8)C43—H43A0.9600
N14—C341.338 (10)C43—H43B0.9600
N14—C391.432 (10)C43—H43C0.9600
N15—C421.340 (9)C44—H44A0.9600
N15—N161.373 (8)C44—H44B0.9600
N16—C401.350 (9)C44—H44C0.9600
N16—C391.457 (9)C45—C461.346 (13)
N17—C471.345 (10)C45—C481.503 (11)
N17—N181.364 (8)C46—C471.385 (12)
N18—C451.351 (10)C46—H46A0.9300
N18—C501.451 (11)C47—C491.500 (11)
N19—C531.358 (9)C48—H48A0.9600
N19—N201.363 (8)C48—H48B0.9600
N20—C511.348 (10)C48—H48C0.9600
N20—C501.445 (10)C49—H49A0.9600
N21—C581.342 (9)C49—H49B0.9600
N21—N221.373 (8)C49—H49C0.9600
N22—C561.364 (10)C50—H50A0.9700
N22—C611.461 (9)C50—H50B0.9700
N23—C641.348 (9)C51—C521.354 (11)
N23—N241.381 (8)C51—C541.506 (11)
N24—C621.342 (9)C52—C531.391 (10)
N24—C611.438 (9)C52—H52A0.9300
C1—C21.357 (12)C53—C551.483 (10)
C1—C51.503 (11)C54—H54A0.9600
C2—C31.406 (11)C54—H54B0.9600
C2—H2A0.9300C54—H54C0.9600
C3—C41.493 (10)C55—H55A0.9600
C4—H4A0.9600C55—H55B0.9600
C4—H4B0.9600C55—H55C0.9600
C4—H4C0.9600C56—C571.364 (11)
C5—H5A0.9600C56—C591.485 (10)
C5—H5B0.9600C57—C581.376 (10)
C5—H5C0.9600C57—H57A0.9300
C6—H6A0.9700C58—C601.491 (10)
C6—H6B0.9700C59—H59A0.9600
C7—C81.369 (11)C59—H59B0.9600
C7—C101.493 (10)C59—H59C0.9600
C8—C91.400 (10)C60—H60A0.9600
C8—H8A0.9300C60—H60B0.9600
C9—C111.473 (10)C60—H60C0.9600
C10—H10A0.9600C61—H61A0.9700
C10—H10B0.9600C61—H61B0.9700
C10—H10C0.9600C62—C631.364 (11)
C11—H11A0.9600C62—C651.494 (11)
C11—H11B0.9600C63—C641.393 (11)
C11—H11C0.9600C63—H63A0.9300
C12—C131.364 (11)C64—C661.484 (11)
C12—C151.508 (10)C65—H65A0.9600
C13—C141.404 (10)C65—H65B0.9600
C13—H13A0.9300C65—H65C0.9600
C14—C161.499 (10)C66—H66A0.9600
C15—H15A0.9600C66—H66B0.9600
C15—H15B0.9600C66—H66C0.9600
C15—H15C0.9600
N7—Fe1—N4175.9 (2)C14—C16—H16C109.5
N7—Fe1—N584.3 (2)H16A—C16—H16C109.5
N4—Fe1—N592.5 (2)H16B—C16—H16C109.5
N7—Fe1—N193.0 (2)N6—C17—N8111.7 (6)
N4—Fe1—N184.4 (2)N6—C17—H17A109.3
N5—Fe1—N190.3 (2)N8—C17—H17A109.3
N7—Fe1—Cl1i93.18 (17)N6—C17—H17B109.3
N4—Fe1—Cl1i89.69 (17)N8—C17—H17B109.3
N5—Fe1—Cl1i95.11 (16)H17A—C17—H17B107.9
N1—Fe1—Cl1i172.16 (16)N8—C18—C19106.3 (6)
N7—Fe1—Cl190.80 (16)N8—C18—C21123.6 (7)
