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

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ISSN: 2056-9890

Di­aqua­hexa-μ2-di­chloro­acetato-μ3-oxido-tetra­hydro­furan­diiron(III)manganese(II)

aDepartment of Chemistry, General Campus, Shahid Beheshti University, Tehran 1983963113, Iran, and bDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
*Correspondence e-mail: seikweng@um.edu.my

(Received 17 December 2009; accepted 17 December 2009; online 24 December 2009)

In the oxido-centered title compound, [Fe2Mn(C2HCl2O2)6O(C4H8O)(H2O)2], the central O atom is linked to three metal atoms, which are themselves each linked to four dichloro­acetate anions, and is in a triangular configuration. Two of the metal atoms are each coordinated by a water mol­ecule, whereas the third is coordinated by a tetra­hydro­furan mol­ecule. In the crystal, adjacent mol­ecules are linked by O—H⋯O and O—H⋯Cl hydrogen bonds across centers of inversion, generating a hydrogen-bonded chain along the c axis. The MnII atoms are disordered with respect to the FeIII atoms, and the same metal site is occupied by 1/3Mn + 2/3Fe.

Related literature

For aqua­bis(tetra­hydro­furan)hexa­kis(trifluoro­acetato)(μ3-oxido)M(II)diiron(III) (M = copper, zinc), see: Amini et al. (2004a[Amini, M. M., Yadavi, M. & Ng, S. W. (2004a). Acta Cryst. E60, m492-m494.],b[Amini, M. M., Yadavi, M. & Ng, S. W. (2004b). Acta Cryst. E60, m495-m497.]).

[Scheme 1]

Experimental

Crystal data
  • [Fe2Mn(C2HCl2O2)6O(C4H8O)(H2O)2]

  • Mr = 1058.34

  • Triclinic, [P \overline 1]

  • a = 9.380 (1) Å

  • b = 13.316 (1) Å

  • c = 15.432 (1) Å

  • α = 90.131 (1)°

  • β = 100.067 (1)°

  • γ = 97.677 (1)°

  • V = 1880.1 (2) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 2.01 mm−1

  • T = 295 K

  • 0.35 × 0.15 × 0.15 mm

Data collection
  • Bruker SMART APEX diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.540, Tmax = 0.753

  • 15425 measured reflections

  • 8543 independent reflections

  • 5788 reflections with I > 2σ(I)

  • Rint = 0.025

Refinement
  • R[F2 > 2σ(F2)] = 0.063

  • wR(F2) = 0.207

  • S = 1.03

  • 8543 reflections

  • 440 parameters

  • 35 restraints

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

  • Δρmax = 1.64 e Å−3

  • Δρmin = −0.90 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O1w—H11⋯O3i 0.85 (1) 2.01 (3) 2.809 (6) 158 (5)
O2w—H22⋯O8ii 0.85 (1) 2.06 (4) 2.821 (5) 149 (7)
O2W—H21⋯O10ii 0.84 (6) 2.19 (7) 2.950 (6) 150 (6)
O1W—H12⋯Cl1i 0.85 (3) 2.47 (4) 3.288 (4) 160 (6)
Symmetry codes: (i) -x+1, -y+1, -z; (ii) -x+1, -y+1, -z+1.

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). APEX2 and SAINT. 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: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: X-SEED (Barbour, 2001[Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). publCIF. In preparation.]).

Supporting information


Related literature top

For aquabis(tetrahydrofuran)hexakis(trifluoroacetato)(µ3-oxo)metal(II)diiron(III) (metal = copper, zinc), see: Amini et al. (2004a,b).

Experimental top

Sodium bicarbonate (4.12 g, 49 mmol) was dissolved in water (50 ml) and this was mixed with dichloroacetic acid (6.19 g, 48 mmol), ferric nitrate nonahydrate (6.46 g, 16 mmol) dissolved in water (30 ml) along with manganese nitrate hexahydrate (2.36 g, 8 mmol) dissolved in water (5 ml). The mixture was stirred for 24 h. The water was removed under reduced pressure and the residue dissolved in a tetrahydrofuran and hexane mixture. The solvent was removed to give an oily residue. This was treated with hexane to remove the oil; the pure compound was obtained by recrystallization from hexane to which several drops of tetrahydrofuran were added. The brown compound melts at 435–436 K.

Refinement top

Carbon-bound H-atoms were placed in calculated positions (C–H = 0.97–0.98 Å) and were included in the refinement in the riding model approximation, with Uiso(H) set to 1.2Ueq(C). The water H-atoms were located in a difference Fourier map, and were refined with distance restraints of O–H = 0.84 (1) Å and H···H 1.37 (1) Å; their Uiso parameters were refined.

