metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 68| Part 5| May 2012| Pages m531-m532

Tris(1,10-phenanthroline-κ2N,N′)iron(II) bis­­[(1,10-phenanthroline-κ2N,N′)tetra­kis­(thio­cyanato-κN)chromate(III)] aceto­nitrile tris­­olvate monohydrate

aDepartment of Inorganic Chemistry, Taras Shevchenko National University of Kyiv, 64 Volodymyrs'ka St., Kyiv 01601, Ukraine, and bDepartment of Chemistry of Complex Compounds, V.I. Vernadsky Institute of General and Inorganic Chemistry, National Academy of Sciences of Ukraine, 32/34 Palladin Ave., Kyiv 03680, Ukraine
*Correspondence e-mail: valya.semenaka@gmail.com

(Received 15 March 2012; accepted 24 March 2012; online 4 April 2012)

Single crystals of the title heterometallic compound, [Fe(C12H8N2)3][Cr(NCS)4(C12H8N2)]2·3CH3CN·H2O or [Fe(Cphen)3][Cr(NCS)4(phen)]2·3CH3CN·H2O, were pre­pared using the one-pot open-air reaction of iron powder, Reineckes salt and 1,10-phenanthroline (phen) in acetonitrile. The asymetric unit consists of an [Fe(phen)3]2+ cation, two [Cr(phen)(NCS)4] anions, three acetonitrile solvent mol­ecules and a water mol­ecule. The Fe and Cr atoms both show a slightly distorted octa­hedral FeN6 and CrN6 coordination geometry with adjacent angles in the range 79.67 (12)–95.21 (12)°. No classical hydrogen bonding involving the water molecule is observed.

Related literature

For background to direct synthesis, see: Makhankova (2011[Makhankova, V. G. (2011). Glob. J. Inorg. Chem. 2, 265-285.]). For background to the use of Reineckes salt as a source of building blocks or metalloligands, see: Zhang et al. (2001[Zhang, K.-L., Chen, W., Xu, Y., Wang, Z., Zhong, Z. J. & You, X.-Z. (2001). Polyhedron, 20, 2033-2036.]); Cucos et al. (2006[Cucos, A., Avarvari, N., Andruh, M., Journaux, Y., Muller, A. & Schmidtmann, M. (2006). Eur. J. Inorg. Chem. pp. 903-907.]); Cherkasova & Gorunova (2003[Cherkasova, T. G. & Gorunova, I. P. (2003). Zh. Neorg. Khim. 48, 611-615.]); Nikitina et al. (2009[Nikitina, V. M., Nesterova, O. V., Kokozay, V. N., Dyakonenko, V. V., Shishkin, O. V. & Jezierska, J. (2009). Polyhedron, 28, 1265-1272.]); Kolotilov et al. (2010[Kolotilov, S. V., Cador, O., Gavrilenko, K. S., Golhen, S., Ouahab, L. & Pavlishchuk, V. V. (2010). Eur. J. Inorg. Chem. 8, 1255-1266.]). For Fe—N bond lengths in iron–phen derivatives, see: Alonso et al. (2005[Alonso, C., Ballster, L., Gutierrez, F., Rerpinaqn, M. F., Sanchez, A. E. & Azcondo, M. T. (2005). Eur. J. Inorg. Chem. pp. 486-495.]). For a related structure, see: Semenaka et al. (2011[Semenaka, V. V., Nesterova, O. V., Kokozay, V. N., Zybatyuk, R. I. & Shishkin, O. V. (2011). Acta Cryst. E67, m1021-m1022.]).

[Scheme 1]

Experimental

Crystal data
  • [Fe(C12H8N2)3][Cr(NCS)4(C12H8N2)]2·3C2H3N·H2O

  • Mr = 1666.69

  • Triclinic, [P \overline 1]

  • a = 12.641 (2) Å

  • b = 16.681 (3) Å

  • c = 20.692 (4) Å

  • α = 111.514 (5)°

  • β = 107.291 (6)°

  • γ = 92.231 (5)°

  • V = 3821.5 (13) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 0.75 mm−1

  • T = 173 K

  • 0.23 × 0.22 × 0.12 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS.. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.847, Tmax = 0.916

  • 48046 measured reflections

  • 15519 independent reflections

  • 8993 reflections with I > 2σ(I)

  • Rint = 0.078

Refinement
  • R[F2 > 2σ(F2)] = 0.051

  • wR(F2) = 0.135

  • S = 0.99

  • 15519 reflections

  • 974 parameters

  • 3 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.43 e Å−3

  • Δρmin = −0.44 e Å−3

Data collection: APEX2 (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS.. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS.. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Supporting information


Comment top

Recently we have reported that the Reineckes salt, (NH)4[Cr(NCS)4(NH3)2].H2O, could be exploited as a source of building blocks or metalloligands in the direct synthesis of heterometallic Cu/Cr and Co/Cr compounds with amines and Schiff-base ligands (Nikitina et al.., 2009; Semenaka et al.., 2011). In the present work, we report that the reaction of iron powder, Reineckes salt and 1,10-phenanthroline (phen) in acetonitrile solution has afforded a single crystals of the novel heterometallic Fe/Cr compound. The asymetric unit of title compound consists of slightly distorted octahedral [Fe(phen)3]2+ cation and two [Cr(phen)(NCS)4]- anion blocks as well as solvate acetonitrile and water molecules (Fig. 1). In complex cation iron centers are in elongated octahedral coordination environment with six nitrogen atoms phen ligands. The bond lengths of Fe–N vary in the range 1,959 (3) – 1,980 (3) Å which is in the range usually found in other iron-phen derivatives (Alonso et al., 2005). The cis and trans N–Fe–N bond angles vary from 82,27 (12)° to 95.21 (12)° and from 172.90 (12)° to 174.04 (11)°, respectively. The Cr(III) ions have N6 donor set formed by two N atoms from phen, which are replaced NCS groups in initial anions of Reineckes salt, and two NCS-groups in the equatorial plane and by two another NCS-groups at the axial positions. The axial Cr–N bond lengths are vary from 1,962 (3) to 2,077 (3) Å. The cis and trans N–Cr–N bond angles vary from 79,80 (11)° to 94,97 (12)° and from 170,61 (12)° to 174,77 (12)°, respectively. The thiocyanate groups are almost linear, bond angles N–C–S are in a narrow range: from 178.1 (3) ° to 179.3 (4)°.

Related literature top

For background to direct synthesis, see: Makhankova (2011). For background to the use of Reineckes salt as a source of building blocks or metalloligands, see: Zhang et al. (2001); Cucos et al. (2006); Cherkasova & Gorunova (2003); Nikitina et al. (2009); Kolotilov et al. (2010). For Fe—N bond lengths in iron–phen derivatives, see: Alonso et al. (2005). For a related structure, see: Semenaka et al. (2011).

Experimental top

Iron powder (0.07 g, 1.25 mmol), NH4[Cr(NCS)4(NH3)2].H2O (0.443 g, 1.25 mmol), NH4NCS (0.190 g, 2.5 mmol), phen.H2O (0.496 g, 2.5 mmol) and acetonitrile (15 ml) were heated to 50–60° and stirred magnetically until total dissolution of the iron was observed (4,5 h). The resulting red solution was slowly evaporated at room temperature until dark-red crystals suitable for crystallographic study were formed. The crystals were filtered off, washed with dry PriOH and finally dried in vacuo at room temperature. Yield: 0.25 g. IR (KBr, cm-1): 3048(sh), 3044(sh), 2314(w), 2066(vs), 1996(sh), 1645(sh), 1638(sh), 1635(m), 1599(m), 1578(m), 1554(sh), 1536(w), 1521(m), 1494(sh), 1472(sh), 1455(sh), 1424(s), 1409(sh), 1373(w), 1307(w), 1271(w), 1256(sh), 1223(sh), 1207(w), 1144(m), 1102(m), 1057(sh), 1039(sh), 990(m), 960(w), 942(sh), 915(sh), 876(w), 870(sh), 843(s), 798(m), 771(w), 737(sh), 719(s), 668(sh), 656(w), 620(w), 581(sh), 557(w), 626(w), 568(sh), 481(m), 451(sh), 433(w), 427(sh). The compound is sparingly soluble in dmso and dmf, insoluble in water and it is indefinitely stable in air.

