Di-μ-aqua-bis­[diaqua­bis(thio­cyanato-κN)iron(II)] 4-(4-chloro­phen­yl)-1,2,4-triazole hexa­solvate

Li, X.; Zuo, Y.

doi:10.1107/S1600536808019326

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 64| Part 8| August 2008| Pages m996-m997

doi:10.1107/S1600536808019326

Open

access

Di-μ-aqua-bis[diaquabis(thiocyanato-κN)iron(II)] 4-(4-chlorophenyl)-1,2,4-triazole hexasolvate

Xiuhua Li ^a ^* and Ya Zuo ^b

^aCollege of Chemistry, Chifeng University, Inner Mongolia 024000, People's Republic of China, and ^bCollege of Science, Inner Mongolia Agricultural University, Inner Mongolia 010018, People's Republic of China
^*Correspondence e-mail: yazoe@mail.nankai.edu.cn

(Received 6 June 2008; accepted 25 June 2008; online 5 July 2008)

The title complex, [Fe₂(NCS)₄(H₂O)₆]·6C₈H₆ClN₃, comprises two distorted octahedral iron(II) centers straddling a crystallographic inversion center and bridged by two aqua O atoms to form a quadrilateral core. The aqua O atom of the core is involved in hydrogen bonds with the triazole N atoms of the solvent molecules, generating one-dimensional ladder motifs, and three intermolecular C—H⋯S hydrogen bonds, forming a three-dimensional hydrogen-bonding network.

Related literature

For related literature, see: Hsu et al. (1999 ); MacMurdo et al. (2000 ); Nordlund & Eklund (1993 ); Sazinsky et al. (2004 ); Stubbe & Van der Donk (1998 ); Yoon et al. (2004 ); Zheng et al. (1999 ).

Experimental

Crystal data

[Fe₂(NCS)₄(H₂O)₆]·6C₈H₆ClN₃
M_r = 1529.76
Triclinic, $[P \overline 1]$
a = 7.944 (3) Å
b = 11.085 (5) Å
c = 19.912 (10) Å
α = 105.613 (10)°
β = 97.750 (10)°
γ = 97.932 (7)°
V = 1645.1 (12) Å³
Z = 1
Mo Kα radiation
μ = 0.88 mm⁻¹
T = 298 (2) K
0.25 × 0.21 × 0.17 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.810, T_max = 0.865
8642 measured reflections
5705 independent reflections
2903 reflections with I > 2σ(I)
R_int = 0.032

Refinement

R[F² > 2σ(F²)] = 0.044
wR(F²) = 0.076
S = 0.77
5705 reflections
439 parameters
9 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.25 e Å⁻³
Δρ_min = −0.24 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

Fe1—N1	2.086 (3)
Fe1—O2	2.100 (2)
Fe1—O3	2.102 (3)
Fe1—N2	2.107 (3)
Fe1—O1ⁱ	2.264 (3)
Fe1—O1	2.281 (2)

N1—Fe1—O2	90.22 (11)
N1—Fe1—O3	89.68 (12)
O2—Fe1—O3	101.01 (10)
N1—Fe1—N2	178.33 (12)
O2—Fe1—O1ⁱ	89.04 (10)
O3—Fe1—O1ⁱ	169.95 (9)
N2—Fe1—O1ⁱ	91.32 (11)
O1ⁱ—Fe1—O1	78.36 (9)
Fe1ⁱ—O1—Fe1	101.64 (9)
Symmetry code: (i) -x+1, -y, -z+1.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1⋯N10ⁱⁱ	0.87 (3)	1.97 (3)	2.827 (4)	170 (3)
O1—H2⋯N9	0.88 (3)	1.94 (3)	2.819 (4)	173 (3)
O2—H3⋯N7ⁱⁱⁱ	0.88 (3)	1.98 (3)	2.866 (5)	178 (3)
O2—H4⋯N4^iv	0.88 (2)	1.97 (3)	2.853 (4)	175 (3)
O3—H5⋯N6	0.88 (3)	1.92 (3)	2.802 (4)	174 (3)
O3—H6⋯N3^v	0.88 (2)	1.93 (2)	2.803 (4)	172 (3)
C3—H7⋯S2^vi	0.93	2.72	3.624 (5)	165
C22—H21⋯S2ⁱⁱ	0.93	2.87	3.736 (5)	156
C11—H13⋯S1^vii	0.93	2.87	3.783 (5)	167
Symmetry codes: (ii) -x, -y, -z+1; (iii) x+1, y, z; (iv) x, y-1, z; (v) x-1, y-1, z; (vi) x, y+1, z; (vii) x-1, y, z.