The manganese(II) atoms are disordered with respect to the iron(III) atoms, with the pair of Mn/Fe atoms occupying the same site. As the occupancy refined to nearly 1:2, the ratio was fixed as exactly 1:2.

For the THF molecule, the O—C distances were restrained to 1.45 (1) Å and the C—C distances to 1.54 (1) Å; the anisotropic displacement parameters of atoms C13, C14, C15 and C16 were restrained to be nearly isotropic.

The final difference map had a peak in the vicinity of O14.

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. Displacement ellipsoid plot (Barbour, 2001) of Fe2MnO(H2O)2(C4H8O)(C2HO2Cl2)6; ellipsoids are drawn at the 50% probability level and H atoms of arbitrary radius.
Diaquahexa-µ2-dichloroacetato-µ3-oxido- tetrahydrofurandiiron(III)manganese(II) top
Crystal data top
[Fe2Mn(C2HCl2O2)6O(C4H8O)(H2O)2]Z = 2
Mr = 1058.34F(000) = 1046
Triclinic, P1Dx = 1.869 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.380 (1) ÅCell parameters from 4712 reflections
b = 13.316 (1) Åθ = 2.4–27.4°
c = 15.432 (1) ŵ = 2.01 mm1
α = 90.131 (1)°T = 295 K
β = 100.067 (1)°Block, brown
γ = 97.677 (1)°0.35 × 0.15 × 0.15 mm
V = 1880.1 (2) Å3
Data collection top
Bruker SMART APEX
diffractometer
8543 independent reflections
Radiation source: fine-focus sealed tube5788 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
ω scansθmax = 27.5°, θmin = 1.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1212
Tmin = 0.540, Tmax = 0.753k = 1717
15425 measured reflectionsl = 2017
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)] = 0.063Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.207H atoms treated by a mixture of independent and constrained refinement
S = 1.03 w = 1/[σ2(Fo2) + (0.1141P)2 + 3.6071P]
where P = (Fo2 + 2Fc2)/3
8543 reflections(Δ/σ)max = 0.001
440 parametersΔρmax = 1.64 e Å3
35 restraintsΔρmin = 0.90 e Å3
Crystal data top
[Fe2Mn(C2HCl2O2)6O(C4H8O)(H2O)2]γ = 97.677 (1)°
Mr = 1058.34V = 1880.1 (2) Å3
Triclinic, P1Z = 2
a = 9.380 (1) ÅMo Kα radiation
b = 13.316 (1) ŵ = 2.01 mm1
c = 15.432 (1) ÅT = 295 K
α = 90.131 (1)°0.35 × 0.15 × 0.15 mm
β = 100.067 (1)°
Data collection top
Bruker SMART APEX
diffractometer
8543 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
5788 reflections with I > 2σ(I)
Tmin = 0.540, Tmax = 0.753Rint = 0.025
15425 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.06335 restraints
wR(F2) = 0.207H atoms treated by a mixture of independent and constrained refinement
S = 1.03Δρmax = 1.64 e Å3
8543 reflectionsΔρmin = 0.90 e Å3
440 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Fe10.48559 (8)0.58734 (5)0.15449 (5)0.02900 (19)0.67
