Hexa-μ2-acetato-triaqua-μ3-oxido-triiron(III) nitrate acetic acid solvate

Yao, S.; Liu, J.; Han, Q.

doi:10.1107/S1600536808019806

Hexa-μ₂-acetato-triaqua-μ₃-oxido-triiron(III) nitrate acetic acid solvate

The asymmetric unit of the title compound, [Fe₃(CH₃COO)₆O(H₂O)₃]NO₃·CH₃COOH, consists of a hexa-μ₂-acetato-triaqua-μ₃-oxo-triiron(III) macrocation, a nitrate ion and an acetic acid solvent molecule. In the cation, each Fe³⁺ ion is coordinated by four carboxylate O atoms, one central bridged O atom and one water molecule, resulting in distorted FeO₆ octahedra. A network of O—H

O hydrogen bonds helps to establish the packing.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536808019806/hb2740sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536808019806/hb2740Isup2.hkl Contains datablock I

CCDC reference: 700328

checkCIF report

Key indicators

Single-crystal X-ray study
T = 296 K
Mean (C-C) = 0.005 Å
R factor = 0.044
wR factor = 0.106
Data-to-parameter ratio = 13.1

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.33 Ratio
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O1
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O6
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        O10
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        O11
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        O12
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C10
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C12
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        C14
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for         N1
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety         C3
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety         C5
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Labels ..........          6

Alert level G
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......          9

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
  14 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   7 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   5 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Comment top

Transiton-metal coordination complexes based on carboxylates have been attracting chemist's interests and constitutes one of the widest families of research (Thirumurugan & Natarajan, 2004). During the past years, lots of novel carboxylates compounds have been reported (Zhang et al., 2005), in which carboxlate-supported Cr₃(/m₃-O) (Fujihara et al., 1998) and Fe₃(/m₃-O) core (Ren et al., 2004; Vrubel et al., 2006), present two large kinds of widely investigated transtion-metal complexes. Herein, we report the title compound (I).

The title compound, (I), presents a macrocation of [Fe₃O(CH₃COO)₆(H₂O)₃]⁺, in which Fe³⁺ is coordinated by four oxygen atoms from four carboxylates of four acetate anions, one central bridged oxygen atom, and one water molecule. The environment of all the Fe ions are distorted octahedral geometry (Fig. 1). The three Fe atoms approximatively reside in an equilateral triangle with an oxide ion in the center [Fe₃O]. The Fe—O distances range from 1.897 (2) to 2.126 (3) Å (Table 1).

In the crystal, the components are linked by O—H···O hydrogen bonds generating a three-dimensional framework (Fig. 2 and Table 2).

Related literature top

For related literature, see: Fujihara et al. (1998); Ren et al. (2004); Thirumurugan & Natarajan (2004); Vrubel et al. (2006); Zhang et al. (2005).

Experimental top

Fe(NO₃)₃.9H₂O (1 mmol, 0.404 g) was suspended in 5 ml water and 3 ml (1 mol/L) NaOH solution was added dropwise to produce a brown precipitate, then 25 ml acetic acid were added to the mixture. It was stirred under reflux for 3 h. The solution was filtered, and the filtrate was kept at the room temperature. After one weeks, xxx blocks of (I) were obtained.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: PLATON (Spek, 2003).

Figures top

	Fig. 1. The molecular structure of (I), with displacement ellipsoids for the non-hydrogen atoms drawn at the 50% probability level.
	Fig. 2. Three-dimensional structure of (I), with hydrogen bonds shown as dashed lines.

Hexa-µ₂-acetato-triaqua-µ₃-oxido-triiron(III) nitrate acetic acid solvate top

Crystal data top

[Fe₃(C₂H₃O₂)₆O(H₂O)₃]NO₃·C₂H₄O₂	F(000) = 1460
M_r = 713.92	D_x = 1.781 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2092 reflections
a = 11.835 (3) Å	θ = 2.2–23.2°
b = 14.755 (4) Å	µ = 1.71 mm⁻¹
c = 15.250 (4) Å	T = 296 K
β = 90.851 (5)°	Block, yellow
V = 2662.8 (12) Å³	0.18 × 0.13 × 0.10 mm
Z = 4