Data collection: SMART (Bruker, 1998 ); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL and PLATON (Spek, 2003 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808019326/si2093sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808019326/si2093Isup2.hkl

checkCIF report

Comment top

The diiron unit, with a carboxylate-rich coordination environment, continue to attract considerable attention due to the enzyme catalysis activity, which occur in related multicompent dioxygen dependent enzymes, including toluene monooxygenase (Sazinsky et al., 2004), the R2 subunit of ribonucleotide reductase (Stubbe & Van der Donk, 1998; Nordlund & Eklund, 1993). With the development of compounds that contained the diiron center, the structure of a series of Fe2(II,II) (MacMurdo et al., 2000), Fe2(III,III) (Zheng et al., 1999) and Fe2(III,IV) (Hsu et al., 1999) complexes with a central 2Fe2O quadrilateral have been currently obtained. Compared with the chelating to the iron atoms with the carboxylic oxygen atoms, it is rarely reported that the quadrilateral center includes both aqueous oxygen atoms. In order to explore the furthur details of the coordinated environment of the diiron system, the title complex was synthesized. As shown in Fig. 1, the complex structure comprises two distorted octahedron iron(II) centers straddling a crystallographic inversion center bridged by two aqueous oxygen atoms to form a quadrilateral core. The separation between the iron atoms is 3.523 (2) Å, which is remarkably different from that 3.0430 (7)Å reported previously, owing to the absence of two carboxylate ligands (Yoon et al., 2004). Moreover, the distance of Fe—Fe is comparatively distinguished from that diiron containing the other higher valence of iron (MacMurdo et al., 2000; Zheng et al., 1999; Hsu et al., 1999). The bond lengths of Fe—O1 and Fe—O1a are 2.264 (3) and 2.281 (2) Å, and the angles of O1—Fe—O1a and Fe1a—O1—Fe are 78.36 (9)° and 101.64 (9)°. Each Fe(II) center resides in a six-coordinated octahedron of N₂O₄. On the equator plane, the center is bridged by two symmetrical O1 (water) to form the quadrilateral core with the mean distance of 2.272 (2) Å, and is connected with O2 and O3 offered by different waters as the terminal ligands with the bond lengths 2.102 (3)Å and 2.100 (2) Å. The axial positions are occupied by two N atoms from the NCS^- anions with the distances 2.086 (3)Å and 2.107 (3)Å to the iron core. Selected bonds and angles are listed in Table 1. As indicated in Fig.2, the classic intermolecular O—H···N H-bonds are formed between the triazol nitrogen atom supplied by the uncoordinated organic ligand 1,2,4-triazol-chloro-benzene and aquous oxygen atoms supplied by the bridging and terminal water ligands to generate a one-dimension ladder structure with the N···O separation ranged from 2.803 (2)Å to 2.866 (4) Å. Moreover, there are three weak intermolecular hydrogen bonding contacts C—H···S that form a three-dimensional network with the C···S distances between 3.624 (5) Å and 3.783 (5) Å. The details of the hydrogen bonds are shown in Table 2.

Related literature top

For related literature, see: Hsu et al. (1999); MacMurdo et al. (2000); Nordlund & Eklund (1993); Sazinsky et al. (2004); Stubbe & Van der Donk (1998); Yoon et al. (2004); Zheng et al. (1999).

Experimental top

The compound was synthesized under hydrothermal conditions. A mixture of L (L=1,2,4-triazol-chloro-benzene) (0.3 mmol, 0.0538 g), FeSO₄˙7H₂O (0.1 mmol, 0.028 g), KSCN (0.2 mmol, 0.019 g) and water (10 mL) was placed in a 25 mL acid digestion bomb and heated at 433 K for two days, then equably cooled to room temperature for three days. After washed by 5 ml water for twice, green block crystals of the compound were obtained.

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2003).

Figures top

	Fig. 1. The structure of the title complex, showing 30% probability displacement ellipsoids and the atom-numbering schemes. H atoms have been omitted for clarity. Atoms of the inversion-related half-complex are indicated with A, symmetry code: (-x + 1, -y, -z + 1).
	Fig. 2. The three-dimensional structure of the title complex, the chains were drawn in different colors. Dashed lines indicate hydrogen bonds.