Refinement top

All non-hydrogen atoms were located from the initial solution and refined with anisotropic thermal parameters. The hydrogen atoms were positioned geometrically and included into refinement using riding model approximation with Uiso = nUeq of non-hydrogen carrier atom (n = 1.5 for CH3 groups and n = 1.2 for remaining H-atoms)

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXS97 (Sheldrick, 2008); molecular graphics: PLATON (Spek, 2009); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. Crystal structure of the complex, showing the atom numbering, with 50% probability displacement ellipsoids. Solvent molecules are omitted for clarity.
Tris(1,10-phenanthroline-κ2N,N')iron(II) bis[(1,10-phenanthroline-κ2N,N')tetrakis(thiocyanato- κN)chromate(III)] acetonitrile trisolvate monohydrate top
Crystal data top
[Fe(C12H8N2)3][Cr(NCS)4(C12H8N2)]2·3C2H3N·H2OZ = 2
Mr = 1666.69F(000) = 1704
Triclinic, P1Dx = 1.448 Mg m3
a = 12.641 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 16.681 (3) ÅCell parameters from 4485 reflections
c = 20.692 (4) Åθ = 2.3–21.7°
α = 111.514 (5)°µ = 0.75 mm1
β = 107.291 (6)°T = 173 K
γ = 92.231 (5)°Block, red
V = 3821.5 (13) Å30.23 × 0.22 × 0.12 mm
Data collection top
Bruker APEXII CCD
diffractometer
15519 independent reflections
Radiation source: fine-focus sealed tube8993 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.078
ϕ and ω scansθmax = 26.4°, θmin = 1.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2005)
h = 1515
Tmin = 0.847, Tmax = 0.916k = 2020
48046 measured reflectionsl = 2525
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)] = 0.051Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.135H atoms treated by a mixture of independent and constrained refinement
S = 0.99 w = 1/[σ2(Fo2) + (0.0572P)2 + 0.0054P]
where P = (Fo2 + 2Fc2)/3
15519 reflections(Δ/σ)max < 0.001
974 parametersΔρmax = 0.43 e Å3
3 restraintsΔρmin = 0.44 e Å3
Crystal data top
[Fe(C12H8N2)3][Cr(NCS)4(C12H8N2)]2·3C2H3N·H2Oγ = 92.231 (5)°
Mr = 1666.69V = 3821.5 (13) Å3
Triclinic, P1Z = 2
a = 12.641 (2) ÅMo Kα radiation
b = 16.681 (3) ŵ = 0.75 mm1
c = 20.692 (4) ÅT = 173 K
α = 111.514 (5)°0.23 × 0.22 × 0.12 mm
β = 107.291 (6)°
Data collection top
Bruker APEXII CCD
diffractometer
15519 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2005)
8993 reflections with I > 2σ(I)
Tmin = 0.847, Tmax = 0.916Rint = 0.078
48046 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0513 restraints
wR(F2) = 0.135H atoms treated by a mixture of independent and constrained refinement
S = 0.99Δρmax = 0.43 e Å3
15519 reflectionsΔρmin = 0.44 e Å3
974 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
Cr10.27228 (5)0.11974 (4)0.24479 (4)0.03091 (17)
Cr20.65438 (5)0.31815 (4)0.08754 (3)0.02873 (16)
Fe10.21655 (4)0.67016 (4)0.34300 (3)0.02632 (14)
S10.27329 (12)0.22111 (9)0.49075 (7)0.0579 (4)
S20.09452 (10)0.17085 (8)0.16961 (8)0.0536 (3)
S30.62676 (10)0.06152 (8)0.35925 (7)0.0531 (3)
S40.37743 (12)0.41344 (8)0.28415 (7)0.0530 (3)
S50.77068 (12)0.50790 (9)0.33991 (7)0.0604 (4)
S60.65109 (9)0.07691 (8)0.15795 (7)0.0441 (3)
S70.62707 (10)0.59283 (8)0.07321 (7)0.0491 (3)
S81.02840 (9)0.36578 (8)0.08940 (7)0.0451 (3)
N10.2488 (3)0.1575 (2)0.3417 (2)0.0376 (9)
N20.2035 (3)0.0022 (2)0.21591 (19)0.0371 (9)
N30.4240 (3)0.0943 (2)0.28350 (18)0.0356 (8)
N40.3298 (3)0.2410 (2)0.26495 (18)0.0358 (8)
N50.6900 (3)0.3873 (2)0.1943 (2)0.0371 (9)
N60.6551 (3)0.2076 (2)0.10439 (18)0.0346 (8)
N70.6422 (3)0.4265 (2)0.07093 (18)0.0341 (8)
N80.8136 (3)0.3295 (2)0.09225 (18)0.0354 (8)
N90.2783 (3)0.0844 (2)0.13939 (18)0.0309 (8)
N100.1155 (3)0.1396 (2)0.19199 (17)0.0285 (7)
N110.6017 (3)0.2448 (2)0.02542 (17)0.0300 (8)
N120.4819 (3)0.2997 (2)0.06400 (17)0.0277 (7)
N130.3234 (3)0.6688 (2)0.43423 (17)0.0318 (8)
N140.1557 (3)0.5523 (2)0.33057 (17)0.0277 (7)
N150.3167 (3)0.6249 (2)0.28571 (18)0.0304 (8)
N160.1125 (3)0.6567 (2)0.24675 (18)0.0303 (8)
N170.2766 (3)0.7928 (2)0.36711 (18)0.0318 (8)
N180.1187 (3)0.7270 (2)0.39894 (17)0.0294 (8)
C10.2574 (3)0.1841 (3)0.4040 (3)0.0363 (10)
C20.1576 (3)0.0722 (3)0.1971 (2)0.0335 (10)
C30.5093 (3)0.0804 (3)0.3150 (2)0.0363 (10)
C40.3482 (3)0.3134 (3)0.2722 (2)0.0304 (9)
C50.7241 (3)0.4381 (3)0.2550 (3)0.0359 (10)
C60.6516 (3)0.1528 (3)0.1264 (2)0.0298 (9)
C70.6361 (3)0.4963 (3)0.0724 (2)0.0294 (9)
C80.9035 (3)0.3456 (3)0.0913 (2)0.0323 (10)
C90.3598 (3)0.0550 (3)0.1145 (2)0.0423 (11)
H90.42600.04870.14780.051*
C100.3528 (4)0.0328 (3)0.0414 (3)0.0476 (12)
H100.41300.01120.02540.057*
C110.2582 (4)0.0423 (3)0.0073 (2)0.0411 (11)
H110.25300.02810.05720.049*
C120.1700 (3)0.0730 (3)0.0169 (2)0.0346 (10)