N4—Fe1—Cl192.58 (16)C19—C18—C21130.1 (7)
N5—Fe1—Cl1173.57 (16)C18—C19—C20106.4 (6)
N1—Fe1—Cl194.09 (16)C18—C19—H19A126.8
Cl1i—Fe1—Cl181.01 (9)C20—C19—H19A126.8
N7—Fe1—Fe1i92.62 (17)N7—C20—C19111.1 (6)
N4—Fe1—Fe1i91.49 (17)N7—C20—C22121.1 (6)
N5—Fe1—Fe1i135.41 (16)C19—C20—C22127.7 (6)
N1—Fe1—Fe1i134.28 (15)C18—C21—H21A109.5
Cl1i—Fe1—Fe1i40.52 (5)C18—C21—H21B109.5
Cl1—Fe1—Fe1i40.49 (6)H21A—C21—H21B109.5
N11—Fe2—N15176.1 (2)C18—C21—H21C109.5
N11—Fe2—N984.6 (2)H21A—C21—H21C109.5
N15—Fe2—N993.6 (2)H21B—C21—H21C109.5
N11—Fe2—N1391.8 (2)C20—C22—H22A109.5
N15—Fe2—N1384.7 (2)C20—C22—H22B109.5
N9—Fe2—N1389.8 (2)H22A—C22—H22B109.5
N11—Fe2—Cl389.59 (18)C20—C22—H22C109.5
N15—Fe2—Cl392.54 (17)H22A—C22—H22C109.5
N9—Fe2—Cl3172.30 (17)H22B—C22—H22C109.5
N13—Fe2—Cl395.43 (18)C24—C23—N10106.9 (7)
N11—Fe2—Cl294.50 (17)C24—C23—C26131.4 (9)
N15—Fe2—Cl289.04 (16)N10—C23—C26121.7 (8)
N9—Fe2—Cl293.04 (17)C23—C24—C25107.5 (8)
N13—Fe2—Cl2173.29 (17)C23—C24—H24A126.3
Cl3—Fe2—Cl282.42 (9)C25—C24—H24A126.3
N11—Fe2—Fe393.45 (17)N9—C25—C24110.4 (8)
N15—Fe2—Fe390.32 (17)N9—C25—C27121.4 (7)
N9—Fe2—Fe3133.71 (16)C24—C25—C27128.1 (8)
N13—Fe2—Fe3136.52 (17)C23—C26—H26A109.5
Cl3—Fe2—Fe341.56 (6)C23—C26—H26B109.5
Cl2—Fe2—Fe340.88 (6)H26A—C26—H26B109.5
N19—Fe3—N23175.4 (2)C23—C26—H26C109.5
N19—Fe3—N2192.1 (2)H26A—C26—H26C109.5
N23—Fe3—N2183.9 (2)H26B—C26—H26C109.5
N19—Fe3—N1784.4 (2)C25—C27—H27A109.5
N23—Fe3—N1793.5 (2)C25—C27—H27B109.5
N21—Fe3—N1791.8 (2)H27A—C27—H27B109.5
N19—Fe3—Cl292.93 (19)C25—C27—H27C109.5
N23—Fe3—Cl291.30 (17)H27A—C27—H27C109.5
N21—Fe3—Cl2172.22 (17)H27B—C27—H27C109.5
N17—Fe3—Cl294.60 (18)N10—C28—N12111.5 (6)
N19—Fe3—Cl388.04 (18)N10—C28—H28A109.3
N23—Fe3—Cl394.39 (17)N12—C28—H28A109.3
N21—Fe3—Cl392.45 (17)N10—C28—H28B109.3
N17—Fe3—Cl3171.44 (18)N12—C28—H28B109.3
Cl2—Fe3—Cl381.80 (9)H28A—C28—H28B108.0
N19—Fe3—Fe291.30 (19)N12—C29—C30105.6 (6)
N23—Fe3—Fe293.09 (17)N12—C29—C32124.5 (7)
N21—Fe3—Fe2132.33 (16)C30—C29—C32129.9 (7)
N17—Fe3—Fe2135.84 (17)C29—C30—C31106.8 (7)
Cl2—Fe3—Fe241.62 (6)C29—C30—H30A126.6