Di-µ-aqua-bis[diaquabis(thiocyanato-κN)iron(II)] 4-(4-chlorophenyl)-1,2,4-triazole hexasolvate top

Crystal data top

[Fe₂(NCS)₄(H₂O)₆]·6C₈H₆ClN₃	Z = 1
M_r = 1529.76	F(000) = 780
Triclinic, P1	D_x = 1.544 Mg m⁻³
a = 7.944 (3) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.085 (5) Å	Cell parameters from 1471 reflections
c = 19.912 (10) Å	θ = 2.5–22.0°
α = 105.613 (10)°	µ = 0.88 mm⁻¹
β = 97.75 (1)°	T = 298 K
γ = 97.932 (7)°	Block, green
V = 1645.1 (12) Å³	0.25 × 0.21 × 0.17 mm

Data collection top

Bruker SMART CCD area-detector diffractometer	5705 independent reflections
Radiation source: fine-focus sealed tube	2903 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.032
ϕ and ω scans	θ_max = 25.0°, θ_min = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −9→9
T_min = 0.811, T_max = 0.865	k = −11→13
8642 measured reflections	l = −21→23

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.044	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.076	H atoms treated by a mixture of independent and constrained refinement
S = 0.77	w = 1/[σ²(F_o²) + (0.0191P)²] where P = (F_o² + 2F_c²)/3
5705 reflections	(Δ/σ)_max = 0.002
439 parameters	Δρ_max = 0.25 e Å⁻³
9 restraints	Δρ_min = −0.24 e Å⁻³

Crystal data top

[Fe₂(NCS)₄(H₂O)₆]·6C₈H₆ClN₃	γ = 97.932 (7)°
M_r = 1529.76	V = 1645.1 (12) Å³
Triclinic, P1	Z = 1
a = 7.944 (3) Å	Mo Kα radiation
b = 11.085 (5) Å	µ = 0.88 mm⁻¹
c = 19.912 (10) Å	T = 298 K
α = 105.613 (10)°	0.25 × 0.21 × 0.17 mm
β = 97.75 (1)°

Data collection top

Bruker SMART CCD area-detector diffractometer	5705 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	2903 reflections with I > 2σ(I)
T_min = 0.811, T_max = 0.865	R_int = 0.032
8642 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.044	9 restraints
wR(F²) = 0.076	H atoms treated by a mixture of independent and constrained refinement
S = 0.77	Δρ_max = 0.25 e Å⁻³
5705 reflections	Δρ_min = −0.24 e Å⁻³
439 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