C130.1840 (3)0.0932 (2)0.0913 (2)0.0301 (9)
C140.0672 (4)0.0842 (3)0.0288 (2)0.0390 (11)
H140.05720.07160.07920.047*
C150.0159 (3)0.1123 (3)0.0024 (2)0.0382 (11)
H150.08320.11920.03430.046*
C160.0044 (3)0.1321 (2)0.0735 (2)0.0315 (10)
C170.0967 (3)0.1231 (2)0.1195 (2)0.0279 (9)
C180.0874 (3)0.1580 (3)0.1043 (2)0.0362 (10)
H180.15780.16360.07460.043*
C190.0685 (3)0.1754 (3)0.1769 (2)0.0379 (10)
H190.12480.19440.19820.045*
C200.0349 (3)0.1652 (2)0.2197 (2)0.0344 (10)
H200.04750.17690.27020.041*
C210.6622 (4)0.2196 (3)0.0695 (2)0.0428 (11)
H210.74150.23670.04870.051*
C220.6150 (4)0.1688 (3)0.1451 (3)0.0525 (13)
H220.66160.15190.17470.063*
C230.5010 (4)0.1438 (3)0.1760 (3)0.0482 (12)
H230.46790.10790.22710.058*
C240.4338 (4)0.1714 (3)0.1322 (2)0.0360 (10)
C250.4875 (3)0.2212 (2)0.0566 (2)0.0288 (9)
C260.3135 (4)0.1526 (3)0.1594 (2)0.0413 (11)
H260.27570.11780.21020.050*
C270.2526 (4)0.1829 (3)0.1146 (2)0.0392 (11)
H270.17290.17050.13470.047*
C280.3064 (3)0.2338 (2)0.0370 (2)0.0311 (9)
C290.4245 (3)0.2515 (2)0.0088 (2)0.0263 (9)
C300.2486 (3)0.2690 (3)0.0123 (2)0.0359 (10)
H300.16880.26010.00490.043*
C310.3074 (3)0.3161 (3)0.0850 (2)0.0388 (11)
H310.26870.33940.11900.047*
C320.4244 (3)0.3298 (3)0.1094 (2)0.0343 (10)
H320.46430.36190.16040.041*
C330.4073 (3)0.7303 (3)0.4874 (2)0.0407 (11)
H330.42050.78460.48350.049*
C340.4762 (4)0.7181 (3)0.5483 (2)0.0498 (13)
H340.53520.76340.58490.060*
C350.4589 (4)0.6411 (4)0.5554 (2)0.0526 (13)
H350.50640.63250.59660.063*
C360.3710 (4)0.5746 (3)0.5017 (2)0.0428 (11)
C370.3056 (3)0.5923 (3)0.4424 (2)0.0316 (9)
C380.3420 (4)0.4927 (3)0.5040 (3)0.0514 (13)
H380.38650.47960.54360.062*
C390.2537 (5)0.4335 (3)0.4520 (3)0.0540 (13)
H390.23610.37990.45580.065*
C400.1863 (4)0.4501 (3)0.3911 (2)0.0407 (11)
C410.2133 (3)0.5289 (3)0.3860 (2)0.0304 (9)
C420.0900 (4)0.3932 (3)0.3352 (3)0.0492 (13)
H420.06590.33920.33620.059*
C430.0321 (4)0.4165 (3)0.2800 (2)0.0456 (12)
H430.03320.37870.24240.055*
C440.0675 (4)0.4948 (3)0.2780 (2)0.0372 (10)
H440.02720.50810.23760.045*
C450.4222 (3)0.6122 (3)0.3077 (3)0.0388 (11)
H450.45870.62540.35850.047*
C460.4818 (4)0.5801 (3)0.2591 (3)0.0531 (14)
H460.55640.57020.27680.064*
C470.4325 (5)0.5629 (3)0.1860 (3)0.0582 (15)
H470.47310.54220.15280.070*
C480.3220 (4)0.5761 (3)0.1604 (3)0.0462 (12)
C490.2676 (4)0.6073 (2)0.2123 (2)0.0326 (10)
C500.2600 (6)0.5605 (3)0.0852 (3)0.0634 (16)
H500.29540.53990.04890.076*
C510.1544 (6)0.5741 (3)0.0648 (3)0.0615 (16)
H510.11620.56250.01450.074*
C520.0969 (5)0.6058 (3)0.1170 (2)0.0466 (12)
C530.1562 (4)0.6232 (2)0.1911 (2)0.0347 (10)
C540.0145 (5)0.6198 (3)0.1000 (3)0.0519 (14)
H540.05920.60690.05040.062*
C550.0581 (4)0.6523 (3)0.1554 (3)0.0479 (12)
H550.13370.66220.14440.057*
C560.0075 (3)0.6712 (3)0.2281 (2)0.0383 (11)
H560.02430.69540.26590.046*
C570.3560 (4)0.8248 (3)0.3485 (3)0.0436 (11)
H570.38770.78530.31590.052*
C580.3943 (4)0.9148 (3)0.3754 (3)0.0540 (13)
H580.45100.93530.36100.065*
C590.3506 (4)0.9725 (3)0.4218 (3)0.0509 (13)
H590.37701.03340.44020.061*
C600.2657 (3)0.9420 (3)0.4428 (2)0.0377 (10)
C610.2327 (3)0.8515 (3)0.4135 (2)0.0310 (9)
C620.2158 (4)0.9964 (3)0.4924 (2)0.0450 (12)
H620.23951.05790.51350.054*
C630.1353 (4)0.9622 (3)0.5098 (2)0.0428 (11)
H630.10360.99990.54340.051*
C640.0968 (3)0.8696 (3)0.4785 (2)0.0350 (10)
C650.1474 (3)0.8161 (3)0.4315 (2)0.0304 (9)
C660.0108 (4)0.8297 (3)0.4916 (2)0.0458 (12)
H660.02650.86390.52300.055*
C670.0190 (4)0.7413 (3)0.4589 (2)0.0450 (12)
H670.07750.71350.46730.054*
C680.0361 (3)0.6915 (3)0.4129 (2)0.0379 (10)
H680.01410.62980.39070.045*
N210.9342 (4)0.8805 (3)0.3236 (3)0.0737 (14)
C700.6627 (4)0.7663 (3)0.3096 (3)0.0519 (13)
N200.6003 (4)0.8084 (3)0.3261 (3)0.0895 (17)
N190.9140 (5)0.2258 (4)0.3444 (3)0.0921 (18)
C690.7423 (4)0.7123 (3)0.2876 (3)0.0703 (16)
H69A0.74750.66770.30820.106*
H69B0.81620.74870.30590.106*
H69C0.71750.68390.23360.106*
C740.8294 (6)0.2449 (4)0.3437 (3)0.078 (2)
C750.7198 (6)0.2697 (4)0.3412 (4)0.105 (3)
H75A0.67190.25210.28980.158*
H75B0.72850.33320.36720.158*
H75C0.68510.24050.36510.158*
C780.9856 (6)1.0175 (4)0.3033 (3)0.105 (3)
H78A1.05941.04930.33880.158*
H78B0.92881.05520.30990.158*
H78C0.98761.00020.25300.158*
C770.9574 (4)0.9401 (4)0.3151 (3)0.0577 (15)
O10.0464 (10)0.5593 (6)0.5096 (4)0.250 (5)
H1O0.065 (13)0.589 (9)0.5548 (17)0.376*
H2O0.001 (11)0.585 (10)0.490 (7)0.376*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr10.0235 (3)0.0264 (4)0.0375 (4)0.0009 (3)0.0060 (3)0.0105 (3)
Cr20.0239 (3)0.0303 (4)0.0328 (4)0.0069 (3)0.0082 (3)0.0142 (3)
Fe10.0257 (3)0.0230 (3)0.0286 (3)0.0021 (2)0.0103 (3)0.0076 (3)
S10.0837 (10)0.0521 (9)0.0546 (8)0.0133 (7)0.0436 (8)0.0232 (7)