Cl3—Fe3—Fe240.19 (6)C31—C30—H30A126.6
Cl6—Fe4—Cl7108.90 (13)N11—C31—C30110.4 (6)
Cl6—Fe4—Cl5110.04 (13)N11—C31—C33122.6 (6)
Cl7—Fe4—Cl5109.23 (11)C30—C31—C33127.0 (7)
Cl6—Fe4—Cl4109.57 (12)C29—C32—H32A109.5
Cl7—Fe4—Cl4108.78 (12)C29—C32—H32B109.5
Cl5—Fe4—Cl4110.28 (12)H32A—C32—H32B109.5
Cl11—Fe5—Cl10110.33 (14)C29—C32—H32C109.5
Cl11—Fe5—Cl9108.39 (13)H32A—C32—H32C109.5
Cl10—Fe5—Cl9111.11 (13)H32B—C32—H32C109.5
Cl11—Fe5—Cl8108.99 (11)C31—C33—H33A109.5
Cl10—Fe5—Cl8108.23 (13)C31—C33—H33B109.5
Cl9—Fe5—Cl8109.77 (10)H33A—C33—H33B109.5
Cl15—Fe6—Cl13109.96 (11)C31—C33—H33C109.5
Cl15—Fe6—Cl14110.51 (12)H33A—C33—H33C109.5
Cl13—Fe6—Cl14109.46 (11)H33B—C33—H33C109.5
Cl15—Fe6—Cl12107.95 (11)N14—C34—C35105.5 (7)
Cl13—Fe6—Cl12109.50 (11)N14—C34—C37121.9 (9)
Cl14—Fe6—Cl12109.43 (11)C35—C34—C37132.5 (9)
Fe1i—Cl1—Fe198.99 (9)C34—C35—C36108.0 (8)
Fe3—Cl2—Fe297.50 (9)C34—C35—H35A126.0
Fe2—Cl3—Fe398.25 (10)C36—C35—H35A126.0
C3—N1—N2105.4 (6)N13—C36—C35109.5 (8)
C3—N1—Fe1135.0 (5)N13—C36—C38122.8 (8)
N2—N1—Fe1118.3 (4)C35—C36—C38127.6 (8)
C1—N2—N1111.1 (6)C34—C37—H37A109.5
C1—N2—C6129.3 (7)C34—C37—H37B109.5
N1—N2—C6119.5 (6)H37A—C37—H37B109.5
C7—N3—N4111.8 (6)C34—C37—H37C109.5
C7—N3—C6129.6 (6)H37A—C37—H37C109.5
N4—N3—C6118.5 (5)H37B—C37—H37C109.5
C9—N4—N3104.8 (5)C36—C38—H38A109.5
C9—N4—Fe1134.9 (5)C36—C38—H38B109.5
N3—N4—Fe1120.2 (4)H38A—C38—H38B109.5
C14—N5—N6104.7 (6)C36—C38—H38C109.5
C14—N5—Fe1137.0 (5)H38A—C38—H38C109.5
N6—N5—Fe1117.7 (4)H38B—C38—H38C109.5
C12—N6—N5111.1 (6)N14—C39—N16112.4 (6)
C12—N6—C17128.5 (6)N14—C39—H39A109.1
N5—N6—C17120.4 (6)N16—C39—H39A109.1
C20—N7—N8103.5 (5)N14—C39—H39B109.1
C20—N7—Fe1135.9 (5)N16—C39—H39B109.1
N8—N7—Fe1120.6 (4)H39A—C39—H39B107.9
C18—N8—N7112.6 (6)N16—C40—C41106.0 (7)
C18—N8—C17128.4 (6)N16—C40—C43124.3 (7)
N7—N8—C17119.0 (5)C41—C40—C43129.7 (7)
C25—N9—N10104.4 (6)C40—C41—C42106.8 (6)
C25—N9—Fe2135.2 (5)C40—C41—H41A126.6
N10—N9—Fe2118.0 (5)C42—C41—H41A126.6
C23—N10—N9110.8 (6)N15—C42—C41110.3 (6)
C23—N10—C28129.7 (7)N15—C42—C44122.0 (6)
N9—N10—C28119.3 (6)C41—C42—C44127.7 (7)
C31—N11—N12104.5 (5)C40—C43—H43A109.5