Data collection top

Bruker SMART CCD diffractometer	4953 independent reflections
Radiation source: fine-focus sealed tube	3355 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.054
ω scans	θ_max = 25.5°, θ_min = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 2001)	h = −14→11
T_min = 0.750, T_max = 0.848	k = −17→17
14072 measured reflections	l = −18→17

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) = 0.106	H atoms treated by a mixture of independent and constrained refinement
S = 1.00	w = 1/[σ²(F_o²) + (0.048P)²] where P = (F_o² + 2F_c²)/3
4953 reflections	(Δ/σ)_max = 0.001
378 parameters	Δρ_max = 0.51 e Å⁻³
9 restraints	Δρ_min = −0.41 e Å⁻³

Crystal data top

[Fe₃(C₂H₃O₂)₆O(H₂O)₃]NO₃·C₂H₄O₂	V = 2662.8 (12) Å³
M_r = 713.92	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 11.835 (3) Å	µ = 1.71 mm⁻¹
b = 14.755 (4) Å	T = 296 K
c = 15.250 (4) Å	0.18 × 0.13 × 0.10 mm
β = 90.851 (5)°

Data collection top

Bruker SMART CCD diffractometer	4953 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2001)	3355 reflections with I > 2σ(I)
T_min = 0.750, T_max = 0.848	R_int = 0.054
14072 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.044	9 restraints
wR(F²) = 0.106	H atoms treated by a mixture of independent and constrained refinement
S = 1.00	Δρ_max = 0.51 e Å⁻³
4953 reflections	Δρ_min = −0.41 e Å⁻³
378 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	0.40305 (4)	0.89656 (3)	0.62790 (3)	0.02692 (12)
Fe2	0.17864 (4)	0.76827 (3)	0.59152 (3)	0.02751 (12)
Fe3	0.16879 (4)	0.93399 (3)	0.73634 (3)	0.02779 (13)
O1W	0.5730 (2)	0.92274 (16)	0.59831 (17)	0.0390 (7)
O2W	0.1067 (2)	0.66185 (17)	0.51505 (18)	0.0536 (8)
O3W	0.0853 (2)	1.01043 (16)	0.82684 (16)	0.0414 (7)
O1	0.4549 (2)	0.76906 (16)	0.61642 (19)	0.0505 (8)
O2	0.30533 (19)	0.67883 (15)	0.61664 (16)	0.0373 (6)
O3	0.3729 (2)	0.90801 (17)	0.49476 (15)	0.0433 (7)
O4	0.2469 (2)	0.79746 (15)	0.47350 (15)	0.0375 (6)
O5	0.0995 (2)	0.71685 (15)	0.69403 (15)	0.0379 (6)
O6	0.0942 (2)	0.82725 (15)	0.79378 (16)	0.0461 (7)
O7	0.0395 (2)	0.84025 (16)	0.55730 (15)	0.0387 (7)
O8	0.03183 (19)	0.94965 (16)	0.65798 (16)	0.0406 (7)
O9	0.2290 (2)	1.05548 (15)	0.69826 (17)	0.0430 (7)
O10	0.38902 (19)	1.03126 (16)	0.62901 (17)	0.0456 (7)
O11	0.2928 (2)	0.92041 (18)	0.82695 (16)	0.0492 (8)
O12	0.4514 (2)	0.89345 (18)	0.75438 (16)	0.0481 (7)
O13	0.25047 (17)	0.86634 (13)	0.65078 (14)	0.0254 (5)
O17	0.1754 (3)	0.16154 (19)	0.9058 (2)	0.0782 (11)