S20.0506 (8)0.0322 (7)0.0728 (9)0.0058 (6)0.0107 (7)0.0243 (7)
S30.0345 (7)0.0514 (8)0.0649 (9)0.0073 (6)0.0027 (6)0.0289 (7)
S40.0887 (10)0.0291 (7)0.0478 (8)0.0071 (6)0.0297 (7)0.0174 (6)
S50.0675 (9)0.0559 (9)0.0355 (7)0.0033 (7)0.0024 (6)0.0060 (7)
S60.0362 (6)0.0504 (8)0.0618 (8)0.0098 (5)0.0209 (6)0.0363 (7)
S70.0433 (7)0.0339 (7)0.0687 (9)0.0040 (5)0.0086 (6)0.0272 (7)
S80.0311 (6)0.0551 (8)0.0519 (7)0.0036 (5)0.0177 (6)0.0217 (6)
N10.033 (2)0.036 (2)0.037 (2)0.0016 (16)0.0077 (18)0.0109 (19)
N20.031 (2)0.030 (2)0.046 (2)0.0031 (16)0.0094 (17)0.0133 (19)
N30.029 (2)0.034 (2)0.035 (2)0.0020 (16)0.0022 (17)0.0109 (18)
N40.0296 (19)0.031 (2)0.039 (2)0.0029 (16)0.0026 (16)0.0126 (18)
N50.036 (2)0.038 (2)0.034 (2)0.0043 (17)0.0089 (18)0.0132 (19)
N60.0309 (19)0.034 (2)0.043 (2)0.0087 (16)0.0124 (17)0.0190 (19)
N70.0314 (19)0.036 (2)0.034 (2)0.0055 (16)0.0067 (16)0.0164 (18)
N80.0265 (19)0.035 (2)0.043 (2)0.0063 (16)0.0072 (17)0.0175 (18)
N90.0203 (17)0.030 (2)0.038 (2)0.0013 (15)0.0074 (16)0.0109 (17)
N100.0224 (17)0.0243 (19)0.034 (2)0.0016 (14)0.0069 (15)0.0082 (16)
N110.0310 (19)0.030 (2)0.034 (2)0.0117 (15)0.0126 (16)0.0151 (17)
N120.0289 (18)0.0254 (19)0.031 (2)0.0070 (15)0.0108 (16)0.0124 (16)
N130.0271 (18)0.030 (2)0.032 (2)0.0050 (15)0.0102 (16)0.0053 (17)
N140.0282 (18)0.0273 (19)0.0263 (18)0.0027 (15)0.0106 (15)0.0081 (16)
N150.035 (2)0.0222 (19)0.039 (2)0.0055 (15)0.0183 (17)0.0126 (17)
N160.035 (2)0.0231 (19)0.036 (2)0.0023 (15)0.0148 (17)0.0134 (16)
N170.0312 (19)0.0223 (19)0.039 (2)0.0005 (15)0.0130 (17)0.0078 (17)
N180.0296 (18)0.033 (2)0.0282 (19)0.0064 (15)0.0106 (15)0.0138 (17)
C10.030 (2)0.028 (2)0.053 (3)0.0021 (19)0.017 (2)0.016 (2)
C20.029 (2)0.032 (3)0.040 (3)0.0062 (19)0.009 (2)0.017 (2)
C30.032 (2)0.034 (3)0.036 (3)0.003 (2)0.005 (2)0.013 (2)
C40.033 (2)0.031 (3)0.025 (2)0.0026 (19)0.0085 (18)0.010 (2)
C50.031 (2)0.036 (3)0.044 (3)0.008 (2)0.010 (2)0.021 (2)
C60.020 (2)0.035 (3)0.030 (2)0.0070 (18)0.0094 (18)0.007 (2)
C70.020 (2)0.038 (3)0.029 (2)0.0034 (18)0.0046 (18)0.016 (2)
C80.031 (2)0.030 (2)0.032 (2)0.0085 (19)0.0026 (19)0.014 (2)
C90.026 (2)0.048 (3)0.047 (3)0.006 (2)0.010 (2)0.014 (2)
C100.037 (3)0.054 (3)0.050 (3)0.009 (2)0.020 (2)0.014 (3)
C110.041 (3)0.037 (3)0.042 (3)0.000 (2)0.016 (2)0.010 (2)
C120.035 (2)0.024 (2)0.038 (3)0.0030 (19)0.011 (2)0.007 (2)
C130.024 (2)0.022 (2)0.037 (2)0.0023 (17)0.0084 (19)0.007 (2)
C140.042 (3)0.033 (3)0.038 (3)0.001 (2)0.008 (2)0.015 (2)
C150.033 (2)0.034 (3)0.047 (3)0.004 (2)0.004 (2)0.023 (2)
C160.027 (2)0.021 (2)0.041 (3)0.0006 (17)0.0040 (19)0.012 (2)
C170.023 (2)0.019 (2)0.037 (2)0.0018 (16)0.0060 (18)0.0090 (19)
C180.023 (2)0.030 (3)0.052 (3)0.0047 (18)0.005 (2)0.018 (2)
C190.026 (2)0.033 (3)0.051 (3)0.0045 (19)0.014 (2)0.011 (2)
C200.031 (2)0.027 (2)0.042 (3)0.0032 (18)0.013 (2)0.008 (2)
C210.037 (3)0.052 (3)0.044 (3)0.018 (2)0.019 (2)0.018 (3)
C220.053 (3)0.069 (4)0.040 (3)0.027 (3)0.026 (3)0.017 (3)
C230.059 (3)0.044 (3)0.033 (3)0.015 (2)0.015 (2)0.006 (2)
C240.042 (3)0.031 (3)0.032 (3)0.007 (2)0.009 (2)0.012 (2)
C250.031 (2)0.023 (2)0.033 (2)0.0071 (18)0.0100 (19)0.012 (2)
C260.045 (3)0.028 (3)0.035 (3)0.002 (2)0.000 (2)0.007 (2)
C270.031 (2)0.031 (3)0.046 (3)0.0037 (19)0.001 (2)0.015 (2)
C280.029 (2)0.023 (2)0.040 (3)0.0028 (18)0.008 (2)0.015 (2)
C290.029 (2)0.020 (2)0.030 (2)0.0035 (17)0.0094 (19)0.0111 (19)
C300.023 (2)0.033 (3)0.049 (3)0.0005 (19)0.009 (2)0.017 (2)
C310.032 (2)0.042 (3)0.052 (3)0.012 (2)0.024 (2)0.022 (2)
C320.032 (2)0.036 (3)0.033 (2)0.0055 (19)0.013 (2)0.011 (2)
C330.027 (2)0.039 (3)0.041 (3)0.003 (2)0.007 (2)0.003 (2)
C340.029 (3)0.063 (4)0.032 (3)0.001 (2)0.001 (2)0.001 (3)
C350.039 (3)0.082 (4)0.030 (3)0.022 (3)0.009 (2)0.016 (3)
C360.039 (3)0.055 (3)0.033 (3)0.019 (2)0.012 (2)0.014 (2)
C370.031 (2)0.033 (3)0.031 (2)0.0106 (19)0.0139 (19)0.011 (2)
C380.061 (3)0.064 (4)0.045 (3)0.033 (3)0.020 (3)0.035 (3)
C390.072 (4)0.051 (3)0.054 (3)0.026 (3)0.027 (3)0.032 (3)
C400.059 (3)0.036 (3)0.036 (3)0.013 (2)0.023 (2)0.017 (2)
C410.034 (2)0.030 (2)0.029 (2)0.0047 (19)0.0134 (19)0.012 (2)
C420.070 (3)0.031 (3)0.047 (3)0.003 (2)0.025 (3)0.012 (2)
C430.058 (3)0.034 (3)0.033 (3)0.011 (2)0.008 (2)0.008 (2)
C440.044 (3)0.029 (3)0.032 (2)0.005 (2)0.009 (2)0.007 (2)
C450.036 (3)0.026 (2)0.061 (3)0.0069 (19)0.027 (2)0.016 (2)
C460.051 (3)0.031 (3)0.094 (4)0.013 (2)0.048 (3)0.023 (3)
C470.080 (4)0.028 (3)0.088 (4)0.011 (3)0.067 (4)0.017 (3)
C480.066 (3)0.027 (3)0.055 (3)0.004 (2)0.041 (3)0.012 (2)
C490.049 (3)0.015 (2)0.039 (3)0.0032 (19)0.026 (2)0.0084 (19)
C500.106 (5)0.043 (3)0.055 (4)0.011 (3)0.053 (4)0.014 (3)
C510.116 (5)0.032 (3)0.035 (3)0.002 (3)0.032 (3)0.007 (2)
