Di-μ-hydroxido-bis­({2,2′-[propane-1,3-diylbis(nitrilo­methyl­idyne)]diphenolato}iron(III)) dimethyl­formamide disolvate

Liu, Q.; Pan, S.; Wang, D.

doi:10.1107/S1600536809005091

metal-organic compounds

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Volume 65| Part 3| March 2009| Page m305

doi:10.1107/S1600536809005091

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Di-μ-hydroxido-bis({2,2′-[propane-1,3-diylbis(nitrilomethylidyne)]diphenolato}iron(III)) dimethylformamide disolvate

Qingyun Liu,^a ^* Shuying Pan ^b and Dongmei Wang ^a

^aSchool of Chemical & Environmental Engineering, Shandong University of Science and Technology, Qingdao 266510, People's Republic of China, and ^bSoil and Fertilizer General Monitoring Station of Shandong Province, Jinan 250100, People's Republic of China
^*Correspondence e-mail: qyliusdu@163.com

(Received 11 February 2009; accepted 12 February 2009; online 21 February 2009)

The structure of the title compound, [Fe₂(C₁₇H₁₆N₂O₂)₂(OH)₂]·2C₃H₇N, consists of centrosymmetric dimeric units in which crystallographically equivalent Fe^III ions are doubly bridged by hydroxide groups. Each Fe^III center in the complex has a six-coordinated distorted cis-FeN₂O₄ octahedral geometry.

Related literature

For background to the use of Schiff base ligands in the assembly of hydroxo-, alkoxo- or phenoxo-bridged clusters and polymers, see: Chen et al. (2006 ); Koizumi et al. (2005 ); Ni & Wang (2007 ). For the use of H₂salpn as a flexible ligand, see: Ni et al. (2005 ); Si et al. (2002 ).

Experimental

Crystal data

[Fe₂(C₁₇H₁₆N₂O₂)₂(OH)₂]·2C₃H₇N
M_r = 852.54
Monoclinic, P 2₁ /c
a = 10.768 (2) Å
b = 10.136 (2) Å
c = 17.540 (4) Å
β = 101.27 (3)°
V = 1877.5 (7) Å³
Z = 2
Mo Kα radiation
μ = 0.84 mm⁻¹
T = 293 K
0.21 × 0.15 × 0.12 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2003 ) T_min = 0.862, T_max = 0.908
10664 measured reflections
3221 independent reflections
2809 reflections with I > 2σ(I)
R_int = 0.038

Refinement

R[F² > 2σ(F²)] = 0.046
wR(F²) = 0.143
S = 1.04
3221 reflections
253 parameters
H-atom parameters constrained
Δρ_max = 0.48 e Å⁻³
Δρ_min = −0.65 e Å⁻³

Data collection: APEX2 (Bruker, 2004 ); cell refinement: SAINT-Plus (Bruker, 2001 ); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: XP in SHELXTL.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809005091/hg2478sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809005091/hg2478Isup2.hkl

checkCIF report

Comment top

Recently, the the Schiff base ligands, especially the relative flexible symmetrical or unsymmetrical Schiff base ligands and their hydrogenerated derivatives have been widely employed to assembly hydroxo-, alkoxo- or phenoxo-bridged clusters and polymers with novel topological structures and interesting magnetic, catalysis and photochemical properties (Chen et al., 2006; Koizumi et al., 2005; Ni & Wang, 2007). Among Schiff base ligands, H₂salpn is a special symmetrical tetradentate Schiff base which can be used as rigid ligand located on the equatorial plane of central metal ion. However, sometimes it also exhibits characteristics of a flexible ligand situated at the terminal of metal ions like a cap. To date, several examples in which H₂salpn is used as flexible ligand have been synthesized (Ni et al., 2005; Si et al., 2002) We recently synthesized a doubly hydroxo-bridged Fe^III dimeric complex where Schiff base H₂salpn exist as flexible terminal ligand with two free DMF solvate molecules, Herein, we reported the synthesis and crystal structure of the complex [Fe^III(salpn)OH]₂.2DMF (I).