Fe20.70394 (8)0.77291 (5)0.26487 (5)0.03113 (19)0.67
Fe30.62644 (8)0.55454 (6)0.36749 (5)0.0331 (2)0.67
Mn10.48559 (8)0.58734 (5)0.15449 (5)0.02900 (19)0.33
Mn20.70394 (8)0.77291 (5)0.26487 (5)0.03113 (19)0.33
Mn30.62644 (8)0.55454 (6)0.36749 (5)0.0331 (2)0.33
Cl10.7881 (3)0.31545 (18)0.11574 (16)0.0856 (7)
Cl20.5060 (4)0.21726 (17)0.1440 (3)0.1210 (11)
Cl30.9003 (3)0.83097 (19)0.00937 (16)0.0953 (8)
Cl40.9893 (3)0.6422 (2)0.0556 (2)0.1111 (10)
Cl50.3394 (5)0.9362 (2)0.0396 (2)0.1385 (14)
Cl60.3033 (4)0.9569 (2)0.2189 (3)0.1291 (12)
Cl70.1673 (3)0.30107 (17)0.22744 (18)0.0944 (8)
Cl80.0953 (3)0.4052 (2)0.37391 (18)0.1134 (11)
Cl90.5161 (3)0.77820 (18)0.60071 (13)0.0888 (7)
Cl100.6888 (3)0.94612 (19)0.53350 (18)0.1011 (9)
Cl111.2099 (2)0.7122 (2)0.3483 (2)0.1044 (9)
Cl121.1217 (3)0.7937 (2)0.5016 (2)0.1191 (11)
O10.5657 (5)0.4523 (3)0.1497 (3)0.0473 (10)
O20.6456 (5)0.4239 (3)0.2908 (3)0.0490 (10)
O30.6341 (4)0.6367 (3)0.0718 (3)0.0449 (9)
O40.7827 (5)0.7618 (3)0.1493 (3)0.0522 (11)
O50.3761 (4)0.7103 (3)0.1277 (3)0.0485 (10)
O60.5320 (4)0.8361 (3)0.2003 (3)0.0532 (11)
O70.3171 (4)0.5173 (3)0.2051 (3)0.0503 (10)
O80.3900 (4)0.4967 (3)0.3482 (2)0.0421 (9)
O90.6494 (6)0.8139 (3)0.3790 (3)0.0556 (11)
O100.5825 (4)0.6753 (3)0.4504 (3)0.0426 (9)
O110.8568 (4)0.6037 (3)0.4047 (3)0.0487 (10)
O120.8968 (4)0.7428 (3)0.3279 (3)0.0523 (11)
O130.6045 (4)0.6424 (2)0.2557 (2)0.0310 (7)
O140.8102 (5)0.9224 (3)0.2647 (3)0.0485 (10)
O1w0.3539 (5)0.5332 (3)0.0336 (2)0.0428 (9)
H110.354 (9)0.4734 (18)0.015 (3)0.07 (2)*
H120.336 (7)0.570 (3)0.011 (2)0.046 (18)*
O2w0.6460 (4)0.4572 (3)0.4791 (3)0.0407 (8)
H210.580 (7)0.408 (4)0.481 (5)0.08 (3)*
H220.662 (11)0.489 (6)0.528 (3)0.13 (4)*
C10.6208 (6)0.4026 (4)0.2124 (4)0.0396 (12)
C20.6613 (9)0.2998 (5)0.1891 (5)0.0596 (18)
H20.70800.27060.24330.072*
C30.7428 (6)0.7024 (4)0.0862 (3)0.0364 (11)
C40.8391 (7)0.7079 (6)0.0146 (5)0.0615 (19)
H40.78290.67300.03910.074*
C50.4141 (6)0.7987 (4)0.1553 (4)0.0425 (13)
C60.3003 (8)0.8696 (5)0.1314 (7)0.079 (3)
H60.20310.82990.11700.095*
C70.3020 (6)0.4845 (4)0.2785 (4)0.0393 (12)
C80.1511 (7)0.4205 (6)0.2740 (5)0.0608 (18)
H80.07830.45250.23400.073*
C90.6017 (6)0.7685 (4)0.4403 (4)0.0374 (11)
C100.5580 (7)0.8389 (5)0.5070 (4)0.0504 (15)
H100.46820.86340.47770.061*
C110.9324 (6)0.6772 (4)0.3815 (4)0.0407 (12)
C121.0941 (7)0.6917 (6)0.4260 (5)0.0584 (17)
H12a1.11480.63030.45800.070*
C130.7881 (14)0.9875 (9)0.1903 (8)0.140 (5)
H13A0.70121.01970.19000.168*
H13B0.77690.94880.13560.168*
C140.9230 (15)1.0664 (10)0.2007 (8)0.143 (5)
H14A1.00471.04060.18160.171*