	x	y	z	U_iso*/U_eq
Fe1	0.53640 (6)	0.12392 (5)	0.46090 (2)	0.04255 (16)
Cl1	0.81665 (15)	0.70325 (12)	−0.09593 (6)	0.0942 (4)
Cl2	0.41822 (16)	0.88209 (11)	0.91545 (5)	0.0932 (4)
Cl3	0.28229 (14)	0.59403 (11)	1.00137 (5)	0.0879 (4)
N1	0.5944 (4)	0.2571 (3)	0.56111 (15)	0.0518 (9)
N2	0.4754 (3)	−0.0065 (3)	0.35844 (15)	0.0493 (8)
N3	1.0886 (4)	1.1192 (3)	0.31387 (16)	0.0633 (10)
N4	0.9153 (4)	1.0935 (3)	0.31608 (16)	0.0545 (9)
N5	0.9562 (4)	0.9986 (3)	0.20814 (15)	0.0469 (8)
N6	0.2192 (4)	0.4095 (3)	0.51909 (16)	0.0575 (9)
N7	0.0498 (4)	0.3852 (3)	0.53051 (17)	0.0575 (9)
N8	0.2018 (4)	0.5377 (3)	0.62253 (16)	0.0447 (8)
N9	0.1490 (4)	0.1463 (3)	0.59896 (14)	0.0468 (8)
N10	−0.0244 (4)	0.1290 (3)	0.60322 (15)	0.0461 (8)
N11	0.1199 (3)	0.2618 (3)	0.70379 (14)	0.0395 (7)
O1	0.3213 (3)	0.0112 (2)	0.49662 (13)	0.0402 (6)
O2	0.7680 (3)	0.2021 (3)	0.43624 (14)	0.0524 (7)
O3	0.3662 (3)	0.2333 (3)	0.42643 (14)	0.0517 (7)
S1	0.67311 (13)	0.44880 (10)	0.69114 (5)	0.0643 (3)
S2	0.40098 (12)	−0.15078 (10)	0.21581 (5)	0.0616 (3)
C1	0.6275 (4)	0.3375 (3)	0.61526 (19)	0.0414 (9)
C2	0.4443 (4)	−0.0668 (3)	0.29919 (19)	0.0432 (10)
C3	0.8410 (5)	1.0220 (4)	0.2526 (2)	0.0539 (11)
H7	0.7229	0.9906	0.2394	0.065*
C4	1.1071 (5)	1.0625 (4)	0.2506 (2)	0.0658 (13)
H8	1.2132	1.0651	0.2357	0.079*
C5	0.9232 (5)	0.9260 (4)	0.13488 (19)	0.0478 (10)
C6	1.0521 (5)	0.9321 (4)	0.0947 (2)	0.0678 (13)
H9	1.1598	0.9828	0.1154	0.081*
C7	1.0201 (5)	0.8626 (4)	0.0238 (2)	0.0769 (14)
H10	1.1065	0.8654	−0.0032	0.092*
C8	0.8611 (5)	0.7902 (4)	−0.00595 (19)	0.0603 (11)
C9	0.7322 (5)	0.7823 (4)	0.0331 (2)	0.0647 (12)
H11	0.6246	0.7318	0.0120	0.078*
C10	0.7645 (5)	0.8500 (4)	0.1036 (2)	0.0633 (12)
H12	0.6784	0.8446	0.1305	0.076*
C11	0.0450 (5)	0.4635 (4)	0.5915 (2)	0.0558 (11)
H13	−0.0540	0.4683	0.6115	0.067*
C12	0.3038 (5)	0.5010 (4)	0.5745 (2)	0.0594 (11)
H14	0.4198	0.5364	0.5802	0.071*
C13	0.2501 (5)	0.6260 (3)	0.69190 (19)	0.0439 (9)
C14	0.1375 (5)	0.6350 (4)	0.7392 (2)	0.0592 (11)
H15	0.0265	0.5867	0.7250	0.071*
C15	0.1885 (5)	0.7152 (4)	0.8074 (2)	0.0665 (12)
H16	0.1112	0.7220	0.8389	0.080*
C16	0.3512 (6)	0.7843 (4)	0.82879 (19)	0.0579 (11)
C17	0.4632 (5)	0.7791 (4)	0.7819 (2)	0.0668 (13)
H17	0.5730	0.8292	0.7963	0.080*
C18	0.4138 (5)	0.7001 (4)	0.7134 (2)	0.0657 (12)
H18	0.4902	0.6966	0.6817	0.079*
C19	−0.0374 (4)	0.1979 (3)	0.66556 (19)	0.0474 (10)
H19	−0.1410	0.2029	0.6821	0.057*
C20	0.2307 (5)	0.2255 (3)	0.65901 (19)	0.0497 (10)
H20	0.3497	0.2536	0.6699	0.060*
C21	0.1591 (4)	0.3441 (3)	0.77494 (18)	0.0412 (9)
C22	0.0297 (4)	0.3605 (3)	0.81508 (19)	0.0527 (11)
H21	−0.0833	0.3191	0.7954	0.063*
C23	0.0681 (5)	0.4380 (4)	0.8839 (2)	0.0591 (11)
H22	−0.0194	0.4500	0.9104	0.071*
C24	0.2350 (5)	0.4975 (4)	0.91359 (19)	0.0560 (11)
C25	0.3640 (5)	0.4839 (4)	0.8742 (2)	0.0591 (11)
H23	0.4763	0.5268	0.8941	0.071*
C26	0.3268 (4)	0.4065 (3)	0.80535 (19)	0.0524 (10)
H24	0.4147	0.3961	0.7790	0.063*
H1	0.237 (3)	−0.039 (3)	0.4646 (12)	0.094 (15)*
H2	0.276 (4)	0.058 (3)	0.5303 (14)	0.108 (18)*
H3	0.854 (3)	0.260 (3)	0.4649 (14)	0.108 (18)*
H4	0.809 (4)	0.170 (3)	0.3975 (10)	0.078 (15)*
H5	0.323 (4)	0.287 (3)	0.4580 (14)	0.100 (17)*