C31—N11—Fe2135.4 (5)C40—C43—H43B109.5
N12—N11—Fe2120.0 (4)H43A—C43—H43B109.5
C29—N12—N11112.6 (6)C40—C43—H43C109.5
C29—N12—C28129.1 (6)H43A—C43—H43C109.5
N11—N12—C28118.2 (5)H43B—C43—H43C109.5
C36—N13—N14104.9 (6)C42—C44—H44A109.5
C36—N13—Fe2133.4 (5)C42—C44—H44B109.5
N14—N13—Fe2115.9 (5)H44A—C44—H44B109.5
C34—N14—N13112.1 (7)C42—C44—H44C109.5
C34—N14—C39129.0 (7)H44A—C44—H44C109.5
N13—N14—C39118.9 (6)H44B—C44—H44C109.5
C42—N15—N16104.3 (5)C46—C45—N18105.8 (7)
C42—N15—Fe2135.5 (5)C46—C45—C48130.8 (9)
N16—N15—Fe2120.0 (4)N18—C45—C48123.3 (9)
C40—N16—N15112.6 (6)C45—C46—C47108.1 (8)
C40—N16—C39129.4 (6)C45—C46—H46A125.9
N15—N16—C39117.6 (5)C47—C46—H46A125.9
C47—N17—N18104.8 (6)N17—C47—C46109.3 (8)
C47—N17—Fe3136.7 (5)N17—C47—C49121.3 (7)
N18—N17—Fe3118.5 (5)C46—C47—C49129.3 (9)
C45—N18—N17111.9 (7)C45—C48—H48A109.5
C45—N18—C50128.5 (7)C45—C48—H48B109.5
N17—N18—C50119.6 (6)H48A—C48—H48B109.5
C53—N19—N20105.1 (6)C45—C48—H48C109.5
C53—N19—Fe3134.9 (5)H48A—C48—H48C109.5
N20—N19—Fe3119.6 (4)H48B—C48—H48C109.5
C51—N20—N19111.5 (6)C47—C49—H49A109.5
C51—N20—C50128.7 (7)C47—C49—H49B109.5
N19—N20—C50119.8 (6)H49A—C49—H49B109.5
C58—N21—N22104.3 (6)C47—C49—H49C109.5
C58—N21—Fe3136.6 (5)H49A—C49—H49C109.5
N22—N21—Fe3117.6 (5)H49B—C49—H49C109.5
C56—N22—N21111.7 (6)N20—C50—N18112.3 (7)
C56—N22—C61128.5 (6)N20—C50—H50A109.1
N21—N22—C61119.8 (6)N18—C50—H50A109.1
C64—N23—N24105.1 (6)N20—C50—H50B109.1
C64—N23—Fe3134.8 (5)N18—C50—H50B109.1
N24—N23—Fe3119.1 (4)H50A—C50—H50B107.9
C62—N24—N23111.3 (6)N20—C51—C52106.8 (7)
C62—N24—C61129.7 (6)N20—C51—C54123.1 (7)
N23—N24—C61118.4 (6)C52—C51—C54130.1 (8)
N2—C1—C2107.5 (7)C51—C52—C53107.4 (7)
N2—C1—C5122.4 (8)C51—C52—H52A126.3
C2—C1—C5130.0 (8)C53—C52—H52A126.3
C1—C2—C3106.4 (7)N19—C53—C52109.1 (7)
C1—C2—H2A126.8N19—C53—C55122.9 (6)
C3—C2—H2A126.8C52—C53—C55128.0 (7)
N1—C3—C2109.7 (7)C51—C54—H54A109.5
N1—C3—C4123.6 (6)C51—C54—H54B109.5
C2—C3—C4126.7 (7)H54A—C54—H54B109.5
C3—C4—H4A109.5C51—C54—H54C109.5
C3—C4—H4B109.5H54A—C54—H54C109.5
H4A—C4—H4B109.5H54B—C54—H54C109.5
C3—C4—H4C109.5C53—C55—H55A109.5