The geometry and labeling scheme for the crystal structure of [Fe^III(salpn)OH]₂.2DMF (I) is depicted in Figure 1. The structure of I consists of centrosymmetric dimer units in which crystallographically equivalent iron(III) ions are doubly bridged by hydroxo groups. The ligand with N₂O₂ donating atoms occupies four coordination sites of the Fe^III ion while the two remaining ones are filled by the bridging hydroxo groups. The Fe^III ions have a slightly distorted-octahedral coordination geometry. The four coordination atoms from salpn^2- are not in a plane for distortion of carbon linkage and the requirement of coordination of hydroxo-bridging groups from the same side to take cis-disposition. The two Fe—O bond distances in the bridging unit are 1.8158 (18) and 1.8172 (18) Å, respectively.

Related literature top

For background to the use of Schiff base ligands in the assembly of hydroxo-, alkoxo- or phenoxo-bridged clusters and polymers with novel topological structures and interesting magnetic, catalytic and photochemical properties, see: Chen et al. (2006); Koizumi et al. (2005); Ni & Wang (2007). For the use of H₂salpn as a flexible ligand, see: Ni et al. (2005); Si et al. (2002).

Experimental top

Ligand H₂salpn (0.5 mmol) was added to a solution of Fe(ClO₄)₂.4H₂O (0.5 mmol) in MeOH and DMF mixing solvent (1/1, v/v). The mixture was stirred for about four hours, and then filtered. The filrate was evaporated in room temperature for two days yielding red brown single-crystals. Yield: 30%. Elemental analysis [found (calculated)] for C₄₀H₄₈Fe₂N₆O₈: C 56.08 (56.35), H 5.45 (5.67), N 9.80 (9.86%).

Computing details top

Data collection: APEX2 (Bruker, 2004); 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: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: XP in SHELXTL (Sheldrick, 2008).

Figures top

Fig. 1. A view of (I) with the unique atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level.

Di-µ-hydroxido-bis({2,2'-[propane-1,3- diylbis(nitrilomethylidyne)]diphenolato}iron(III)) dimethylformamide disolvate top

Crystal data top

[Fe₂(C₁₇H₁₆N₂O₂)₂(OH)₂]·2C₃H₇N	F(000) = 892
M_r = 852.54	D_x = 1.508 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 221 reflections
a = 10.768 (2) Å	θ = 3.1–25.0°
b = 10.136 (2) Å	µ = 0.84 mm⁻¹
c = 17.540 (4) Å	T = 293 K
β = 101.27 (3)°	Block, brown
V = 1877.5 (7) Å³	0.21 × 0.15 × 0.12 mm
Z = 2

Data collection top

Bruker APEXII CCD area-detector diffractometer	3221 independent reflections
Radiation source: fine-focus sealed tube	2809 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.038
ϕ and ω scans	θ_max = 25.0°, θ_min = 3.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −12→12
T_min = 0.862, T_max = 0.908	k = −12→11
10664 measured reflections	l = −20→20

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)] = 0.046	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.143	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0957P)² + 1.7319P] where P = (F_o² + 2F_c²)/3
3221 reflections	(Δ/σ)_max = 0.001
253 parameters	Δρ_max = 0.48 e Å⁻³
0 restraints	Δρ_min = −0.65 e Å⁻³

Crystal data top

[Fe₂(C₁₇H₁₆N₂O₂)₂(OH)₂]·2C₃H₇N	V = 1877.5 (7) Å³
M_r = 852.54	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 10.768 (2) Å	µ = 0.84 mm⁻¹
b = 10.136 (2) Å	T = 293 K
c = 17.540 (4) Å	0.21 × 0.15 × 0.12 mm
β = 101.27 (3)°