H6	0.279 (3)	0.192 (3)	0.3924 (12)	0.085 (15)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.0324 (3)	0.0523 (3)	0.0402 (3)	0.0071 (3)	0.0074 (2)	0.0088 (3)
Cl1	0.0811 (9)	0.1224 (11)	0.0619 (7)	0.0147 (8)	0.0189 (6)	−0.0027 (7)
Cl2	0.1116 (11)	0.0920 (9)	0.0594 (7)	0.0173 (8)	0.0104 (7)	−0.0025 (6)
Cl3	0.0801 (8)	0.1053 (10)	0.0563 (7)	−0.0014 (7)	0.0202 (6)	−0.0076 (7)
N1	0.043 (2)	0.057 (2)	0.050 (2)	0.0085 (17)	0.0069 (16)	0.0060 (17)
N2	0.0364 (19)	0.060 (2)	0.050 (2)	0.0120 (16)	0.0093 (16)	0.0124 (18)
N3	0.046 (2)	0.089 (3)	0.051 (2)	0.0173 (19)	0.0071 (18)	0.012 (2)
N4	0.040 (2)	0.072 (2)	0.052 (2)	0.0103 (18)	0.0118 (17)	0.0165 (18)
N5	0.0368 (19)	0.060 (2)	0.048 (2)	0.0127 (17)	0.0119 (17)	0.0190 (17)
N6	0.050 (2)	0.057 (2)	0.059 (2)	0.0136 (18)	0.0077 (18)	0.0059 (18)
N7	0.047 (2)	0.057 (2)	0.062 (2)	0.0009 (18)	0.0069 (18)	0.0117 (19)
N8	0.0355 (19)	0.046 (2)	0.051 (2)	0.0050 (16)	0.0086 (16)	0.0118 (16)
N9	0.0387 (19)	0.052 (2)	0.046 (2)	0.0069 (16)	0.0086 (16)	0.0082 (17)
N10	0.0346 (19)	0.054 (2)	0.0464 (19)	0.0113 (16)	0.0056 (15)	0.0086 (17)
N11	0.0306 (18)	0.0447 (19)	0.0417 (18)	0.0053 (15)	0.0082 (15)	0.0103 (15)
O1	0.0296 (14)	0.0511 (17)	0.0322 (14)	0.0038 (13)	0.0064 (12)	0.0007 (12)
O2	0.0385 (16)	0.0649 (19)	0.0454 (17)	−0.0036 (15)	0.0167 (14)	0.0044 (15)
O3	0.0391 (16)	0.0647 (19)	0.0468 (17)	0.0134 (15)	0.0049 (15)	0.0081 (15)
S1	0.0502 (7)	0.0720 (8)	0.0539 (6)	0.0008 (6)	0.0134 (5)	−0.0062 (6)
S2	0.0481 (7)	0.0740 (8)	0.0474 (6)	−0.0018 (6)	0.0103 (5)	−0.0020 (6)
C1	0.024 (2)	0.050 (3)	0.052 (2)	0.0080 (18)	0.0129 (18)	0.014 (2)
C2	0.026 (2)	0.048 (3)	0.051 (2)	0.0037 (18)	0.0081 (19)	0.009 (2)
C3	0.037 (2)	0.066 (3)	0.060 (3)	0.005 (2)	0.014 (2)	0.022 (2)
C4	0.036 (3)	0.095 (4)	0.060 (3)	0.004 (2)	0.005 (2)	0.019 (3)
C5	0.042 (2)	0.060 (3)	0.046 (2)	0.014 (2)	0.011 (2)	0.019 (2)
C6	0.049 (3)	0.092 (3)	0.055 (3)	−0.002 (2)	0.013 (2)	0.015 (3)
C7	0.055 (3)	0.116 (4)	0.056 (3)	0.007 (3)	0.020 (2)	0.017 (3)
C8	0.060 (3)	0.068 (3)	0.053 (3)	0.016 (2)	0.016 (2)	0.013 (2)
C9	0.048 (3)	0.075 (3)	0.062 (3)	−0.002 (2)	0.014 (2)	0.008 (2)
C10	0.046 (3)	0.077 (3)	0.060 (3)	0.002 (2)	0.016 (2)	0.012 (2)
C11	0.038 (3)	0.060 (3)	0.065 (3)	0.001 (2)	0.013 (2)	0.014 (2)
C12	0.043 (2)	0.066 (3)	0.064 (3)	0.012 (2)	0.015 (2)	0.006 (2)
C13	0.042 (2)	0.046 (2)	0.047 (2)	0.010 (2)	0.011 (2)	0.018 (2)
C14	0.048 (3)	0.062 (3)	0.070 (3)	0.008 (2)	0.019 (2)	0.021 (2)
C15	0.070 (3)	0.072 (3)	0.057 (3)	0.013 (3)	0.024 (2)	0.012 (2)
C16	0.070 (3)	0.054 (3)	0.045 (3)	0.011 (2)	0.008 (2)	0.009 (2)
C17	0.059 (3)	0.069 (3)	0.057 (3)	−0.008 (2)	0.009 (2)	0.002 (2)
C18	0.056 (3)	0.077 (3)	0.060 (3)	−0.002 (2)	0.022 (2)	0.015 (2)
C19	0.027 (2)	0.062 (3)	0.052 (2)	0.004 (2)	0.0068 (19)	0.016 (2)
C20	0.034 (2)	0.060 (3)	0.055 (3)	0.010 (2)	0.018 (2)	0.010 (2)
C21	0.034 (2)	0.046 (2)	0.045 (2)	0.0076 (18)	0.0099 (18)	0.0128 (19)
C22	0.035 (2)	0.066 (3)	0.050 (3)	0.002 (2)	0.011 (2)	0.008 (2)
C23	0.047 (3)	0.072 (3)	0.059 (3)	0.012 (2)	0.023 (2)	0.013 (2)
C24	0.063 (3)	0.055 (3)	0.046 (3)	0.007 (2)	0.013 (2)	0.007 (2)
C25	0.044 (3)	0.068 (3)	0.054 (3)	0.001 (2)	0.011 (2)	0.003 (2)
C26	0.036 (2)	0.065 (3)	0.053 (3)	0.009 (2)	0.016 (2)	0.008 (2)