O18	0.2920 (3)	0.26869 (19)	0.9325 (2)	0.0674 (9)
O14	0.7459 (2)	0.9001 (2)	0.9425 (2)	0.0738 (10)
H14	0.7698	0.8798	0.9893	0.111*
O15	0.9248 (2)	0.9381 (2)	0.92925 (19)	0.0637 (9)
C1	0.4856 (3)	0.6134 (2)	0.6411 (3)	0.0472 (11)
H1A	0.4414	0.5590	0.6445	0.071*
H1B	0.5258	0.6224	0.6956	0.071*
H1C	0.5386	0.6080	0.5943	0.071*
C2	0.4094 (3)	0.6923 (2)	0.6240 (2)	0.0302 (8)
C3	0.3290 (3)	0.8632 (3)	0.3488 (2)	0.0479 (11)
H3A	0.3837	0.9093	0.3361	0.072*
H3B	0.2576	0.8792	0.3225	0.072*
H3C	0.3539	0.8063	0.3256	0.072*
C4	0.3164 (3)	0.8553 (2)	0.4464 (2)	0.0305 (9)
C5	0.0056 (3)	0.6886 (3)	0.8275 (2)	0.0458 (11)
H5A	−0.0075	0.6307	0.8004	0.069*
H5B	−0.0655	0.7167	0.8400	0.069*
H5C	0.0478	0.6803	0.8811	0.069*
C6	0.0711 (3)	0.7479 (2)	0.7666 (2)	0.0317 (9)
C7	−0.1126 (3)	0.9443 (3)	0.5496 (3)	0.0476 (11)
H7A	−0.1380	0.9960	0.5820	0.071*
H7B	−0.1696	0.8980	0.5504	0.071*
H7C	−0.0987	0.9618	0.4901	0.071*
C8	−0.0058 (3)	0.9087 (2)	0.5905 (2)	0.0317 (9)
C9	0.3287 (3)	1.1823 (2)	0.6455 (3)	0.0512 (12)
H9A	0.3975	1.1935	0.6147	0.077*
H9B	0.3322	1.2118	0.7016	0.077*
H9C	0.2659	1.2056	0.6120	0.077*
C10	0.3142 (3)	1.0824 (2)	0.6584 (2)	0.0303 (9)
C11	0.4539 (3)	0.8788 (3)	0.9092 (2)	0.0487 (11)
H11A	0.4025	0.8865	0.9567	0.073*
H11B	0.5168	0.9193	0.9168	0.073*
H11C	0.4807	0.8174	0.9084	0.073*
C12	0.3942 (3)	0.8995 (2)	0.8241 (2)	0.0324 (9)
O16	0.1840 (3)	0.2745 (2)	0.8165 (2)	0.0802 (11)
N1	0.2187 (3)	0.2358 (2)	0.8830 (2)	0.0534 (10)
C13	0.7984 (4)	0.9702 (3)	0.8110 (3)	0.0624 (13)
H13A	0.7694	1.0306	0.8163	0.094*
H13B	0.7415	0.9318	0.7851	0.094*
H13C	0.8637	0.9707	0.7744	0.094*
C14	0.8301 (3)	0.9353 (3)	0.8986 (3)	0.0470 (11)
H3AW	0.0417 (12)	0.9921 (13)	0.8637 (11)	0.083 (16)*
H1AW	0.6123 (14)	0.8779 (8)	0.5921 (16)	0.048 (12)*
H3BW	0.1149 (16)	1.0579 (9)	0.8427 (17)	0.085 (16)*
H2AW	0.0434 (9)	0.6407 (19)	0.5202 (14)	0.106 (19)*
H2BW	0.122 (2)	0.667 (3)	0.4630 (7)	0.16 (3)*
H1BW	0.584 (3)	0.9594 (9)	0.5594 (11)	0.079 (16)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.0246 (3)	0.0245 (2)	0.0317 (3)	−0.0017 (2)	0.0026 (2)	−0.0008 (2)
Fe2	0.0289 (3)	0.0224 (2)	0.0313 (3)	−0.0028 (2)	0.0011 (2)	0.0004 (2)
Fe3	0.0276 (3)	0.0232 (2)	0.0327 (3)	−0.0019 (2)	0.0055 (2)	−0.0002 (2)
O1W	0.0293 (13)	0.0336 (13)	0.0542 (16)	0.0006 (11)	0.0079 (12)	0.0048 (12)
O2W	0.0598 (18)	0.0415 (16)	0.0590 (19)	−0.0159 (14)	−0.0129 (15)	−0.0030 (14)
O3W	0.0436 (15)	0.0338 (14)	0.0472 (15)	−0.0071 (12)	0.0163 (13)	−0.0110 (12)