C520.079 (4)0.021 (2)0.031 (3)0.005 (2)0.012 (3)0.007 (2)
C530.051 (3)0.020 (2)0.035 (3)0.002 (2)0.019 (2)0.009 (2)
C540.076 (4)0.027 (3)0.031 (3)0.011 (2)0.009 (3)0.011 (2)
C550.050 (3)0.038 (3)0.050 (3)0.001 (2)0.001 (3)0.026 (3)
C560.035 (3)0.038 (3)0.041 (3)0.004 (2)0.008 (2)0.018 (2)
C570.043 (3)0.030 (3)0.064 (3)0.006 (2)0.030 (2)0.016 (2)
C580.052 (3)0.039 (3)0.078 (4)0.000 (2)0.030 (3)0.025 (3)
C590.051 (3)0.024 (3)0.073 (4)0.003 (2)0.020 (3)0.015 (3)
C600.036 (2)0.027 (3)0.043 (3)0.007 (2)0.009 (2)0.010 (2)
C610.031 (2)0.026 (2)0.033 (2)0.0090 (18)0.0069 (19)0.011 (2)
C620.046 (3)0.024 (3)0.045 (3)0.011 (2)0.004 (2)0.001 (2)
C630.046 (3)0.039 (3)0.033 (3)0.019 (2)0.011 (2)0.003 (2)
C640.034 (2)0.039 (3)0.031 (2)0.016 (2)0.012 (2)0.012 (2)
C650.030 (2)0.028 (2)0.031 (2)0.0089 (18)0.0063 (19)0.012 (2)
C660.051 (3)0.051 (3)0.039 (3)0.022 (2)0.023 (2)0.014 (3)
C670.045 (3)0.053 (3)0.051 (3)0.013 (2)0.031 (2)0.024 (3)
C680.039 (3)0.037 (3)0.041 (3)0.007 (2)0.020 (2)0.015 (2)
N210.066 (3)0.083 (4)0.068 (3)0.011 (3)0.011 (3)0.036 (3)
C700.042 (3)0.050 (3)0.065 (4)0.000 (3)0.014 (3)0.030 (3)
N200.083 (4)0.079 (4)0.135 (5)0.030 (3)0.064 (4)0.050 (4)
N190.100 (5)0.093 (4)0.077 (4)0.000 (4)0.052 (4)0.011 (3)
C690.049 (3)0.068 (4)0.098 (5)0.004 (3)0.023 (3)0.039 (4)
C740.106 (6)0.053 (4)0.079 (4)0.007 (4)0.065 (5)0.006 (3)
C750.132 (6)0.056 (4)0.161 (7)0.021 (4)0.109 (6)0.032 (4)
C780.165 (7)0.057 (4)0.101 (5)0.020 (4)0.084 (5)0.011 (4)
C770.053 (3)0.069 (4)0.034 (3)0.014 (3)0.013 (2)0.005 (3)
O10.305 (13)0.339 (13)0.093 (5)0.207 (11)0.040 (7)0.076 (9)
Geometric parameters (Å, º) top
Cr1—N41.969 (3)C27—H270.9500
Cr1—N31.975 (3)C28—C301.398 (5)
Cr1—N21.978 (4)C28—C291.407 (5)
Cr1—N11.986 (4)C30—C311.363 (6)
Cr1—N102.064 (3)C30—H300.9500
Cr1—N92.066 (3)C31—C321.393 (5)
Cr2—N71.963 (3)C31—H310.9500
Cr2—N51.977 (4)C32—H320.9500
Cr2—N81.984 (3)C33—C341.392 (6)
Cr2—N61.999 (3)C33—H330.9500
Cr2—N122.071 (3)C34—C351.361 (6)
Cr2—N112.078 (3)C34—H340.9500
Fe1—N161.959 (3)C35—C361.402 (6)
Fe1—N151.972 (3)C35—H350.9500
Fe1—N131.976 (3)C36—C371.399 (5)
Fe1—N181.977 (3)C36—C381.423 (6)
Fe1—N171.978 (3)C37—C411.425 (5)
Fe1—N141.978 (3)C38—C391.342 (6)
S1—C11.615 (5)C38—H380.9500
S2—C21.616 (4)C39—C401.424 (6)
S3—C31.608 (4)C39—H390.9500
S4—C41.606 (4)C40—C411.395 (5)
S5—C51.619 (5)C40—C421.410 (6)
S6—C61.623 (4)C42—C431.357 (6)
S7—C71.612 (4)C42—H420.9500
S8—C81.616 (4)C43—C441.382 (5)
N1—C11.168 (5)C43—H430.9500
N2—C21.153 (5)C44—H440.9500
N3—C31.163 (5)C45—C461.397 (6)
N4—C41.166 (5)C45—H450.9500
N5—C51.163 (5)C46—C471.366 (7)
N6—C61.166 (5)C46—H460.9500
N7—C71.160 (5)C47—C481.396 (7)
N8—C81.166 (5)C47—H470.9500
N9—C91.318 (5)C48—C491.398 (6)
N9—C131.359 (5)C48—C501.437 (7)
N10—C201.324 (5)C49—C531.412 (6)
N10—C171.364 (5)C50—C511.330 (7)
N11—C211.324 (5)C50—H500.9500
N11—C251.368 (5)C51—C521.432 (7)
N12—C321.324 (5)C51—H510.9500
N12—C291.364 (5)C52—C541.397 (7)
N13—C331.335 (5)C52—C531.403 (6)
N13—C371.366 (5)C54—C551.362 (6)
N14—C441.334 (5)C54—H540.9500
N14—C411.361 (5)C55—C561.394 (6)
N15—C451.327 (5)C55—H550.9500
N15—C491.370 (5)C56—H560.9500
N16—C561.327 (5)C57—C581.403 (6)
N16—C531.370 (5)C57—H570.9500
N17—C571.334 (5)C58—C591.354 (6)
N17—C611.363 (5)C58—H580.9500
N18—C681.335 (5)C59—C601.412 (6)
N18—C651.368 (5)C59—H590.9500
C9—C101.393 (6)C60—C611.396 (5)
C9—H90.9500C60—C621.421 (6)
C10—C111.373 (6)C61—C651.415 (5)
C10—H100.9500C62—C631.348 (6)
C11—C121.395 (6)C62—H620.9500
C11—H110.9500C63—C641.435 (6)
C12—C131.403 (5)C63—H630.9500
C12—C141.427 (6)C64—C651.390 (5)
C13—C171.422 (5)C64—C661.396 (6)
C14—C151.347 (6)C66—C671.358 (6)
C14—H140.9500C66—H660.9500
C15—C161.442 (5)C67—C681.393 (6)
C15—H150.9500C67—H670.9500
C16—C181.386 (5)C68—H680.9500
C16—C171.399 (5)N21—C771.114 (6)
C18—C191.364 (6)C70—N201.123 (6)
C18—H180.9500C70—C691.440 (7)
C19—C201.400 (5)N19—C741.125 (8)
C19—H190.9500C69—H69A0.9800
C20—H200.9500C69—H69B0.9800
C21—C221.398 (6)C69—H69C0.9800
C21—H210.9500C74—C751.453 (9)
C22—C231.367 (6)C75—H75A0.9800
C22—H220.9500C75—H75B0.9800
C23—C241.392 (6)C75—H75C0.9800
C23—H230.9500C78—C771.449 (7)
C24—C251.403 (5)C78—H78A0.9800
C24—C261.433 (6)C78—H78B0.9800
C25—C291.414 (5)C78—H78C0.9800
C26—C271.348 (6)O1—H1O0.84 (2)
C26—H260.9500O1—H2O0.85 (2)
C27—C281.439 (6)
N4—Cr1—N393.08 (13)C28—C27—H27119.5
N4—Cr1—N2174.49 (14)C30—C28—C29117.6 (4)
N3—Cr1—N291.37 (14)C30—C28—C27124.1 (4)
N4—Cr1—N191.16 (14)C29—C28—C27118.3 (4)
N3—Cr1—N193.32 (14)N12—C29—C28121.9 (4)
N2—Cr1—N191.82 (14)N12—C29—C25117.9 (3)
N4—Cr1—N1087.71 (13)C28—C29—C25120.2 (4)
N3—Cr1—N10173.14 (14)C31—C30—C28119.6 (4)
N2—Cr1—N1087.50 (13)C31—C30—H30120.2
N1—Cr1—N1093.48 (14)C28—C30—H30120.2
