Literature DB >> 21582083

Di-μ-hydroxido-bis-({2,2'-[propane-1,3-diylbis(nitrilo-methyl-idyne)]diphenolato}iron(III)) dimethyl-formamide disolvate.

Abstract

The structure of the title compound, [Fe(2)(C(17)H(16)N(2)O(2))(2)(OH)(2)]·2C(3)H(7)N, 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-FeN(2)O(4) octa-hedral geometry.

Entities: Chemical Disease Gene

Year: 2009 PMID： 21582083 PMCID： PMC2968628 DOI： 10.1107/S1600536809005091

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

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 = 852.54 Monoclinic, 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[F 2 > 2σ(F 2)] = 0.046 wR(F 2) = 0.143 S = 1.04 3221 reflections 253 parameters H-atom parameters constrained Δρmax = 0.48 e Å−3 Δρmin = −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. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809005091/hg2478sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809005091/hg2478Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[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

Bruker APEXII CCD area-detector diffractometer	3221 independent reflections
Radiation source: fine-focus sealed tube	2809 reflections with I > 2σ(I)
graphite	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 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

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.

	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*

	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)

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

2 in total

1. A short history of SHELX.

Authors: George M Sheldrick
Journal: Acta Crystallogr A Date: 2007-12-21 Impact factor: 2.290

2. Antiferromagnetic FeIII6 ring and single-molecule magnet MnII3MnIII4 wheel.

Authors: Satoshi Koizumi; Masayuki Nihei; Motohiro Nakano; Hiroki Oshio
Journal: Inorg Chem Date: 2005-03-07 Impact factor: 5.165

2 in total