Geometric parameters (Å, º) top

Fe1—N1	2.086 (3)	S2—C2	1.633 (4)
Fe1—O2	2.100 (2)	C3—H7	0.9300
Fe1—O3	2.102 (3)	C4—H8	0.9300
Fe1—N2	2.107 (3)	C5—C10	1.378 (4)
Fe1—O1ⁱ	2.264 (3)	C5—C6	1.387 (4)
Fe1—O1	2.281 (2)	C6—C7	1.383 (5)
Cl1—C8	1.752 (4)	C6—H9	0.9300
Cl2—C16	1.738 (4)	C7—C8	1.362 (5)
Cl3—C24	1.745 (4)	C7—H10	0.9300
N1—C1	1.169 (4)	C8—C9	1.373 (4)
N2—C2	1.162 (4)	C9—C10	1.372 (4)
N3—C4	1.285 (4)	C9—H11	0.9300
N3—N4	1.376 (4)	C10—H12	0.9300
N4—C3	1.305 (4)	C11—H13	0.9300
N5—C4	1.351 (4)	C12—H14	0.9300
N5—C3	1.360 (4)	C13—C14	1.377 (4)
N5—C5	1.432 (4)	C13—C18	1.384 (4)
N6—C12	1.306 (4)	C14—C15	1.380 (4)
N6—N7	1.397 (4)	C14—H15	0.9300
N7—C11	1.298 (4)	C15—C16	1.357 (5)
N8—C12	1.352 (4)	C15—H16	0.9300
N8—C11	1.359 (4)	C16—C17	1.370 (4)
N8—C13	1.428 (4)	C17—C18	1.378 (4)
N9—C20	1.300 (4)	C17—H17	0.9300
N9—N10	1.381 (3)	C18—H18	0.9300
N10—C19	1.296 (4)	C19—H19	0.9300
N11—C19	1.361 (4)	C20—H20	0.9300
N11—C20	1.359 (4)	C21—C26	1.387 (4)
N11—C21	1.429 (4)	C21—C22	1.387 (4)
O1—Fe1ⁱ	2.264 (3)	C22—C23	1.374 (4)
O1—H1	0.869 (10)	C22—H21	0.9300
O1—H2	0.880 (10)	C23—C24	1.371 (4)
O2—H3	0.884 (10)	C23—H22	0.9300
O2—H4	0.881 (10)	C24—C25	1.372 (4)
O3—H5	0.885 (10)	C25—C26	1.375 (4)
O3—H6	0.875 (10)	C25—H23	0.9300
S1—C1	1.632 (4)	C26—H24	0.9300