O1	0.0332 (14)	0.0288 (13)	0.090 (2)	0.0000 (12)	0.0072 (14)	−0.0050 (14)
O2	0.0375 (14)	0.0235 (12)	0.0506 (15)	0.0018 (11)	−0.0025 (12)	−0.0014 (11)
O3	0.0430 (15)	0.0563 (16)	0.0306 (13)	−0.0180 (13)	0.0012 (12)	0.0004 (12)
O4	0.0425 (14)	0.0368 (13)	0.0333 (13)	−0.0113 (12)	0.0046 (11)	−0.0004 (11)
O5	0.0445 (15)	0.0337 (13)	0.0356 (14)	−0.0096 (12)	0.0077 (12)	0.0040 (11)
O6	0.0565 (16)	0.0293 (14)	0.0530 (16)	−0.0106 (12)	0.0223 (13)	0.0000 (12)
O7	0.0382 (14)	0.0376 (14)	0.0399 (14)	0.0067 (12)	−0.0069 (12)	−0.0032 (12)
O8	0.0323 (14)	0.0413 (14)	0.0482 (16)	0.0094 (12)	−0.0028 (12)	−0.0082 (12)
O9	0.0410 (15)	0.0247 (13)	0.0638 (17)	−0.0030 (11)	0.0204 (13)	0.0019 (12)
O10	0.0341 (14)	0.0250 (13)	0.0784 (19)	−0.0050 (11)	0.0198 (14)	−0.0003 (13)
O11	0.0411 (15)	0.0685 (18)	0.0376 (15)	0.0119 (14)	−0.0061 (13)	−0.0085 (13)
O12	0.0355 (14)	0.0763 (19)	0.0324 (14)	−0.0086 (14)	−0.0018 (12)	0.0012 (14)
O13	0.0236 (12)	0.0226 (11)	0.0303 (12)	−0.0007 (9)	0.0018 (10)	−0.0004 (10)
O17	0.116 (3)	0.0492 (18)	0.069 (2)	−0.0405 (18)	−0.019 (2)	0.0065 (16)
O18	0.0604 (19)	0.0547 (18)	0.087 (2)	−0.0155 (16)	−0.0065 (18)	0.0070 (17)
O14	0.0485 (18)	0.096 (2)	0.076 (2)	−0.0236 (18)	−0.0037 (16)	0.0325 (19)
O15	0.0425 (17)	0.089 (2)	0.0599 (19)	−0.0098 (16)	0.0070 (15)	0.0113 (17)
C1	0.050 (2)	0.038 (2)	0.053 (2)	0.0169 (19)	0.000 (2)	0.0056 (19)
C2	0.034 (2)	0.0310 (18)	0.0254 (18)	0.0068 (17)	0.0036 (15)	−0.0009 (15)
C3	0.053 (2)	0.060 (3)	0.031 (2)	−0.006 (2)	0.0001 (19)	0.0040 (19)
C4	0.0294 (19)	0.0318 (19)	0.0305 (19)	0.0023 (16)	0.0027 (16)	0.0025 (16)
C5	0.047 (2)	0.047 (2)	0.043 (2)	−0.017 (2)	0.0054 (19)	0.0111 (19)
C6	0.0297 (19)	0.0257 (19)	0.040 (2)	−0.0044 (15)	−0.0030 (16)	0.0085 (15)
C7	0.039 (2)	0.049 (2)	0.054 (3)	0.0014 (19)	−0.008 (2)	0.010 (2)
C8	0.0255 (18)	0.035 (2)	0.035 (2)	−0.0030 (16)	0.0037 (16)	0.0117 (17)
C9	0.046 (2)	0.032 (2)	0.076 (3)	−0.0016 (19)	0.013 (2)	0.010 (2)
C10	0.0274 (19)	0.0260 (18)	0.038 (2)	−0.0042 (15)	0.0007 (16)	0.0009 (15)
C11	0.054 (3)	0.050 (2)	0.041 (2)	−0.005 (2)	−0.008 (2)	0.0116 (19)
C12	0.040 (2)	0.0230 (17)	0.034 (2)	−0.0067 (16)	−0.0057 (17)	0.0055 (16)
O16	0.120 (3)	0.070 (2)	0.0502 (19)	−0.002 (2)	0.002 (2)	0.0049 (17)
N1	0.063 (2)	0.045 (2)	0.053 (2)	−0.0038 (19)	0.0088 (19)	−0.0055 (18)
C13	0.063 (3)	0.066 (3)	0.058 (3)	0.007 (3)	−0.001 (2)	0.006 (2)
C14	0.039 (2)	0.042 (2)	0.061 (3)	0.0000 (19)	0.005 (2)	0.001 (2)