N4—Cr1—N988.10 (13)C30—C31—C32119.7 (4)
N3—Cr1—N993.48 (13)C30—C31—H31120.2
N2—Cr1—N988.38 (13)C32—C31—H31120.2
N1—Cr1—N9173.20 (13)N12—C32—C31122.3 (4)
N10—Cr1—N979.73 (13)N12—C32—H32118.8
N7—Cr2—N589.11 (14)C31—C32—H32118.8
N7—Cr2—N889.61 (13)N13—C33—C34122.6 (4)
N5—Cr2—N894.14 (14)N13—C33—H33118.7
N7—Cr2—N6175.77 (13)C34—C33—H33118.7
N5—Cr2—N690.40 (14)C35—C34—C33119.9 (4)
N8—Cr2—N694.62 (13)C35—C34—H34120.0
N7—Cr2—N1288.04 (12)C33—C34—H34120.0
N5—Cr2—N1295.01 (13)C34—C35—C36119.9 (4)
N8—Cr2—N12170.52 (13)C34—C35—H35120.0
N6—Cr2—N1287.81 (12)C36—C35—H35120.0
N7—Cr2—N1190.64 (13)C37—C36—C35116.5 (4)
N5—Cr2—N11174.81 (13)C37—C36—C38118.2 (4)
N8—Cr2—N1191.05 (13)C35—C36—C38125.3 (4)
N6—Cr2—N1189.46 (13)N13—C37—C36124.0 (4)
N12—Cr2—N1179.80 (12)N13—C37—C41115.8 (4)
N16—Fe1—N1582.94 (14)C36—C37—C41120.2 (4)
N16—Fe1—N13173.04 (13)C39—C38—C36121.9 (4)
N15—Fe1—N1392.81 (13)C39—C38—H38119.0
N16—Fe1—N1895.12 (13)C36—C38—H38119.0
N15—Fe1—N18173.96 (13)C38—C39—C40120.7 (5)
N13—Fe1—N1889.65 (13)C38—C39—H39119.7
N16—Fe1—N1792.39 (13)C40—C39—H39119.7
N15—Fe1—N1792.11 (13)C41—C40—C42116.1 (4)
N13—Fe1—N1793.27 (13)C41—C40—C39119.1 (4)
N18—Fe1—N1782.24 (13)C42—C40—C39124.7 (4)
N16—Fe1—N1492.28 (13)N14—C41—C40124.7 (4)
N15—Fe1—N1493.11 (12)N14—C41—C37115.5 (3)
N13—Fe1—N1482.42 (13)C40—C41—C37119.8 (4)
N18—Fe1—N1492.68 (13)C43—C42—C40119.3 (4)
N17—Fe1—N14173.38 (13)C43—C42—H42120.3
C1—N1—Cr1166.9 (3)C40—C42—H42120.3
C2—N2—Cr1176.1 (3)C42—C43—C44120.5 (4)
C3—N3—Cr1170.3 (3)C42—C43—H43119.7
C4—N4—Cr1170.4 (3)C44—C43—H43119.7
C5—N5—Cr2167.4 (3)N14—C44—C43122.8 (4)
C6—N6—Cr2166.9 (3)N14—C44—H44118.6
C7—N7—Cr2169.4 (3)C43—C44—H44118.6
C8—N8—Cr2170.1 (3)N15—C45—C46122.7 (5)
C9—N9—C13118.1 (3)N15—C45—H45118.6
C9—N9—Cr1128.4 (3)C46—C45—H45118.6
C13—N9—Cr1113.5 (3)C47—C46—C45119.9 (5)
C20—N10—C17118.6 (3)C47—C46—H46120.1
C20—N10—Cr1128.2 (3)C45—C46—H46120.1
C17—N10—Cr1113.2 (2)C46—C47—C48119.5 (4)
C21—N11—C25117.5 (4)C46—C47—H47120.3
C21—N11—Cr2129.3 (3)C48—C47—H47120.3
C25—N11—Cr2113.1 (3)C47—C48—C49117.2 (5)
C32—N12—C29118.8 (3)C47—C48—C50125.3 (5)
C32—N12—Cr2128.5 (3)C49—C48—C50117.5 (5)
C29—N12—Cr2112.7 (2)N15—C49—C48123.6 (4)
C33—N13—C37117.0 (4)N15—C49—C53115.7 (4)
C33—N13—Fe1130.0 (3)C48—C49—C53120.8 (4)
C37—N13—Fe1113.0 (3)C51—C50—C48121.9 (5)
C44—N14—C41116.5 (3)C51—C50—H50119.1
C44—N14—Fe1130.2 (3)C48—C50—H50119.1
C41—N14—Fe1113.3 (2)C50—C51—C52121.6 (5)
C45—N15—C49117.1 (4)C50—C51—H51119.2
C45—N15—Fe1130.3 (3)C52—C51—H51119.2
C49—N15—Fe1112.6 (3)C54—C52—C53117.1 (4)
C56—N16—C53117.1 (4)C54—C52—C51125.2 (5)
C56—N16—Fe1129.9 (3)C53—C52—C51117.7 (5)
C53—N16—Fe1112.9 (3)N16—C53—C52123.6 (4)
C57—N17—C61117.1 (4)N16—C53—C49115.9 (4)
C57—N17—Fe1130.0 (3)C52—C53—C49120.6 (4)
C61—N17—Fe1112.7 (3)C55—C54—C52119.2 (4)
C68—N18—C65117.0 (3)C55—C54—H54120.4
C68—N18—Fe1129.8 (3)C52—C54—H54120.4
C65—N18—Fe1113.0 (2)C54—C55—C56120.4 (5)
N1—C1—S1178.2 (4)C54—C55—H55119.8
N2—C2—S2178.8 (4)C56—C55—H55119.8
N3—C3—S3179.4 (4)N16—C56—C55122.6 (4)
N4—C4—S4178.2 (4)N16—C56—H56118.7
N5—C5—S5179.2 (4)C55—C56—H56118.7
N6—C6—S6178.1 (3)N17—C57—C58122.1 (4)
N7—C7—S7179.2 (4)N17—C57—H57118.9
N8—C8—S8178.8 (4)C58—C57—H57118.9
N9—C9—C10122.6 (4)C59—C58—C57120.2 (4)
N9—C9—H9118.7C59—C58—H58119.9
C10—C9—H9118.7C57—C58—H58119.9
C11—C10—C9119.5 (4)C58—C59—C60119.9 (4)
C11—C10—H10120.2C58—C59—H59120.1
C9—C10—H10120.2C60—C59—H59120.1
C10—C11—C12119.5 (4)C61—C60—C59116.1 (4)
C10—C11—H11120.2C61—C60—C62119.2 (4)
C12—C11—H11120.2C59—C60—C62124.6 (4)
C11—C12—C13117.0 (4)N17—C61—C60124.5 (4)
C11—C12—C14124.5 (4)N17—C61—C65116.1 (4)
C13—C12—C14118.4 (4)C60—C61—C65119.4 (4)
N9—C13—C12123.2 (4)C63—C62—C60121.1 (4)
N9—C13—C17116.6 (3)C63—C62—H62119.5
C12—C13—C17120.2 (4)C60—C62—H62119.5
C15—C14—C12121.6 (4)C62—C63—C64121.0 (4)
C15—C14—H14119.2C62—C63—H63119.5
C12—C14—H14119.2C64—C63—H63119.5
C14—C15—C16121.1 (4)C65—C64—C66117.6 (4)
C14—C15—H15119.5C65—C64—C63118.1 (4)
C16—C15—H15119.5C66—C64—C63124.3 (4)
C18—C16—C17117.2 (4)N18—C65—C64123.4 (4)
C18—C16—C15124.6 (4)N18—C65—C61115.4 (3)
C17—C16—C15118.1 (4)C64—C65—C61121.2 (4)
N10—C17—C16122.6 (4)C67—C66—C64119.3 (4)
N10—C17—C13116.9 (3)C67—C66—H66120.3
C16—C17—C13120.6 (4)C64—C66—H66120.3
C19—C18—C16120.4 (4)C66—C67—C68120.1 (4)
C19—C18—H18119.8C66—C67—H67119.9
C16—C18—H18119.8C68—C67—H67119.9
C18—C19—C20119.3 (4)N18—C68—C67122.5 (4)
C18—C19—H19120.4N18—C68—H68118.7
C20—C19—H19120.4C67—C68—H68118.7
N10—C20—C19122.0 (4)N20—C70—C69179.3 (6)
N10—C20—H20119.0C70—C69—H69A109.5
C19—C20—H20119.0C70—C69—H69B109.5
N11—C21—C22123.1 (4)H69A—C69—H69B109.5
N11—C21—H21118.5C70—C69—H69C109.5
C22—C21—H21118.5H69A—C69—H69C109.5
C23—C22—C21119.4 (4)H69B—C69—H69C109.5