Data collection top

Bruker APEXII CCD area-detector diffractometer	3221 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	2809 reflections with I > 2σ(I)
T_min = 0.862, T_max = 0.908	R_int = 0.038
10664 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.046	0 restraints
wR(F²) = 0.143	H-atom parameters constrained
S = 1.04	Δρ_max = 0.48 e Å⁻³
3221 reflections	Δρ_min = −0.65 e Å⁻³
253 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	0.50501 (4)	0.37734 (4)	0.03284 (2)	0.01386 (19)
O1	0.54651 (17)	0.43569 (19)	0.13793 (11)	0.0140 (4)
O2	0.63819 (18)	0.24760 (19)	0.05879 (11)	0.0148 (4)
O3	0.39002 (17)	0.50795 (18)	0.00288 (10)	0.0127 (4)
H3B	0.3390	0.5576	0.0209	0.015*
O4	0.9440 (2)	0.6587 (3)	0.27864 (14)	0.0360 (6)
N1	0.3654 (2)	0.2624 (2)	0.06536 (13)	0.0135 (5)
N2	0.4579 (2)	0.2834 (2)	−0.07001 (13)	0.0128 (5)
N3	0.9331 (2)	0.5320 (3)	0.16973 (15)	0.0251 (6)
C1	0.4628 (3)	0.4666 (3)	0.18093 (15)	0.0131 (6)
C2	0.4952 (3)	0.5623 (3)	0.24001 (17)	0.0186 (6)
H2A	0.5754	0.6002	0.2486	0.022*
C3	0.4098 (3)	0.6008 (3)	0.28532 (18)	0.0216 (7)
H3A	0.4322	0.6665	0.3225	0.026*
C4	0.2905 (3)	0.5423 (3)	0.27608 (17)	0.0213 (7)
H4A	0.2329	0.5701	0.3059	0.026*
C5	0.2586 (3)	0.4420 (3)	0.22176 (17)	0.0206 (7)
H5A	0.1811	0.3993	0.2173	0.025*
C6	0.3431 (3)	0.4043 (3)	0.17312 (17)	0.0152 (6)
C7	0.3077 (3)	0.2952 (3)	0.12009 (16)	0.0156 (6)
H7A	0.2379	0.2451	0.1261	0.019*
C8	0.3228 (3)	0.1439 (3)	0.01922 (18)	0.0190 (6)
H8A	0.2676	0.0928	0.0454	0.023*
H8B	0.3957	0.0897	0.0156	0.023*
C9	0.2526 (3)	0.1786 (3)	−0.06223 (17)	0.0231 (7)
H9A	0.1701	0.2139	−0.0589	0.028*
H9B	0.2391	0.0985	−0.0930	0.028*
C10	0.3225 (3)	0.2798 (3)	−0.10456 (17)	0.0170 (6)
H10A	0.3116	0.2562	−0.1591	0.020*
H10B	0.2861	0.3666	−0.1013	0.020*
C11	0.5369 (3)	0.2250 (3)	−0.10447 (16)	0.0146 (6)
H11A	0.5069	0.1928	−0.1543	0.018*
C12	0.6696 (3)	0.2055 (3)	−0.07143 (17)	0.0149 (6)
C13	0.7523 (3)	0.1622 (3)	−0.11903 (18)	0.0199 (6)
H13A	0.7222	0.1542	−0.1723	0.024*
C14	0.8760 (3)	0.1314 (3)	−0.0891 (2)	0.0236 (7)
H14A	0.9297	0.1035	−0.1215	0.028*
C15	0.9204 (3)	0.1426 (3)	−0.00837 (19)	0.0209 (7)
H15A	1.0046	0.1232	0.0124	0.025*
C16	0.8409 (3)	0.1821 (3)	0.04073 (17)	0.0172 (6)
H16A	0.8718	0.1870	0.0940	0.021*
C17	0.7135 (3)	0.2150 (3)	0.01030 (17)	0.0146 (6)
C18	0.9718 (3)	0.6354 (3)	0.2146 (2)	0.0293 (8)
H18A	1.0243	0.6957	0.1964	0.035*
C19	0.8528 (3)	0.4313 (3)	0.1945 (2)	0.0289 (7)