H14B0.90391.12800.17000.171*
C150.9457 (18)1.0811 (8)0.2983 (8)0.144 (5)
H15A0.87731.12290.31500.173*
H15B1.04451.11260.32130.173*
C160.9183 (18)0.9741 (9)0.3316 (9)0.165 (6)
H16A1.00690.94240.33960.198*
H16B0.88330.97440.38710.198*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0335 (4)0.0263 (4)0.0262 (4)0.0008 (3)0.0051 (3)0.0000 (3)
Fe20.0348 (4)0.0247 (4)0.0311 (4)0.0016 (3)0.0025 (3)0.0006 (3)
Fe30.0358 (4)0.0320 (4)0.0305 (4)0.0010 (3)0.0059 (3)0.0003 (3)
Mn10.0335 (4)0.0263 (4)0.0262 (4)0.0008 (3)0.0051 (3)0.0000 (3)
Mn20.0348 (4)0.0247 (4)0.0311 (4)0.0016 (3)0.0025 (3)0.0006 (3)
Mn30.0358 (4)0.0320 (4)0.0305 (4)0.0010 (3)0.0059 (3)0.0003 (3)
Cl10.0947 (15)0.0943 (15)0.0880 (15)0.0563 (13)0.0386 (12)0.0159 (12)
Cl20.131 (2)0.0474 (11)0.186 (3)0.0117 (13)0.050 (2)0.0354 (15)
Cl30.1197 (19)0.0878 (15)0.0785 (14)0.0301 (14)0.0511 (14)0.0132 (12)
Cl40.0769 (14)0.120 (2)0.155 (3)0.0284 (14)0.0592 (17)0.0058 (19)
Cl50.214 (4)0.104 (2)0.098 (2)0.074 (2)0.009 (2)0.0416 (17)
Cl60.134 (2)0.0947 (19)0.185 (3)0.0527 (18)0.072 (2)0.010 (2)
Cl70.1038 (17)0.0655 (13)0.1057 (18)0.0294 (12)0.0273 (14)0.0193 (12)
Cl80.0954 (17)0.150 (3)0.0903 (17)0.0524 (17)0.0554 (14)0.0208 (16)
Cl90.145 (2)0.0797 (14)0.0520 (11)0.0171 (14)0.0442 (12)0.0051 (10)
Cl100.1105 (18)0.0784 (14)0.1083 (18)0.0314 (13)0.0369 (15)0.0541 (14)
Cl110.0527 (11)0.142 (2)0.132 (2)0.0308 (13)0.0393 (13)0.0530 (18)
Cl120.0953 (18)0.121 (2)0.116 (2)0.0117 (16)0.0304 (16)0.0442 (18)
O10.072 (3)0.033 (2)0.037 (2)0.0182 (19)0.0018 (19)0.0010 (16)
O20.074 (3)0.042 (2)0.034 (2)0.018 (2)0.0087 (19)0.0006 (17)
O30.044 (2)0.053 (2)0.035 (2)0.0111 (18)0.0133 (16)0.0022 (17)
O40.063 (3)0.046 (2)0.045 (2)0.013 (2)0.020 (2)0.0057 (19)
O50.048 (2)0.038 (2)0.055 (3)0.0091 (18)0.0061 (19)0.0007 (18)
O60.043 (2)0.033 (2)0.075 (3)0.0012 (17)0.010 (2)0.004 (2)
O70.043 (2)0.065 (3)0.035 (2)0.0156 (19)0.0043 (17)0.0022 (19)
O80.039 (2)0.052 (2)0.033 (2)0.0039 (17)0.0066 (16)0.0045 (17)
O90.088 (3)0.033 (2)0.048 (2)0.005 (2)0.028 (2)0.0066 (18)
O100.055 (2)0.036 (2)0.039 (2)0.0071 (17)0.0136 (18)0.0020 (16)
O110.036 (2)0.049 (2)0.059 (3)0.0001 (18)0.0065 (18)0.012 (2)
O120.039 (2)0.046 (2)0.063 (3)0.0021 (18)0.0071 (19)0.013 (2)
O130.0362 (18)0.0248 (16)0.0294 (17)0.0007 (13)0.0021 (14)0.0022 (13)
O140.055 (2)0.031 (2)0.054 (3)0.0073 (17)0.003 (2)0.0038 (17)
O1w0.051 (2)0.045 (2)0.0296 (19)0.0013 (19)0.0038 (17)0.0049 (17)
O2w0.046 (2)0.043 (2)0.032 (2)0.0025 (18)0.0067 (16)0.0062 (17)
C10.049 (3)0.035 (3)0.037 (3)0.007 (2)0.013 (2)0.000 (2)
C20.101 (5)0.039 (3)0.048 (4)0.032 (3)0.020 (4)0.004 (3)