Geometric parameters (Å, º) top

Fe1—O13	1.897 (2)	O12—C12	1.272 (4)
Fe1—O1	1.987 (2)	O17—N1	1.260 (4)
Fe1—O10	1.995 (2)	O18—N1	1.240 (4)
Fe1—O12	2.005 (3)	O14—C14	1.316 (4)
Fe1—O3	2.063 (2)	O14—H14	0.8200
Fe1—O1W	2.104 (2)	O15—C14	1.209 (5)
Fe2—O13	1.900 (2)	C1—C2	1.494 (5)
Fe2—O5	1.985 (2)	C1—H1A	0.9600
Fe2—O7	2.021 (2)	C1—H1B	0.9600
Fe2—O2	2.030 (2)	C1—H1C	0.9600
Fe2—O4	2.030 (2)	C3—C4	1.501 (5)
Fe2—O2W	2.126 (3)	C3—H3A	0.9600
Fe3—O13	1.916 (2)	C3—H3B	0.9600
Fe3—O11	2.011 (3)	C3—H3C	0.9600
Fe3—O6	2.013 (2)	C5—C6	1.500 (5)
Fe3—O8	2.013 (2)	C5—H5A	0.9600
Fe3—O9	2.017 (2)	C5—H5B	0.9600
Fe3—O3W	2.048 (2)	C5—H5C	0.9600
O1W—H1AW	0.815 (9)	C7—C8	1.497 (5)
O1W—H1BW	0.814 (9)	C7—H7A	0.9600
O2W—H2AW	0.816 (9)	C7—H7B	0.9600
O2W—H2BW	0.819 (9)	C7—H7C	0.9600
O3W—H3AW	0.816 (9)	C9—C10	1.497 (5)
O3W—H3BW	0.818 (9)	C9—H9A	0.9600
O1—C2	1.260 (4)	C9—H9B	0.9600
O2—C2	1.251 (4)	C9—H9C	0.9600
O3—C4	1.258 (4)	C11—C12	1.499 (5)
O4—C4	1.260 (4)	C11—H11A	0.9600
O5—C6	1.249 (4)	C11—H11B	0.9600
O6—C6	1.270 (4)	C11—H11C	0.9600
O7—C8	1.254 (4)	O16—N1	1.229 (5)
O8—C8	1.268 (4)	C13—C14	1.475 (6)
O9—C10	1.251 (4)	C13—H13A	0.9600
O10—C10	1.251 (4)	C13—H13B	0.9600
O11—C12	1.241 (4)	C13—H13C	0.9600