H19A	0.8366	0.4537	0.2448	0.043*
H19B	0.8948	0.3474	0.1971	0.043*
H19C	0.7741	0.4264	0.1578	0.043*
C20	0.9676 (4)	0.5132 (4)	0.0947 (2)	0.0354 (8)
H20A	1.0208	0.5846	0.0847	0.053*
H20B	0.8924	0.5111	0.0549	0.053*
H20C	1.0125	0.4314	0.0946	0.053*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.0147 (3)	0.0133 (3)	0.0142 (3)	0.00014 (14)	0.00425 (18)	0.00012 (15)
O1	0.0146 (10)	0.0165 (10)	0.0118 (10)	0.0006 (7)	0.0051 (8)	−0.0002 (8)
O2	0.0164 (10)	0.0152 (10)	0.0140 (10)	0.0044 (8)	0.0055 (8)	0.0018 (8)
O3	0.0124 (10)	0.0121 (9)	0.0149 (11)	0.0020 (7)	0.0056 (7)	0.0010 (8)
O4	0.0397 (15)	0.0405 (14)	0.0263 (14)	−0.0019 (12)	0.0025 (11)	−0.0087 (11)
N1	0.0130 (11)	0.0143 (12)	0.0130 (12)	−0.0004 (9)	0.0021 (9)	0.0018 (9)
N2	0.0134 (12)	0.0112 (11)	0.0139 (12)	−0.0014 (8)	0.0029 (9)	0.0008 (9)
N3	0.0229 (14)	0.0270 (15)	0.0244 (15)	0.0009 (11)	0.0022 (11)	0.0015 (11)
C1	0.0159 (14)	0.0142 (14)	0.0089 (14)	0.0031 (10)	0.0017 (11)	0.0045 (11)
C2	0.0246 (15)	0.0183 (15)	0.0134 (15)	−0.0006 (12)	0.0046 (12)	0.0006 (12)
C3	0.0320 (18)	0.0206 (15)	0.0130 (16)	0.0014 (12)	0.0066 (13)	−0.0017 (12)
C4	0.0264 (16)	0.0239 (16)	0.0167 (16)	0.0065 (12)	0.0118 (13)	0.0009 (12)
C5	0.0198 (15)	0.0237 (16)	0.0204 (16)	0.0039 (12)	0.0093 (12)	0.0028 (13)
C6	0.0167 (14)	0.0174 (14)	0.0119 (15)	0.0020 (11)	0.0039 (11)	0.0032 (11)
C7	0.0137 (13)	0.0146 (14)	0.0196 (15)	0.0009 (10)	0.0056 (11)	0.0047 (11)
C8	0.0193 (15)	0.0140 (14)	0.0260 (17)	−0.0047 (11)	0.0102 (13)	−0.0008 (12)
C9	0.0217 (16)	0.0279 (17)	0.0207 (16)	−0.0119 (13)	0.0069 (13)	−0.0075 (13)
C10	0.0154 (14)	0.0169 (15)	0.0174 (15)	−0.0032 (11)	0.0001 (11)	−0.0018 (12)
C11	0.0235 (15)	0.0098 (13)	0.0112 (14)	−0.0026 (11)	0.0051 (11)	0.0007 (11)
C12	0.0198 (14)	0.0099 (13)	0.0165 (15)	0.0010 (10)	0.0075 (11)	0.0019 (11)
C13	0.0243 (16)	0.0184 (14)	0.0188 (16)	0.0003 (12)	0.0088 (12)	0.0000 (12)
C14	0.0219 (16)	0.0235 (17)	0.0309 (19)	0.0037 (12)	0.0184 (14)	0.0025 (13)
C15	0.0142 (14)	0.0189 (15)	0.0306 (18)	0.0020 (11)	0.0070 (13)	0.0021 (13)
C16	0.0191 (15)	0.0157 (15)	0.0176 (15)	−0.0018 (11)	0.0057 (12)	0.0015 (12)
C17	0.0175 (14)	0.0075 (13)	0.0198 (16)	0.0008 (10)	0.0056 (12)	0.0025 (11)
C18	0.0253 (17)	0.0283 (18)	0.032 (2)	−0.0040 (13)	−0.0003 (15)	0.0003 (14)
C19	0.0254 (17)	0.0279 (17)	0.033 (2)	−0.0028 (14)	0.0044 (14)	0.0001 (15)
C20	0.037 (2)	0.039 (2)	0.031 (2)	0.0001 (16)	0.0084 (15)	−0.0057 (16)