C23—C22—H22120.3N19—C74—C75178.8 (8)
C21—C22—H22120.3C74—C75—H75A109.5
C22—C23—C24119.5 (4)C74—C75—H75B109.5
C22—C23—H23120.3H75A—C75—H75B109.5
C24—C23—H23120.3C74—C75—H75C109.5
C23—C24—C25117.8 (4)H75A—C75—H75C109.5
C23—C24—C26124.2 (4)H75B—C75—H75C109.5
C25—C24—C26117.9 (4)C77—C78—H78A109.5
N11—C25—C24122.7 (4)C77—C78—H78B109.5
N11—C25—C29116.4 (4)H78A—C78—H78B109.5
C24—C25—C29120.9 (4)C77—C78—H78C109.5
C27—C26—C24121.7 (4)H78A—C78—H78C109.5
C27—C26—H26119.2H78B—C78—H78C109.5
C24—C26—H26119.2N21—C77—C78179.0 (7)
C26—C27—C28121.0 (4)H1O—O1—H2O105 (5)
C26—C27—H27119.5
N4—Cr1—N1—C165.0 (15)C20—N10—C17—C160.0 (5)
N3—Cr1—N1—C128.2 (15)Cr1—N10—C17—C16179.7 (3)
N2—Cr1—N1—C1119.7 (15)C20—N10—C17—C13178.1 (3)
N10—Cr1—N1—C1152.7 (15)Cr1—N10—C17—C131.6 (4)
N9—Cr1—N1—C1148.7 (13)C18—C16—C17—N100.7 (5)
N4—Cr1—N2—C230 (6)C15—C16—C17—N10179.6 (3)
N3—Cr1—N2—C2173 (5)C18—C16—C17—C13177.3 (3)
N1—Cr1—N2—C293 (5)C15—C16—C17—C131.6 (5)
N10—Cr1—N2—C20 (5)N9—C13—C17—N100.4 (5)
N9—Cr1—N2—C280 (5)C12—C13—C17—N10178.7 (3)
N4—Cr1—N3—C3104 (2)N9—C13—C17—C16178.5 (3)
N2—Cr1—N3—C379 (2)C12—C13—C17—C160.6 (5)
N1—Cr1—N3—C313 (2)C17—C16—C18—C191.4 (6)
N10—Cr1—N3—C3159.7 (17)C15—C16—C18—C19179.9 (4)
N9—Cr1—N3—C3168 (2)C16—C18—C19—C201.3 (6)
N3—Cr1—N4—C4177 (2)C17—N10—C20—C190.1 (5)
N2—Cr1—N4—C433 (3)Cr1—N10—C20—C19179.5 (3)
N1—Cr1—N4—C490 (2)C18—C19—C20—N100.5 (6)
N10—Cr1—N4—C44 (2)C25—N11—C21—C221.5 (6)
N9—Cr1—N4—C483 (2)Cr2—N11—C21—C22179.1 (3)
N7—Cr2—N5—C545.6 (16)N11—C21—C22—C230.3 (7)
N8—Cr2—N5—C543.9 (16)C21—C22—C23—C241.9 (7)
N6—Cr2—N5—C5138.6 (16)C22—C23—C24—C252.6 (6)
N12—Cr2—N5—C5133.6 (16)C22—C23—C24—C26177.0 (4)
N11—Cr2—N5—C5132.9 (16)C21—N11—C25—C240.7 (5)
N7—Cr2—N6—C661 (3)Cr2—N11—C25—C24179.9 (3)
N5—Cr2—N6—C622.6 (14)C21—N11—C25—C29177.9 (3)
N8—Cr2—N6—C6116.8 (14)Cr2—N11—C25—C291.6 (4)
N12—Cr2—N6—C672.4 (14)C23—C24—C25—N111.4 (6)
N11—Cr2—N6—C6152.2 (14)C26—C24—C25—N11178.2 (3)
N5—Cr2—N7—C79.2 (17)C23—C24—C25—C29179.9 (4)
N8—Cr2—N7—C7103.3 (17)C26—C24—C25—C290.3 (6)
N6—Cr2—N7—C774 (3)C23—C24—C26—C27178.2 (4)
N12—Cr2—N7—C785.8 (17)C25—C24—C26—C271.4 (6)
N11—Cr2—N7—C7165.6 (17)C24—C26—C27—C281.7 (6)
N7—Cr2—N8—C811 (2)C26—C27—C28—C30178.5 (4)
N5—Cr2—N8—C8100 (2)C26—C27—C28—C290.3 (6)
N6—Cr2—N8—C8169 (2)C32—N12—C29—C280.6 (5)
N12—Cr2—N8—C865 (2)Cr2—N12—C29—C28177.9 (3)
N11—Cr2—N8—C880 (2)C32—N12—C29—C25179.0 (3)
N4—Cr1—N9—C993.9 (3)Cr2—N12—C29—C250.5 (4)
N3—Cr1—N9—C90.9 (3)C30—C28—C29—N121.3 (5)
N2—Cr1—N9—C990.4 (3)C27—C28—C29—N12179.6 (3)
N1—Cr1—N9—C9177.8 (10)C30—C28—C29—C25177.0 (3)
N10—Cr1—N9—C9178.1 (4)C27—C28—C29—C251.3 (5)
N4—Cr1—N9—C1386.6 (3)N11—C25—C29—N121.4 (5)
N3—Cr1—N9—C13179.6 (3)C24—C25—C29—N12180.0 (3)
N2—Cr1—N9—C1389.2 (3)N11—C25—C29—C28177.0 (3)
N1—Cr1—N9—C132.7 (12)C24—C25—C29—C281.5 (5)
N10—Cr1—N9—C131.4 (2)C29—C28—C30—C312.1 (6)
N4—Cr1—N10—C2093.5 (3)C27—C28—C30—C31179.7 (4)
N3—Cr1—N10—C20169.8 (10)C28—C30—C31—C321.0 (6)
N2—Cr1—N10—C2089.2 (3)C29—N12—C32—C311.8 (6)
N1—Cr1—N10—C202.5 (3)Cr2—N12—C32—C31176.5 (3)
N9—Cr1—N10—C20178.0 (3)C30—C31—C32—N121.0 (6)
N4—Cr1—N10—C1786.9 (3)C37—N13—C33—C341.2 (6)
N3—Cr1—N10—C179.8 (12)Fe1—N13—C33—C34179.2 (3)
N2—Cr1—N10—C1790.4 (3)N13—C33—C34—C350.2 (7)
N1—Cr1—N10—C17177.9 (3)C33—C34—C35—C360.7 (7)
N9—Cr1—N10—C171.6 (2)C34—C35—C36—C370.5 (6)
N7—Cr2—N11—C2190.5 (3)C34—C35—C36—C38177.8 (4)
N5—Cr2—N11—C21178 (61)C33—N13—C37—C361.4 (6)
N8—Cr2—N11—C210.8 (3)Fe1—N13—C37—C36179.0 (3)
N6—Cr2—N11—C2193.8 (3)C33—N13—C37—C41178.1 (3)
N12—Cr2—N11—C21178.4 (4)Fe1—N13—C37—C411.5 (4)
N7—Cr2—N11—C2588.9 (3)C35—C36—C37—N130.6 (6)
N5—Cr2—N11—C251.7 (16)C38—C36—C37—N13179.0 (4)
N8—Cr2—N11—C25178.5 (3)C35—C36—C37—C41179.0 (4)
N6—Cr2—N11—C2586.8 (3)C38—C36—C37—C410.5 (6)
N12—Cr2—N11—C251.0 (2)C37—C36—C38—C391.0 (7)
N7—Cr2—N12—C3287.0 (3)C35—C36—C38—C39177.3 (5)
N5—Cr2—N12—C321.9 (3)C36—C38—C39—C401.2 (7)
N8—Cr2—N12—C32162.8 (7)C38—C39—C40—C410.2 (7)
N6—Cr2—N12—C3292.1 (3)C38—C39—C40—C42177.8 (5)
N11—Cr2—N12—C32178.0 (3)C44—N14—C41—C400.0 (6)
N7—Cr2—N12—C2991.3 (3)Fe1—N14—C41—C40178.7 (3)
N5—Cr2—N12—C29179.7 (3)C44—N14—C41—C37178.5 (3)
N8—Cr2—N12—C2915.6 (9)Fe1—N14—C41—C370.2 (4)
N6—Cr2—N12—C2989.5 (3)C42—C40—C41—N142.0 (6)
N11—Cr2—N12—C290.3 (2)C39—C40—C41—N14179.8 (4)
N16—Fe1—N13—C33141.1 (10)C42—C40—C41—C37176.5 (4)
N15—Fe1—N13—C3388.9 (4)C39—C40—C41—C371.7 (6)
N18—Fe1—N13—C3385.6 (4)N13—C37—C41—N140.9 (5)
N17—Fe1—N13—C333.4 (4)C36—C37—C41—N14179.5 (4)
N14—Fe1—N13—C33178.3 (4)N13—C37—C41—C40177.7 (4)
N16—Fe1—N13—C3739.3 (12)C36—C37—C41—C401.9 (6)
N15—Fe1—N13—C3791.5 (3)C41—C40—C42—C431.6 (6)
N18—Fe1—N13—C3794.0 (3)C39—C40—C42—C43179.7 (4)
N17—Fe1—N13—C37176.2 (3)C40—C42—C43—C440.5 (7)
N14—Fe1—N13—C371.2 (3)C41—N14—C44—C432.4 (6)