C30.040 (3)0.038 (3)0.032 (3)0.001 (2)0.011 (2)0.002 (2)
C40.052 (4)0.080 (5)0.052 (4)0.019 (3)0.027 (3)0.009 (3)
C50.036 (3)0.039 (3)0.051 (3)0.004 (2)0.005 (2)0.009 (3)
C60.046 (4)0.038 (3)0.145 (8)0.011 (3)0.010 (4)0.016 (4)
C70.030 (2)0.044 (3)0.042 (3)0.005 (2)0.008 (2)0.005 (2)
C80.047 (3)0.067 (4)0.065 (4)0.015 (3)0.016 (3)0.000 (3)
C90.040 (3)0.034 (3)0.036 (3)0.002 (2)0.001 (2)0.005 (2)
C100.060 (4)0.045 (3)0.047 (3)0.006 (3)0.013 (3)0.012 (3)
C110.033 (3)0.043 (3)0.045 (3)0.006 (2)0.004 (2)0.004 (2)
C120.038 (3)0.063 (4)0.069 (4)0.002 (3)0.002 (3)0.012 (3)
C130.154 (9)0.108 (7)0.138 (8)0.014 (7)0.003 (7)0.030 (7)
C140.152 (8)0.112 (7)0.154 (9)0.030 (6)0.039 (7)0.032 (7)
C150.188 (9)0.082 (6)0.136 (8)0.059 (6)0.013 (7)0.009 (6)
C160.179 (9)0.122 (8)0.167 (9)0.020 (7)0.010 (8)0.010 (7)
Geometric parameters (Å, º) top
Fe1—O131.841 (3)O7—C71.239 (7)
Fe1—O72.004 (4)O8—C71.232 (7)
Fe1—O12.045 (4)O9—C91.241 (7)
Fe1—O52.052 (4)O10—C91.244 (6)
Fe1—O32.092 (4)O11—C111.222 (7)
Fe1—O1w2.116 (4)O12—C111.241 (7)
Fe2—O131.852 (3)O14—C161.419 (9)
Fe2—O121.991 (4)O14—C131.442 (8)
Fe2—O92.012 (4)O1w—H110.85 (1)
Fe2—O62.026 (4)O1w—H120.85 (1)
Fe2—O42.058 (4)O2w—H210.85 (1)
Fe2—O142.104 (4)O2w—H220.85 (1)
Fe3—O132.082 (3)C1—C21.528 (8)
Fe3—O22.146 (4)C2—H20.98
Fe3—O112.148 (4)C3—C41.541 (8)
Fe3—O2w2.155 (4)C4—H40.98
Fe3—O102.178 (4)C5—C61.516 (8)
Fe3—O82.216 (4)C6—H60.98
Cl1—C21.773 (8)C7—C81.542 (8)
Cl2—C21.740 (9)C8—H80.98
Cl3—C41.725 (8)C9—C101.534 (8)
Cl4—C41.781 (9)C10—H100.98
Cl5—C61.740 (10)C11—C121.538 (8)
Cl6—C61.774 (10)C12—H12a0.98
Cl7—C81.779 (8)C13—C141.519 (9)
Cl8—C81.717 (7)C13—H13A0.97
Cl9—C101.736 (7)C13—H13B0.97
Cl10—C101.751 (7)C14—C151.493 (9)
Cl11—C121.751 (8)C14—H14A0.97
Cl12—C121.752 (8)C14—H14B0.97
O1—C11.250 (7)C15—C161.521 (9)
O2—C11.217 (7)C15—H15A0.97
O3—C31.240 (6)C15—H15B0.97
O4—C31.226 (7)C16—H16A0.97
O5—C51.236 (7)C16—H16B0.97
O6—C51.240 (7)
O13—Fe1—O7100.17 (16)Cl2—C2—Cl1111.0 (4)
O13—Fe1—O198.93 (16)C1—C2—H2108.3
O7—Fe1—O189.64 (19)Cl2—C2—H2108.3
O13—Fe1—O595.75 (16)Cl1—C2—H2108.3
O7—Fe1—O589.80 (19)O4—C3—O3128.6 (5)
O1—Fe1—O5165.17 (16)O4—C3—C4117.0 (5)
O13—Fe1—O394.81 (15)O3—C3—C4114.4 (5)
O7—Fe1—O3164.61 (16)C3—C4—Cl3112.5 (5)
O1—Fe1—O384.53 (18)C3—C4—Cl4106.3 (5)
O5—Fe1—O392.22 (18)Cl3—C4—Cl4110.5 (4)
O13—Fe1—O1w176.02 (16)C3—C4—H4109.1
O7—Fe1—O1w83.07 (16)Cl3—C4—H4109.1
O1—Fe1—O1w83.33 (17)Cl4—C4—H4109.1
O5—Fe1—O1w81.89 (17)O5—C5—O6128.3 (5)
O3—Fe1—O1w82.11 (16)O5—C5—C6115.3 (5)
O13—Fe2—O1298.58 (16)O6—C5—C6116.4 (6)
O13—Fe2—O997.57 (16)C5—C6—Cl5107.9 (6)
O12—Fe2—O990.9 (2)C5—C6—Cl6111.4 (6)
O13—Fe2—O694.49 (16)Cl5—C6—Cl6109.1 (4)