Geometric parameters (Å, º) top

Fe1—O3ⁱ	1.8163 (18)	C6—C7	1.447 (4)
Fe1—O3	1.8186 (19)	C7—H7A	0.9300
Fe1—O1	1.9040 (19)	C8—C9	1.521 (4)
Fe1—O2	1.9334 (19)	C8—H8A	0.9700
Fe1—N2	2.015 (2)	C8—H8B	0.9700
Fe1—N1	2.069 (2)	C9—C10	1.546 (4)
Fe1—Fe1ⁱ	2.7337 (9)	C9—H9A	0.9700
O1—C1	1.321 (3)	C9—H9B	0.9700
O2—C17	1.327 (3)	C10—H10A	0.9700
O3—Fe1ⁱ	1.8163 (18)	C10—H10B	0.9700
O3—H3B	0.8500	C11—C12	1.447 (4)
O4—C18	1.241 (4)	C11—H11A	0.9300
N1—C7	1.285 (4)	C12—C13	1.405 (4)
N1—C8	1.471 (4)	C12—C17	1.422 (4)
N2—C11	1.281 (4)	C13—C14	1.369 (4)
N2—C10	1.465 (4)	C13—H13A	0.9300
N3—C18	1.328 (4)	C14—C15	1.407 (5)
N3—C20	1.449 (4)	C14—H14A	0.9300
N3—C19	1.458 (4)	C15—C16	1.386 (4)
C1—C2	1.412 (4)	C15—H15A	0.9300
C1—C6	1.417 (4)	C16—C17	1.412 (4)
C2—C3	1.384 (4)	C16—H16A	0.9300
C2—H2A	0.9300	C18—H18A	0.9300
C3—C4	1.395 (5)	C19—H19A	0.9600
C3—H3A	0.9300	C19—H19B	0.9600
C4—C5	1.389 (4)	C19—H19C	0.9600
C4—H4A	0.9300	C20—H20A	0.9600
C5—C6	1.416 (4)	C20—H20B	0.9600
C5—H5A	0.9300	C20—H20C	0.9600

