Tri­ethano­laminate iron perchlorate revisited: change of space group, chemical composition and oxidation states in [Fe7(tea)3(tea-H)3](ClO4)2 (tea-H3 is tri­ethano­lamine)

Horn, J.A. van der; Lutz, M.

doi:10.1107/S2053229617018460

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Triethanolaminate iron perchlorate revisited: change of space group, chemical composition and oxidation states in [Fe₇(tea)₃(tea-H)₃](ClO₄)₂ (tea-H₃ is triethanolamine)

J. A. van der Horn and M. Lutz

The X-ray crystal structure of tris[N-(2-hydroxyethyl)-2,2′-iminodiethanolato]tris(2,2′,2′′-nitrilotriethanolato)tetrairon(II)triiron(III) bis(perchlorate), [Fe₇(C₆H₁₂NO₃)₃(C₆H₁₃NO₃)₃](ClO₄)₂ or [Fe₇(tea)₃(tea-H)₃](ClO₄)₂ (tea-H₃ is triethanolamine), is known from the literature [Liu et al. (2008). Z. Anorg. Allg. Chem. 634, 778–783] as a heptanuclear coordination cluster. The space group was given as I2₁3 and is reinvestigated in the present study. We find a new space-group symmetry of Pa $\overline{3}$ and could detect O—H hydrogens, which were missing in the original publication. Consequences on the Fe oxidation states are investigated with the bond-valence method, resulting in a mixed-valence core of four Fe^II and three Fe^III centres. Symmetry relationships between the two space groups and the average supergroup Ia $\overline{3}$ are discussed in detail.

Keywords: heptanuclear mixed-valence coordination cluster; pseudosymmetry; iron oxidation state; validation; crystal structure.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229617018460/qf3003sup1.cif Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S2053229617018460/qf3003Isup2.hkl Contains datablock I

CCDC reference: 1813756

Computing details top

Data collection: APEX3 (Bruker, 2016); cell refinement: PEAKREF (Schreurs, 2016); data reduction: EVAL15 (Schreurs et al., 2010) and SADABS (Sheldrick, 2014); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2017 (Sheldrick, 2015b); molecular graphics: PLATON (Spek, 2009); software used to prepare material for publication: publCIF (Westrip, 2010).

Tris[N-(2-hydroxyethyl)-2,2'-iminodiiethanolato]tris(2,2',2''-\ nitrilotriethanolato)tetrairon(II)triiron(III) bis(perchlorate) top

Crystal data top

[Fe₇(C₆H₁₂NO₃)₃(C₆H₁₃NO₃)₃](ClO₄)₂	Mo Kα radiation, λ = 0.71073 Å
M_r = 1469.87	Cell parameters from 104201 reflections
Cubic, Pa3	θ = 1.3–35.1°
a = 22.0884 (6) Å	µ = 2.02 mm⁻¹
V = 10776.9 (8) Å³	T = 100 K
Z = 8	Block, black
F(000) = 6056	0.22 × 0.09 × 0.08 mm
D_x = 1.812 Mg m⁻³

Data collection top

Bruker Kappa APEXII diffractometer	6121 reflections with I > 2σ(I)
Radiation source: sealed tube	R_int = 0.055
φ and ω scans	θ_max = 35.1°, θ_min = 1.6°
Absorption correction: numerical (SADABS; Sheldrick, 2014)	h = −35→30
T_min = 0.687, T_max = 0.887	k = −34→35
211368 measured reflections	l = −33→31
7962 independent reflections

Refinement top

Refinement on F²	Primary atom site location: dual
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.028	Hydrogen site location: difference Fourier map
wR(F²) = 0.070	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	w = 1/[σ²(F_o²) + (0.0318P)² + 4.712P] where P = (F_o² + 2F_c²)/3
7962 reflections	(Δ/σ)_max = 0.002
236 parameters	Δρ_max = 0.67 e Å⁻³
0 restraints	Δρ_min = −0.47 e Å⁻³