O12—Fe2—O6166.89 (17)C5—C6—H6109.5
O9—Fe2—O688.4 (2)Cl5—C6—H6109.5
O13—Fe2—O494.61 (16)Cl6—C6—H6109.5
O12—Fe2—O487.6 (2)O8—C7—O7128.3 (5)
O9—Fe2—O4167.81 (17)O8—C7—C8121.0 (5)
O6—Fe2—O490.4 (2)O7—C7—C8110.7 (5)
O13—Fe2—O14175.47 (16)C7—C8—Cl8114.3 (5)
O12—Fe2—O1484.51 (17)C7—C8—Cl7105.4 (5)
O9—Fe2—O1485.66 (17)Cl8—C8—Cl7110.5 (4)
O6—Fe2—O1482.38 (16)C7—C8—H8108.8
O4—Fe2—O1482.17 (17)Cl8—C8—H8108.8
O13—Fe3—O291.27 (14)Cl7—C8—H8108.8
O13—Fe3—O1194.02 (15)O9—C9—O10127.3 (5)
O2—Fe3—O1196.35 (18)O9—C9—C10113.6 (5)
O13—Fe3—O2w177.25 (15)O10—C9—C10119.1 (5)
O2—Fe3—O2w86.15 (16)C9—C10—Cl9113.7 (4)
O11—Fe3—O2w87.23 (16)C9—C10—Cl10111.5 (4)
O13—Fe3—O1092.63 (14)Cl9—C10—Cl10111.7 (4)
O2—Fe3—O10172.53 (16)C9—C10—H10106.5
O11—Fe3—O1089.72 (17)Cl9—C10—H10106.5
O2w—Fe3—O1089.82 (15)Cl10—C10—H10106.5
O13—Fe3—O893.57 (14)O11—C11—O12129.2 (5)
O2—Fe3—O885.85 (17)O11—C11—C12115.5 (5)
O11—Fe3—O8172.04 (15)O12—C11—C12115.3 (5)
O2w—Fe3—O885.28 (15)C11—C12—Cl11111.3 (5)
O10—Fe3—O887.56 (15)C11—C12—Cl12107.9 (5)
C1—O1—Fe1128.2 (4)Cl11—C12—Cl12111.4 (4)
C1—O2—Fe3134.2 (4)C11—C12—H12a108.7
C3—O3—Fe1129.1 (3)Cl11—C12—H12a108.7
C3—O4—Fe2130.9 (4)Cl12—C12—H12a108.7
C5—O5—Fe1128.3 (4)O14—C13—C14106.2 (8)
C5—O6—Fe2132.2 (4)O14—C13—H13A110.5
C7—O7—Fe1134.5 (4)C14—C13—H13A110.5
C7—O8—Fe3128.0 (3)O14—C13—H13B110.5
C9—O9—Fe2135.5 (4)C14—C13—H13B110.5
C9—O10—Fe3128.8 (4)H13A—C13—H13B108.7
C11—O11—Fe3130.0 (4)C15—C14—C1397.9 (9)
C11—O12—Fe2132.6 (4)C15—C14—H14A112.2
Fe1—O13—Fe2123.79 (18)C13—C14—H14A112.2
Fe1—O13—Fe3118.50 (16)C15—C14—H14B112.2
Fe2—O13—Fe3117.70 (17)C13—C14—H14B112.2
C16—O14—C13108.7 (7)H14A—C14—H14B109.8
C16—O14—Fe2127.9 (5)C14—C15—C16103.8 (10)
C13—O14—Fe2123.3 (5)C14—C15—H15A111.0
Fe1—O1w—H11121 (4)C16—C15—H15A111.0
Fe1—O1w—H12124 (4)C14—C15—H15B111.0
H11—O1w—H12107.6 (17)C16—C15—H15B111.0
Fe3—O2w—H21119 (6)H15A—C15—H15B109.0
Fe3—O2w—H22114 (7)O14—C16—C15104.4 (8)
H21—O2w—H22107.5 (18)O14—C16—H16A110.9
O2—C1—O1129.0 (5)C15—C16—H16A110.9
O2—C1—C2114.4 (5)O14—C16—H16B110.9
O1—C1—C2116.5 (5)C15—C16—H16B110.9
C1—C2—Cl2110.8 (5)H16A—C16—H16B108.9
C1—C2—Cl1110.0 (5)
O13—Fe1—O1—C130.2 (5)O3—Fe1—O13—Fe3134.8 (2)
O7—Fe1—O1—C170.1 (5)O12—Fe2—O13—Fe1135.3 (2)
O5—Fe1—O1—C1157.9 (6)O9—Fe2—O13—Fe1132.7 (2)
O3—Fe1—O1—C1124.2 (5)O6—Fe2—O13—Fe143.7 (3)
O1w—Fe1—O1—C1153.2 (5)O4—Fe2—O13—Fe147.0 (3)
O13—Fe3—O2—C114.5 (6)O12—Fe2—O13—Fe345.9 (2)
O11—Fe3—O2—C1108.7 (6)O9—Fe2—O13—Fe346.1 (2)
O2w—Fe3—O2—C1164.6 (6)O6—Fe2—O13—Fe3135.1 (2)
O8—Fe3—O2—C179.0 (6)O4—Fe2—O13—Fe3134.2 (2)
O13—Fe1—O3—C316.7 (5)O2—Fe3—O13—Fe143.2 (2)
O7—Fe1—O3—C3176.6 (6)O11—Fe3—O13—Fe1139.6 (2)