N16—Fe1—N14—C446.8 (4)Fe1—N14—C44—C43176.0 (3)
N15—Fe1—N14—C4489.9 (4)C42—C43—C44—N142.7 (7)
N13—Fe1—N14—C44177.7 (4)C49—N15—C45—C461.6 (5)
N18—Fe1—N14—C4488.4 (3)Fe1—N15—C45—C46179.3 (3)
N17—Fe1—N14—C44128.1 (11)N15—C45—C46—C471.9 (6)
N16—Fe1—N14—C41174.7 (3)C45—C46—C47—C481.3 (7)
N15—Fe1—N14—C4191.7 (3)C46—C47—C48—C490.5 (6)
N13—Fe1—N14—C410.7 (3)C46—C47—C48—C50179.8 (4)
N18—Fe1—N14—C4190.0 (3)C45—N15—C49—C480.8 (5)
N17—Fe1—N14—C4150.4 (13)Fe1—N15—C49—C48178.9 (3)
N16—Fe1—N15—C45177.4 (3)C45—N15—C49—C53178.8 (3)
N13—Fe1—N15—C458.1 (3)Fe1—N15—C49—C530.8 (4)
N18—Fe1—N15—C45105.9 (13)C47—C48—C49—N150.2 (6)
N17—Fe1—N15—C4585.3 (3)C50—C48—C49—N15180.0 (4)
N14—Fe1—N15—C4590.6 (3)C47—C48—C49—C53179.4 (4)
N16—Fe1—N15—C490.3 (2)C50—C48—C49—C530.4 (6)
N13—Fe1—N15—C49174.2 (3)C47—C48—C50—C51179.6 (5)
N18—Fe1—N15—C4971.9 (14)C49—C48—C50—C510.7 (7)
N17—Fe1—N15—C4992.4 (3)C48—C50—C51—C520.6 (8)
N14—Fe1—N15—C4991.6 (3)C50—C51—C52—C54178.4 (5)
N15—Fe1—N16—C56178.0 (3)C50—C51—C52—C530.6 (7)
N13—Fe1—N16—C56125.3 (10)C56—N16—C53—C521.5 (5)
N18—Fe1—N16—C567.8 (3)Fe1—N16—C53—C52178.6 (3)
N17—Fe1—N16—C5690.2 (3)C56—N16—C53—C49179.2 (3)
N14—Fe1—N16—C5685.1 (3)Fe1—N16—C53—C492.1 (4)
N15—Fe1—N16—C531.3 (2)C54—C52—C53—N163.4 (6)
N13—Fe1—N16—C5351.4 (11)C51—C52—C53—N16177.5 (4)
N18—Fe1—N16—C53175.6 (2)C54—C52—C53—C49177.4 (4)
N17—Fe1—N16—C5393.2 (3)C51—C52—C53—C491.7 (6)
N14—Fe1—N16—C5391.5 (3)N15—C49—C53—N161.9 (5)
N16—Fe1—N17—C5783.2 (4)C48—C49—C53—N16177.7 (3)
N15—Fe1—N17—C570.2 (4)N15—C49—C53—C52178.8 (3)
N13—Fe1—N17—C5792.7 (4)C48—C49—C53—C521.6 (6)
N18—Fe1—N17—C57178.1 (4)C53—C52—C54—C552.5 (6)
N14—Fe1—N17—C57141.9 (11)C51—C52—C54—C55178.4 (4)
N16—Fe1—N17—C61101.1 (3)C52—C54—C55—C560.1 (6)
N15—Fe1—N17—C61175.9 (3)C53—N16—C56—C551.1 (6)
N13—Fe1—N17—C6183.0 (3)Fe1—N16—C56—C55175.4 (3)
N18—Fe1—N17—C616.2 (3)C54—C55—C56—N161.8 (6)
N14—Fe1—N17—C6133.8 (13)C61—N17—C57—C580.5 (6)
N16—Fe1—N18—C6886.4 (3)Fe1—N17—C57—C58175.1 (3)
N15—Fe1—N18—C68157.4 (12)N17—C57—C58—C590.1 (7)
N13—Fe1—N18—C6888.5 (3)C57—C58—C59—C600.4 (7)
N17—Fe1—N18—C68178.1 (4)C58—C59—C60—C610.5 (7)
N14—Fe1—N18—C686.1 (3)C58—C59—C60—C62178.5 (5)
N16—Fe1—N18—C6598.4 (3)C57—N17—C61—C600.4 (6)
N15—Fe1—N18—C6527.5 (14)Fe1—N17—C61—C60175.9 (3)
N13—Fe1—N18—C6586.6 (3)C57—N17—C61—C65179.0 (4)
N17—Fe1—N18—C656.7 (2)Fe1—N17—C61—C654.8 (4)
N14—Fe1—N18—C65169.0 (3)C59—C60—C61—N170.1 (6)
Cr1—N1—C1—S16 (14)C62—C60—C61—N17178.2 (4)
Cr1—N2—C2—S2108 (22)C59—C60—C61—C65179.4 (4)
Cr1—N3—C3—S312 (36)C62—C60—C61—C652.4 (6)
Cr1—N4—C4—S4164 (11)C61—C60—C62—C631.8 (6)
Cr2—N5—C5—S5173 (100)C59—C60—C62—C63179.8 (4)
Cr2—N6—C6—S6102 (11)C60—C62—C63—C640.5 (7)
Cr2—N7—C7—S7167 (100)C62—C63—C64—C652.0 (6)
Cr2—N8—C8—S8146 (16)C62—C63—C64—C66177.3 (4)
C13—N9—C9—C100.0 (6)C68—N18—C65—C641.3 (5)
Cr1—N9—C9—C10179.5 (3)Fe1—N18—C65—C64174.5 (3)
N9—C9—C10—C110.6 (7)C68—N18—C65—C61178.1 (3)
C9—C10—C11—C120.8 (6)Fe1—N18—C65—C616.1 (4)
C10—C11—C12—C130.4 (6)C66—C64—C65—N181.3 (6)
C10—C11—C12—C14179.0 (4)C63—C64—C65—N18179.3 (3)
C9—N9—C13—C120.5 (5)C66—C64—C65—C61178.0 (4)
Cr1—N9—C13—C12179.9 (3)C63—C64—C65—C611.3 (6)
C9—N9—C13—C17178.6 (3)N17—C61—C65—N180.9 (5)
Cr1—N9—C13—C171.0 (4)C60—C61—C65—N18178.5 (3)
C11—C12—C13—N90.3 (6)N17—C61—C65—C64179.7 (4)
C14—C12—C13—N9179.7 (3)C60—C61—C65—C640.9 (6)
C11—C12—C13—C17178.7 (3)C65—C64—C66—C670.6 (6)
C14—C12—C13—C170.7 (5)C63—C64—C66—C67179.9 (4)
C11—C12—C14—C15178.5 (4)C64—C66—C67—C680.1 (7)
C13—C12—C14—C150.9 (6)C65—N18—C68—C670.5 (6)
C12—C14—C15—C160.1 (6)Fe1—N18—C68—C67174.5 (3)
C14—C15—C16—C18177.4 (4)C66—C67—C68—N180.2 (7)
C14—C15—C16—C171.4 (6)

Experimental details

Crystal data
Chemical formula[Fe(C12H8N2)3][Cr(NCS)4(C12H8N2)]2·3C2H3N·H2O
Mr1666.69
Crystal system, space groupTriclinic, P1
Temperature (K)173
a, b, c (Å)12.641 (2), 16.681 (3), 20.692 (4)
α, β, γ (°)111.514 (5), 107.291 (6), 92.231 (5)
V3)3821.5 (13)
Z2
Radiation typeMo Kα
µ (mm1)0.75
Crystal size (mm)0.23 × 0.22 × 0.12
Data collection
DiffractometerBruker APEXII CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2005)
Tmin, Tmax0.847, 0.916
No. of measured, independent and
observed [I > 2σ(I)] reflections
48046, 15519, 8993
Rint0.078
(sin θ/λ)max1)0.626
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.051, 0.135, 0.99
No. of reflections15519
No. of parameters974
No. of restraints3
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.43, 0.44

Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXS97 (Sheldrick, 2008), PLATON (Spek, 2009), publCIF (Westrip, 2010).

 

References

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Volume 68| Part 5| May 2012| Pages m531-m532
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