N1—Fe1—O2	90.22 (11)	C8—C7—H10	120.3
N1—Fe1—O3	89.68 (12)	C6—C7—H10	120.3
O2—Fe1—O3	101.01 (10)	C7—C8—C9	121.6 (4)
N1—Fe1—N2	178.33 (12)	C7—C8—Cl1	120.2 (3)
O2—Fe1—N2	89.47 (11)	C9—C8—Cl1	118.2 (3)
O3—Fe1—N2	88.76 (11)	C8—C9—C10	119.0 (4)
N1—Fe1—O1ⁱ	90.32 (11)	C8—C9—H11	120.5
O2—Fe1—O1ⁱ	89.04 (10)	C10—C9—H11	120.5
O3—Fe1—O1ⁱ	169.95 (9)	C9—C10—C5	120.7 (4)
N2—Fe1—O1ⁱ	91.32 (11)	C9—C10—H12	119.6
N1—Fe1—O1	89.79 (10)	C5—C10—H12	119.6
O2—Fe1—O1	167.40 (10)	N7—C11—N8	111.9 (3)
O3—Fe1—O1	91.59 (10)	N7—C11—H13	124.0
N2—Fe1—O1	90.87 (10)	N8—C11—H13	124.0
O1ⁱ—Fe1—O1	78.36 (9)	N6—C12—N8	111.7 (3)
C1—N1—Fe1	175.9 (3)	N6—C12—H14	124.2
C2—N2—Fe1	172.4 (3)	N8—C12—H14	124.2
C4—N3—N4	107.0 (3)	C14—C13—C18	119.2 (4)
C3—N4—N3	105.8 (3)	C14—C13—N8	120.7 (3)
C4—N5—C3	102.1 (3)	C18—C13—N8	120.1 (3)
C4—N5—C5	129.6 (3)	C15—C14—C13	120.4 (4)
C3—N5—C5	128.4 (3)	C15—C14—H15	119.8
C12—N6—N7	106.4 (3)	C13—C14—H15	119.8
C11—N7—N6	106.3 (3)	C16—C15—C14	120.1 (4)
C12—N8—C11	103.7 (3)	C16—C15—H16	120.0
C12—N8—C13	128.3 (3)	C14—C15—H16	120.0
C11—N8—C13	127.9 (3)	C15—C16—C17	120.2 (4)
C20—N9—N10	106.8 (3)	C15—C16—Cl2	120.3 (3)
C19—N10—N9	106.9 (3)	C17—C16—Cl2	119.4 (3)
C19—N11—C20	103.5 (3)	C16—C17—C18	120.3 (4)
C19—N11—C21	128.0 (3)	C16—C17—H17	119.8
C20—N11—C21	128.5 (3)	C18—C17—H17	119.8
Fe1ⁱ—O1—Fe1	101.64 (9)	C17—C18—C13	119.7 (4)
Fe1ⁱ—O1—H1	104 (3)	C17—C18—H18	120.1
Fe1—O1—H1	119 (2)	C13—C18—H18	120.1
Fe1ⁱ—O1—H2	110 (3)	N10—C19—N11	111.4 (3)
Fe1—O1—H2	114 (2)	N10—C19—H19	124.3
H1—O1—H2	108 (2)	N11—C19—H19	124.3
Fe1—O2—H3	128 (2)	N9—C20—N11	111.3 (3)
Fe1—O2—H4	125 (2)	N9—C20—H20	124.3
H3—O2—H4	106 (2)	N11—C20—H20	124.3
Fe1—O3—H5	119 (3)	C26—C21—C22	119.0 (3)
Fe1—O3—H6	117 (2)	C26—C21—N11	120.8 (3)
H5—O3—H6	106 (2)	C22—C21—N11	120.2 (3)
N1—C1—S1	179.6 (3)	C23—C22—C21	120.1 (3)
N2—C2—S2	179.7 (3)	C23—C22—H21	119.9
N4—C3—N5	112.2 (3)	C21—C22—H21	119.9
N4—C3—H7	123.9	C24—C23—C22	120.2 (4)
N5—C3—H7	123.9	C24—C23—H22	119.9
N3—C4—N5	112.9 (4)	C22—C23—H22	119.9
N3—C4—H8	123.6	C25—C24—C23	120.4 (4)
N5—C4—H8	123.6	C25—C24—Cl3	119.9 (3)
C10—C5—C6	119.4 (4)	C23—C24—Cl3	119.7 (3)
C10—C5—N5	120.8 (3)	C24—C25—C26	119.8 (4)
C6—C5—N5	119.8 (3)	C24—C25—H23	120.1
C5—C6—C7	119.9 (4)	C26—C25—H23	120.1
C5—C6—H9	120.1	C25—C26—C21	120.4 (3)
C7—C6—H9	120.1	C25—C26—H24	119.8
C8—C7—C6	119.4 (4)	C21—C26—H24	119.8

Symmetry code: (i) −x+1, −y, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···N10ⁱⁱ	0.87 (3)	1.97 (3)	2.827 (4)	170 (3)
O1—H2···N9	0.88 (3)	1.94 (3)	2.819 (4)	173 (3)
O2—H3···N7ⁱⁱⁱ	0.88 (3)	1.98 (3)	2.866 (5)	178 (3)
O2—H4···N4^iv	0.88 (2)	1.97 (3)	2.853 (4)	175 (3)
O3—H5···N6	0.88 (3)	1.92 (3)	2.802 (4)	174 (3)
O3—H6···N3^v	0.88 (2)	1.93 (2)	2.803 (4)	172 (3)
C3—H7···S2^vi	0.93	2.72	3.624 (5)	165
C22—H21···S2ⁱⁱ	0.93	2.87	3.736 (5)	156
C11—H13···S1^vii	0.93	2.87	3.783 (5)	167

Symmetry codes: (ii) −x, −y, −z+1; (iii) x+1, y, z; (iv) x, y−1, z; (v) x−1, y−1, z; (vi) x, y+1, z; (vii) x−1, y, z.