O1—Fe1—O3—C3115.2 (5)O10—Fe3—O13—Fe1130.5 (2)
O5—Fe1—O3—C379.3 (5)O8—Fe3—O13—Fe142.8 (2)
O1w—Fe1—O3—C3160.8 (5)O2—Fe3—O13—Fe2138.0 (2)
O13—Fe2—O4—C318.4 (6)O11—Fe3—O13—Fe241.5 (2)
O12—Fe2—O4—C3116.8 (6)O10—Fe3—O13—Fe248.4 (2)
O9—Fe2—O4—C3160.3 (8)O8—Fe3—O13—Fe2136.1 (2)
O6—Fe2—O4—C376.2 (6)O12—Fe2—O14—C13139.5 (9)
O14—Fe2—O4—C3158.4 (6)O9—Fe2—O14—C13129.2 (9)
O13—Fe1—O5—C519.9 (5)O6—Fe2—O14—C1340.2 (9)
O7—Fe1—O5—C5120.1 (5)O4—Fe2—O14—C1351.2 (9)
O1—Fe1—O5—C5152.1 (7)Fe3—O2—C1—O14.6 (10)
O3—Fe1—O5—C575.2 (5)Fe3—O2—C1—C2176.5 (5)
O1w—Fe1—O5—C5156.9 (5)Fe1—O1—C1—C2175.7 (4)
O13—Fe2—O6—C513.1 (6)O2—C1—C2—Cl2114.7 (6)
O12—Fe2—O6—C5162.4 (8)O1—C1—C2—Cl264.4 (7)
O9—Fe2—O6—C5110.6 (6)O2—C1—C2—Cl1122.3 (5)
O4—Fe2—O6—C581.6 (6)O1—C1—C2—Cl158.7 (7)
O14—Fe2—O6—C5163.6 (6)Fe2—O4—C3—C4172.8 (5)
O13—Fe1—O7—C723.4 (6)Fe1—O3—C3—O47.7 (9)
O1—Fe1—O7—C775.7 (6)Fe1—O3—C3—C4171.8 (4)
O5—Fe1—O7—C7119.2 (6)O4—C3—C4—Cl341.7 (8)
O3—Fe1—O7—C7143.2 (6)O3—C3—C4—Cl3138.7 (5)
O1w—Fe1—O7—C7159.0 (6)O4—C3—C4—Cl479.4 (6)
O13—Fe3—O8—C728.5 (5)O3—C3—C4—Cl4100.2 (5)
O2—Fe3—O8—C762.6 (5)Fe1—O5—C5—C6173.3 (5)
O2w—Fe3—O8—C7149.0 (5)Fe2—O6—C5—C6169.0 (5)
O10—Fe3—O8—C7120.9 (5)O5—C5—C6—Cl597.9 (6)
O13—Fe2—O9—C918.2 (6)O6—C5—C6—Cl582.8 (7)
O12—Fe2—O9—C980.6 (6)O5—C5—C6—Cl6142.3 (5)
O6—Fe2—O9—C9112.5 (6)O6—C5—C6—Cl637.0 (8)
O4—Fe2—O9—C9163.2 (8)Fe3—O8—C7—O713.7 (9)
O14—Fe2—O9—C9165.0 (6)Fe3—O8—C7—C8165.3 (4)
O13—Fe3—O10—C925.7 (5)Fe1—O7—C7—C8169.9 (5)
O11—Fe3—O10—C968.3 (5)O8—C7—C8—Cl820.3 (8)
O2w—Fe3—O10—C9155.5 (5)O7—C7—C8—Cl8160.5 (5)
O8—Fe3—O10—C9119.2 (5)O8—C7—C8—Cl7101.2 (6)
O13—Fe3—O11—C1117.7 (5)O7—C7—C8—Cl778.0 (6)
O2—Fe3—O11—C11109.4 (5)Fe2—O9—C9—C10171.7 (5)
O2w—Fe3—O11—C11164.8 (5)Fe3—O10—C9—O91.0 (9)
O10—Fe3—O11—C1174.9 (5)Fe3—O10—C9—C10178.3 (4)
O13—Fe2—O12—C1130.9 (6)O9—C9—C10—Cl9171.3 (5)
O9—Fe2—O12—C1166.9 (6)O10—C9—C10—Cl911.0 (7)
O6—Fe2—O12—C11153.6 (8)O9—C9—C10—Cl1044.0 (7)
O4—Fe2—O12—C11125.2 (6)O10—C9—C10—Cl10138.4 (5)
O14—Fe2—O12—C11152.4 (6)Fe3—O11—C11—C12176.9 (4)
O7—Fe1—O13—Fe2137.2 (2)Fe2—O12—C11—C12170.4 (4)
O1—Fe1—O13—Fe2131.6 (2)O11—C11—C12—Cl11131.1 (5)
O5—Fe1—O13—Fe246.3 (2)O12—C11—C12—Cl1149.9 (7)
O3—Fe1—O13—Fe246.4 (2)O11—C11—C12—Cl12106.4 (6)
O7—Fe1—O13—Fe341.6 (2)O12—C11—C12—Cl1272.7 (6)
O1—Fe1—O13—Fe349.6 (2)Fe2—O14—C13—C14157.0 (8)
O5—Fe1—O13—Fe3132.5 (2)Fe2—O14—C16—C15175.9 (8)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H11···O3i0.85 (1)2.01 (3)2.809 (6)158 (5)
O2w—H22···O8ii0.85 (1)2.06 (4)2.821 (5)149 (7)
O2W—H21···O10ii0.84 (6)2.19 (7)2.950 (6)150 (6)
O1W—H12···Cl1i0.85 (3)2.47 (4)3.288 (4)160 (6)
Symmetry codes: (i) x+1, y+1, z; (ii) x+1, y+1, z+1.