O3ⁱ—Fe1—O3	82.46 (9)	C6—C7—H7A	117.5
O3ⁱ—Fe1—O1	95.22 (8)	N1—C8—C9	111.9 (2)
O3—Fe1—O1	94.09 (8)	N1—C8—H8A	109.2
O3ⁱ—Fe1—O2	91.93 (8)	C9—C8—H8A	109.2
O3—Fe1—O2	174.23 (8)	N1—C8—H8B	109.2
O1—Fe1—O2	87.73 (9)	C9—C8—H8B	109.2
O3ⁱ—Fe1—N2	93.36 (9)	H8A—C8—H8B	107.9
O3—Fe1—N2	92.70 (9)	C8—C9—C10	113.9 (2)
O1—Fe1—N2	169.68 (9)	C8—C9—H9A	108.8
O2—Fe1—N2	86.26 (9)	C10—C9—H9A	108.8
O3ⁱ—Fe1—N1	172.13 (9)	C8—C9—H9B	108.8
O3—Fe1—N1	89.95 (9)	C10—C9—H9B	108.8
O1—Fe1—N1	87.35 (9)	H9A—C9—H9B	107.7
O2—Fe1—N1	95.61 (9)	N2—C10—C9	110.9 (2)
N2—Fe1—N1	84.90 (9)	N2—C10—H10A	109.5
O3ⁱ—Fe1—Fe1ⁱ	41.26 (6)	C9—C10—H10A	109.5
O3—Fe1—Fe1ⁱ	41.20 (6)	N2—C10—H10B	109.5
O1—Fe1—Fe1ⁱ	96.19 (6)	C9—C10—H10B	109.5
O2—Fe1—Fe1ⁱ	133.18 (6)	H10A—C10—H10B	108.0
N2—Fe1—Fe1ⁱ	94.03 (7)	N2—C11—C12	124.7 (3)
N1—Fe1—Fe1ⁱ	131.11 (7)	N2—C11—H11A	117.6
C1—O1—Fe1	124.69 (17)	C12—C11—H11A	117.6
C17—O2—Fe1	122.47 (17)	C13—C12—C17	119.7 (3)
Fe1ⁱ—O3—Fe1	97.54 (9)	C13—C12—C11	119.7 (3)
Fe1ⁱ—O3—H3B	103.9	C17—C12—C11	120.1 (2)
Fe1—O3—H3B	140.9	C14—C13—C12	121.7 (3)
C7—N1—C8	118.6 (2)	C14—C13—H13A	119.2
C7—N1—Fe1	122.95 (19)	C12—C13—H13A	119.2
C8—N1—Fe1	118.25 (17)	C13—C14—C15	118.8 (3)
C11—N2—C10	119.5 (2)	C13—C14—H14A	120.6
C11—N2—Fe1	124.5 (2)	C15—C14—H14A	120.6
C10—N2—Fe1	115.99 (17)	C16—C15—C14	121.2 (3)
C18—N3—C20	122.4 (3)	C16—C15—H15A	119.4
C18—N3—C19	120.8 (3)	C14—C15—H15A	119.4
C20—N3—C19	116.8 (3)	C15—C16—C17	120.4 (3)
O1—C1—C2	118.9 (2)	C15—C16—H16A	119.8
O1—C1—C6	123.2 (3)	C17—C16—H16A	119.8
C2—C1—C6	117.8 (2)	O2—C17—C16	119.2 (3)
C3—C2—C1	121.2 (3)	O2—C17—C12	122.6 (2)
C3—C2—H2A	119.4	C16—C17—C12	118.2 (2)
C1—C2—H2A	119.4	O4—C18—N3	125.7 (3)
C2—C3—C4	120.9 (3)	O4—C18—H18A	117.1
C2—C3—H3A	119.5	N3—C18—H18A	117.1
C4—C3—H3A	119.5	N3—C19—H19A	109.5
C3—C4—C5	119.2 (3)	N3—C19—H19B	109.5
C3—C4—H4A	120.4	H19A—C19—H19B	109.5
C5—C4—H4A	120.4	N3—C19—H19C	109.5
C4—C5—C6	120.6 (3)	H19A—C19—H19C	109.5
C4—C5—H5A	119.7	H19B—C19—H19C	109.5
C6—C5—H5A	119.7	N3—C20—H20A	109.5
C1—C6—C5	120.0 (3)	N3—C20—H20B	109.5
C1—C6—C7	121.6 (2)	H20A—C20—H20B	109.5
C5—C6—C7	118.3 (3)	N3—C20—H20C	109.5
N1—C7—C6	124.9 (3)	H20A—C20—H20C	109.5
N1—C7—H7A	117.5	H20B—C20—H20C	109.5

Symmetry code: (i) −x+1, −y+1, −z.

Experimental details

Crystal data
Chemical formula	[Fe₂(C₁₇H₁₆N₂O₂)₂(OH)₂]·2C₃H₇N
M_r	852.54
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	10.768 (2), 10.136 (2), 17.540 (4)
β (°)	101.27 (3)
V (Å³)	1877.5 (7)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.84
Crystal size (mm)	0.21 × 0.15 × 0.12

Data collection
Diffractometer	Bruker APEXII CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2003)
T_min, T_max	0.862, 0.908
No. of measured, independent and observed [I > 2σ(I)] reflections	10664, 3221, 2809
R_int	0.038
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.046, 0.143, 1.04
No. of reflections	3221
No. of parameters	253
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.48, −0.65

Computer programs: APEX2 (Bruker, 2004), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008).

Acknowledgements

This work was supported by the Science Foundation of Shandong Provincial Education Department, China.

References

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