Experimental details

Crystal data
Chemical formula	[Fe₂(NCS)₄(H₂O)₆]·6C₈H₆ClN₃
M_r	1529.76
Crystal system, space group	Triclinic, P1
Temperature (K)	298
a, b, c (Å)	7.944 (3), 11.085 (5), 19.912 (10)
α, β, γ (°)	105.613 (10), 97.75 (1), 97.932 (7)
V (Å³)	1645.1 (12)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	0.88
Crystal size (mm)	0.25 × 0.21 × 0.17

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.811, 0.865
No. of measured, independent and observed [I > 2σ(I)] reflections	8642, 5705, 2903
R_int	0.032
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.044, 0.076, 0.77
No. of reflections	5705
No. of parameters	439
No. of restraints	9
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.25, −0.24

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2003).

Selected geometric parameters (Å, º) top

Fe1—N1	2.086 (3)	Fe1—N2	2.107 (3)
Fe1—O2	2.100 (2)	Fe1—O1ⁱ	2.264 (3)
Fe1—O3	2.102 (3)	Fe1—O1	2.281 (2)

N1—Fe1—O2	90.22 (11)	O3—Fe1—O1ⁱ	169.95 (9)
N1—Fe1—O3	89.68 (12)	N2—Fe1—O1ⁱ	91.32 (11)
O2—Fe1—O3	101.01 (10)	O1ⁱ—Fe1—O1	78.36 (9)
N1—Fe1—N2	178.33 (12)	Fe1ⁱ—O1—Fe1	101.64 (9)
O2—Fe1—O1ⁱ	89.04 (10)

Symmetry code: (i) −x+1, −y, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···N10ⁱⁱ	0.87 (3)	1.97 (3)	2.827 (4)	170 (3)
O1—H2···N9	0.88 (3)	1.94 (3)	2.819 (4)	173 (3)
O2—H3···N7ⁱⁱⁱ	0.88 (3)	1.98 (3)	2.866 (5)	178 (3)
O2—H4···N4^iv	0.88 (2)	1.97 (3)	2.853 (4)	175 (3)
O3—H5···N6	0.88 (3)	1.92 (3)	2.802 (4)	174 (3)
O3—H6···N3^v	0.88 (2)	1.93 (2)	2.803 (4)	172 (3)
C3—H7···S2^vi	0.93	2.72	3.624 (5)	165
C22—H21···S2ⁱⁱ	0.93	2.87	3.736 (5)	156
C11—H13···S1^vii	0.93	2.87	3.783 (5)	167

Symmetry codes: (ii) −x, −y, −z+1; (iii) x+1, y, z; (iv) x, y−1, z; (v) x−1, y−1, z; (vi) x, y+1, z; (vii) x−1, y, z.

References

Bruker (1998). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Hsu, H. F., Dong, Y., Shu, L., Young, V. G. Jr & Que, L. Jr (1999). J. Am. Chem. Soc. 121, 5230–5237. Web of Science CSD CrossRef CAS Google Scholar
MacMurdo, V. L., Zheng, H. & Que, L. Jr (2000). Inorg. Chem. 39, 2254–2255. Web of Science CSD CrossRef PubMed CAS Google Scholar
Nordlund, P. & Eklund, H. (1993). J. Mol. Biol. 232, 123–164. CrossRef CAS PubMed Web of Science Google Scholar
Sazinsky, M. H., Bard, J., Di Donato, A. & Lippard, S. J. (2004). J. Biol. Chem. 279, 30600–30610. Web of Science CrossRef PubMed CAS Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Spek, A. L. (2003). J. Appl. Cryst. 36, 7–13. Web of Science CrossRef CAS IUCr Journals Google Scholar
Stubbe, J. & Van der Donk, W. A. (1998). Chem. Rev. 98, 705–762. Web of Science CrossRef PubMed CAS Google Scholar
Yoon, S., Kelly, A. E. & Lippard, S. J. (2004). Polyhedron, 23, 2805–2812. Web of Science CSD CrossRef CAS Google Scholar
Zheng, H., Zang, Y., Dong, Y., Young, V. G. Jr & Que, L. Jr (1999). J. Am. Chem. Soc. 121, 2226–2235. Web of Science CSD CrossRef CAS Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 64| Part 8| August 2008| Pages m996-m997

doi:10.1107/S1600536808019326

Open

access

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page

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

Di-μ-aqua-bis­­[di­aqua­bis­(thio­cyanato-κN)iron(II)] 4-(4-chloro­phen­yl)-1,2,4-triazole hexa­solvate

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

References

metal-organic compounds

Di-μ-aqua-bis[diaquabis(thiocyanato-κN)iron(II)] 4-(4-chlorophenyl)-1,2,4-triazole hexasolvate