Experimental details

Crystal data
Chemical formula[Fe2Mn(C2HCl2O2)6O(C4H8O)(H2O)2]
Mr1058.34
Crystal system, space groupTriclinic, P1
Temperature (K)295
a, b, c (Å)9.380 (1), 13.316 (1), 15.432 (1)
α, β, γ (°)90.131 (1), 100.067 (1), 97.677 (1)
V3)1880.1 (2)
Z2
Radiation typeMo Kα
µ (mm1)2.01
Crystal size (mm)0.35 × 0.15 × 0.15
Data collection
DiffractometerBruker SMART APEX
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.540, 0.753
No. of measured, independent and
observed [I > 2σ(I)] reflections
15425, 8543, 5788
Rint0.025
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.063, 0.207, 1.03
No. of reflections8543
No. of parameters440
No. of restraints35
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.64, 0.90

Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H11···O3i0.85 (1)2.01 (3)2.809 (6)158 (5)
O2w—H22···O8ii0.85 (1)2.06 (4)2.821 (5)149 (7)
O2W—H21···O10ii0.84 (6)2.19 (7)2.950 (6)150 (6)
O1W—H12···Cl1i0.85 (3)2.47 (4)3.288 (4)160 (6)
Symmetry codes: (i) x+1, y+1, z; (ii) x+1, y+1, z+1.
 

Acknowledgements

The authors thank Shahid Beheshti University and the University of Malaya for supporting this study.

References

First citationAmini, M. M., Yadavi, M. & Ng, S. W. (2004a). Acta Cryst. E60, m492–m494.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationAmini, M. M., Yadavi, M. & Ng, S. W. (2004b). Acta Cryst. E60, m495–m497.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationBarbour, L. J. (2001). J. Supramol. Chem. 1, 189–191.  CrossRef CAS Google Scholar
First citationBruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationWestrip, S. P. (2010). publCIF. In preparation.  Google Scholar

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