H4A—C4—H4C109.5C53—C55—H55B109.5
H4B—C4—H4C109.5H55A—C55—H55B109.5
C1—C5—H5A109.5C53—C55—H55C109.5
C1—C5—H5B109.5H55A—C55—H55C109.5
H5A—C5—H5B109.5H55B—C55—H55C109.5
C1—C5—H5C109.5C57—C56—N22105.5 (6)
H5A—C5—H5C109.5C57—C56—C59132.1 (8)
H5B—C5—H5C109.5N22—C56—C59122.3 (8)
N2—C6—N3113.0 (6)C56—C57—C58107.6 (7)
N2—C6—H6A109.0C56—C57—H57A126.2
N3—C6—H6A109.0C58—C57—H57A126.2
N2—C6—H6B109.0N21—C58—C57110.8 (7)
N3—C6—H6B109.0N21—C58—C60121.6 (7)
H6A—C6—H6B107.8C57—C58—C60127.6 (7)
N3—C7—C8106.6 (6)C56—C59—H59A109.5
N3—C7—C10124.3 (7)C56—C59—H59B109.5
C8—C7—C10129.1 (7)H59A—C59—H59B109.5
C7—C8—C9106.9 (7)C56—C59—H59C109.5
C7—C8—H8A126.6H59A—C59—H59C109.5
C9—C8—H8A126.6H59B—C59—H59C109.5
N4—C9—C8109.7 (7)C58—C60—H60A109.5
N4—C9—C11122.4 (7)C58—C60—H60B109.5
C8—C9—C11127.9 (7)H60A—C60—H60B109.5
C7—C10—H10A109.5C58—C60—H60C109.5
C7—C10—H10B109.5H60A—C60—H60C109.5
H10A—C10—H10B109.5H60B—C60—H60C109.5
C7—C10—H10C109.5N24—C61—N22112.5 (6)
H10A—C10—H10C109.5N24—C61—H61A109.1
H10B—C10—H10C109.5N22—C61—H61A109.1
C9—C11—H11A109.5N24—C61—H61B109.1
C9—C11—H11B109.5N22—C61—H61B109.1
H11A—C11—H11B109.5H61A—C61—H61B107.8
C9—C11—H11C109.5N24—C62—C63106.8 (7)
H11A—C11—H11C109.5N24—C62—C65122.7 (7)
H11B—C11—H11C109.5C63—C62—C65130.5 (7)
N6—C12—C13107.0 (6)C62—C63—C64107.3 (7)
N6—C12—C15123.5 (7)C62—C63—H63A126.3
C13—C12—C15129.5 (7)C64—C63—H63A126.3
C12—C13—C14106.0 (7)N23—C64—C63109.4 (7)
C12—C13—H13A127.0N23—C64—C66122.8 (7)
C14—C13—H13A127.0C63—C64—C66127.8 (7)
N5—C14—C13111.3 (6)C62—C65—H65A109.5
N5—C14—C16121.6 (7)C62—C65—H65B109.5
C13—C14—C16127.1 (7)H65A—C65—H65B109.5
C12—C15—H15A109.5C62—C65—H65C109.5
C12—C15—H15B109.5H65A—C65—H65C109.5
H15A—C15—H15B109.5H65B—C65—H65C109.5
C12—C15—H15C109.5C64—C66—H66A109.5
H15A—C15—H15C109.5C64—C66—H66B109.5
H15B—C15—H15C109.5H66A—C66—H66B109.5
C14—C16—H16A109.5C64—C66—H66C109.5
C14—C16—H16B109.5H66A—C66—H66C109.5
H16A—C16—H16B109.5H66B—C66—H66C109.5

Symmetry codes: (i) −x+1, −y+1, −z+1.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BR2084).

References

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