O13—Fe1—O1	95.13 (10)	Fe2—O13—Fe3	119.60 (11)
O13—Fe1—O10	98.80 (9)	C14—O14—H14	109.5
O1—Fe1—O10	165.92 (10)	C2—C1—H1A	109.5
O13—Fe1—O12	94.40 (10)	C2—C1—H1B	109.5
O1—Fe1—O12	88.79 (12)	H1A—C1—H1B	109.5
O10—Fe1—O12	92.13 (11)	C2—C1—H1C	109.5
O13—Fe1—O3	92.81 (9)	H1A—C1—H1C	109.5
O1—Fe1—O3	92.29 (11)	H1B—C1—H1C	109.5
O10—Fe1—O3	85.04 (11)	O2—C2—O1	123.8 (3)
O12—Fe1—O3	172.58 (10)	O2—C2—C1	118.9 (3)
O13—Fe1—O1W	176.56 (9)	O1—C2—C1	117.4 (3)
O1—Fe1—O1W	81.82 (10)	C4—C3—H3A	109.5
O10—Fe1—O1W	84.19 (9)	C4—C3—H3B	109.5
O12—Fe1—O1W	87.14 (10)	H3A—C3—H3B	109.5
O3—Fe1—O1W	85.75 (10)	C4—C3—H3C	109.5
O13—Fe2—O5	97.45 (9)	H3A—C3—H3C	109.5
O13—Fe2—O7	94.56 (9)	H3B—C3—H3C	109.5
O5—Fe2—O7	90.68 (10)	O3—C4—O4	124.8 (3)
O13—Fe2—O2	94.67 (9)	O3—C4—C3	118.2 (3)
O5—Fe2—O2	87.64 (10)	O4—C4—C3	117.0 (3)
O7—Fe2—O2	170.76 (10)	C6—C5—H5A	109.5
O13—Fe2—O4	94.54 (9)	C6—C5—H5B	109.5
O5—Fe2—O4	167.95 (10)	H5A—C5—H5B	109.5
O7—Fe2—O4	89.59 (10)	C6—C5—H5C	109.5
O2—Fe2—O4	90.17 (10)	H5A—C5—H5C	109.5
O13—Fe2—O2W	174.84 (10)	H5B—C5—H5C	109.5
O5—Fe2—O2W	87.69 (11)	O5—C6—O6	124.6 (3)
O7—Fe2—O2W	85.90 (10)	O5—C6—C5	118.9 (3)
O2—Fe2—O2W	84.95 (10)	O6—C6—C5	116.5 (3)
O4—Fe2—O2W	80.32 (10)	C8—C7—H7A	109.5
O13—Fe3—O11	92.62 (10)	C8—C7—H7B	109.5
O13—Fe3—O6	96.76 (9)	H7A—C7—H7B	109.5
O11—Fe3—O6	86.74 (11)	C8—C7—H7C	109.5
O13—Fe3—O8	93.76 (10)	H7A—C7—H7C	109.5
O11—Fe3—O8	173.00 (10)	H7B—C7—H7C	109.5
O6—Fe3—O8	89.64 (11)	O7—C8—O8	124.4 (3)
O13—Fe3—O9	94.77 (9)	O7—C8—C7	118.5 (3)
O11—Fe3—O9	91.68 (11)	O8—C8—C7	117.1 (3)
O6—Fe3—O9	168.42 (10)	C10—C9—H9A	109.5
O8—Fe3—O9	90.67 (10)	C10—C9—H9B	109.5
O13—Fe3—O3W	177.83 (10)	H9A—C9—H9B	109.5
O11—Fe3—O3W	86.91 (10)	C10—C9—H9C	109.5
O6—Fe3—O3W	85.33 (10)	H9A—C9—H9C	109.5
O8—Fe3—O3W	86.82 (10)	H9B—C9—H9C	109.5
O9—Fe3—O3W	83.13 (10)	O9—C10—O10	124.3 (3)
Fe1—O1W—H1AW	115.2 (13)	O9—C10—C9	118.1 (3)
Fe1—O1W—H1BW	116 (2)	O10—C10—C9	117.6 (3)
H1AW—O1W—H1BW	111.0 (16)	C12—C11—H11A	109.5
Fe2—O2W—H2AW	126.2 (19)	C12—C11—H11B	109.5
Fe2—O2W—H2BW	112 (3)	H11A—C11—H11B	109.5
H2AW—O2W—H2BW	109.8 (15)	C12—C11—H11C	109.5
Fe3—O3W—H3AW	126.8 (15)	H11A—C11—H11C	109.5
Fe3—O3W—H3BW	117.5 (16)	H11B—C11—H11C	109.5
H3AW—O3W—H3BW	110.7 (16)	O11—C12—O12	125.1 (3)
C2—O1—Fe1	135.3 (2)	O11—C12—C11	117.6 (3)
C2—O2—Fe2	129.6 (2)	O12—C12—C11	117.3 (3)
C4—O3—Fe1	127.6 (2)	O16—N1—O18	122.8 (4)
C4—O4—Fe2	134.9 (2)	O16—N1—O17	119.9 (4)
C6—O5—Fe2	134.0 (2)	O18—N1—O17	117.2 (4)
C6—O6—Fe3	132.3 (2)	C14—C13—H13A	109.5
C8—O7—Fe2	132.1 (2)	C14—C13—H13B	109.5
C8—O8—Fe3	134.2 (2)	H13A—C13—H13B	109.5
C10—O9—Fe3	135.5 (2)	C14—C13—H13C	109.5
C10—O10—Fe1	131.6 (2)	H13A—C13—H13C	109.5
C12—O11—Fe3	134.2 (2)	H13B—C13—H13C	109.5
C12—O12—Fe1	130.9 (2)	O15—C14—O14	121.4 (4)
Fe1—O13—Fe2	120.78 (11)	O15—C14—C13	124.1 (4)
Fe1—O13—Fe3	119.60 (11)	O14—C14—C13	114.5 (4)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O14—H14···O17ⁱ	0.82	1.82	2.642 (4)	178
O3W—H3AW···O15ⁱⁱ	0.82 (1)	1.89 (1)	2.697 (4)	168 (2)
O1W—H1AW···O18ⁱⁱⁱ	0.82 (1)	2.01 (1)	2.821 (4)	176 (2)
O3W—H3BW···O17^iv	0.82 (1)	1.94 (1)	2.742 (4)	167 (3)
O2W—H2AW···O15^v	0.82 (1)	2.28 (2)	2.904 (4)	134 (2)
O1W—H1BW···O3^vi	0.81 (1)	2.19 (1)	2.948 (3)	155 (2)

Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) x−1, y, z; (iii) −x+1, y+1/2, −z+3/2; (iv) x, y+1, z; (v) x−1, −y+3/2, z−1/2; (vi) −x+1, −y+2, −z+1.

Experimental details

Crystal data
Chemical formula	[Fe₃(C₂H₃O₂)₆O(H₂O)₃]NO₃·C₂H₄O₂
M_r	713.92
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	296
a, b, c (Å)	11.835 (3), 14.755 (4), 15.250 (4)
β (°)	90.851 (5)
V (Å³)	2662.8 (12)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.71
Crystal size (mm)	0.18 × 0.13 × 0.10

Data collection
Diffractometer	Bruker SMART CCD diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2001)
T_min, T_max	0.750, 0.848
No. of measured, independent and observed [I > 2σ(I)] reflections	14072, 4953, 3355
R_int	0.054
(sin θ/λ)_max (Å⁻¹)	0.606

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.044, 0.106, 1.00
No. of reflections	4953
No. of parameters	378
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)	0.51, −0.41

Computer programs: SMART (Bruker, 2001), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2003).

Selected bond lengths (Å) top

Fe1—O13	1.897 (2)	Fe2—O2	2.030 (2)
Fe1—O1	1.987 (2)	Fe2—O4	2.030 (2)
Fe1—O10	1.995 (2)	Fe2—O2W	2.126 (3)
Fe1—O12	2.005 (3)	Fe3—O13	1.916 (2)
Fe1—O3	2.063 (2)	Fe3—O11	2.011 (3)
Fe1—O1W	2.104 (2)	Fe3—O6	2.013 (2)
Fe2—O13	1.900 (2)	Fe3—O8	2.013 (2)
Fe2—O5	1.985 (2)	Fe3—O9	2.017 (2)
Fe2—O7	2.021 (2)	Fe3—O3W	2.048 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O14—H14···O17ⁱ	0.82	1.82	2.642 (4)	178
O3W—H3AW···O15ⁱⁱ	0.816 (9)	1.894 (9)	2.697 (4)	168 (2)
O1W—H1AW···O18ⁱⁱⁱ	0.815 (9)	2.008 (10)	2.821 (4)	176 (2)
O3W—H3BW···O17^iv	0.818 (9)	1.938 (13)	2.742 (4)	167 (3)
O2W—H2AW···O15^v	0.816 (9)	2.28 (2)	2.904 (4)	134 (2)
O1W—H1BW···O3^vi	0.814 (9)	2.188 (12)	2.948 (3)	155 (2)

Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) x−1, y, z; (iii) −x+1, y+1/2, −z+3/2; (iv) x, y+1, z; (v) x−1, −y+3/2, z−1/2; (vi) −x+1, −y+2, −z+1.

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