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe1	0.25330 (2)	0.25330 (2)	0.25330 (2)	0.00791 (5)
Fe2	0.22069 (2)	0.16731 (2)	0.36722 (2)	0.00893 (4)
Fe3	0.33830 (2)	0.13764 (2)	0.28373 (2)	0.00842 (4)
O1	0.17204 (4)	0.21290 (4)	0.29115 (4)	0.00986 (14)
O2	0.21869 (4)	0.12195 (4)	0.45628 (4)	0.01637 (17)
H2	0.2383 (9)	0.1233 (11)	0.4913 (9)	0.048 (7)*
O3	0.26809 (4)	0.10217 (4)	0.32397 (4)	0.01312 (16)
O4	0.29956 (4)	0.21244 (4)	0.32770 (4)	0.00978 (14)
O5	0.37899 (4)	0.05905 (4)	0.27734 (4)	0.01365 (16)
O6	0.40289 (4)	0.18411 (4)	0.24104 (4)	0.01275 (15)
N1	0.14858 (4)	0.10076 (4)	0.35394 (4)	0.01091 (17)
N2	0.40266 (4)	0.15008 (4)	0.35735 (4)	0.01108 (17)
C1	0.10275 (5)	0.13060 (5)	0.31484 (5)	0.0129 (2)
H1A	0.076640	0.156948	0.340002	0.015*
H1B	0.076764	0.099374	0.295911	0.015*
C2	0.13276 (5)	0.16854 (5)	0.26538 (5)	0.01151 (19)
H2A	0.156258	0.141764	0.238188	0.014*
H2B	0.101192	0.188918	0.240948	0.014*
C3	0.12445 (5)	0.08718 (6)	0.41514 (5)	0.0146 (2)
H3A	0.097115	0.051736	0.412797	0.017*
H3B	0.100542	0.122151	0.429773	0.017*
C4	0.17503 (6)	0.07400 (5)	0.45961 (5)	0.0152 (2)
H4A	0.158507	0.071214	0.501178	0.018*
H4B	0.194465	0.034891	0.449512	0.018*
C5	0.17540 (5)	0.04711 (5)	0.32310 (6)	0.0134 (2)
H5A	0.166443	0.049253	0.279232	0.016*
H5B	0.156514	0.009797	0.339230	0.016*
C6	0.24374 (5)	0.04385 (5)	0.33227 (5)	0.0126 (2)
H6A	0.252965	0.029135	0.373582	0.015*
H6B	0.261812	0.015364	0.302765	0.015*
C7	0.37356 (5)	0.18936 (5)	0.40332 (5)	0.0130 (2)
H7A	0.404749	0.207173	0.430125	0.016*
H7B	0.345497	0.165143	0.428525	0.016*
C8	0.33886 (5)	0.23950 (5)	0.37111 (5)	0.0121 (2)
H8A	0.314986	0.263136	0.400776	0.014*
H8B	0.367487	0.267273	0.350669	0.014*
C9	0.41247 (6)	0.08692 (5)	0.37804 (5)	0.0149 (2)
H9A	0.376760	0.072762	0.401131	0.018*
H9B	0.448238	0.085129	0.404990	0.018*
C10	0.42245 (5)	0.04634 (5)	0.32320 (6)	0.0146 (2)
H10A	0.463706	0.052964	0.306983	0.018*
H10B	0.419081	0.003389	0.335540	0.018*
C11	0.45825 (5)	0.17931 (6)	0.33281 (5)	0.0137 (2)
H11A	0.494455	0.160261	0.351123	0.016*
H11B	0.458364	0.222757	0.343807	0.016*
C12	0.46122 (5)	0.17298 (5)	0.26411 (5)	0.0130 (2)
H12A	0.490419	0.202435	0.247136	0.016*
H12B	0.474609	0.131682	0.252974	0.016*
Cl1	0.09580 (2)	0.09580 (2)	0.09580 (2)	0.01534 (9)
O7	0.08074 (5)	0.08564 (5)	0.15863 (5)	0.0266 (2)
O8	0.05841 (5)	0.05841 (5)	0.05841 (5)	0.0304 (4)
Cl2	0.41017 (2)	0.41017 (2)	0.41017 (2)	0.01490 (9)
O9	0.42281 (5)	0.34728 (5)	0.42264 (5)	0.0253 (2)
O10	0.44765 (5)	0.44765 (5)	0.44765 (5)	0.0281 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.00791 (5)	0.00791 (5)	0.00791 (5)	0.00099 (5)	0.00099 (5)	0.00099 (5)
Fe2	0.00892 (7)	0.00825 (7)	0.00963 (7)	0.00067 (5)	0.00126 (5)	0.00061 (5)
Fe3	0.00793 (7)	0.00863 (7)	0.00871 (7)	0.00104 (5)	0.00021 (5)	0.00058 (5)
O1	0.0105 (3)	0.0091 (3)	0.0101 (3)	−0.0005 (3)	0.0005 (3)	−0.0005 (3)
O2	0.0209 (4)	0.0160 (4)	0.0123 (4)	−0.0039 (3)	−0.0032 (3)	0.0034 (3)
O3	0.0131 (4)	0.0087 (3)	0.0176 (4)	0.0000 (3)	0.0047 (3)	0.0006 (3)
O4	0.0096 (3)	0.0099 (3)	0.0098 (3)	0.0005 (3)	−0.0010 (3)	0.0001 (3)
O5	0.0129 (4)	0.0120 (4)	0.0161 (4)	0.0025 (3)	−0.0014 (3)	−0.0013 (3)
O6	0.0079 (3)	0.0176 (4)	0.0127 (4)	0.0008 (3)	−0.0002 (3)	0.0042 (3)
N1	0.0105 (4)	0.0106 (4)	0.0117 (4)	0.0003 (3)	0.0015 (3)	0.0007 (3)
N2	0.0106 (4)	0.0115 (4)	0.0111 (4)	0.0018 (3)	−0.0005 (3)	0.0009 (3)
C1	0.0101 (5)	0.0132 (5)	0.0153 (5)	−0.0011 (4)	−0.0004 (4)	0.0016 (4)
C2	0.0114 (5)	0.0119 (5)	0.0112 (5)	−0.0016 (4)	−0.0015 (4)	−0.0007 (4)
C3	0.0138 (5)	0.0161 (5)	0.0138 (5)	−0.0016 (4)	0.0033 (4)	0.0027 (4)
C4	0.0204 (6)	0.0133 (5)	0.0118 (5)	−0.0028 (4)	0.0011 (4)	0.0025 (4)
C5	0.0141 (5)	0.0096 (5)	0.0164 (5)	−0.0009 (4)	0.0006 (4)	−0.0010 (4)
C6	0.0139 (5)	0.0079 (4)	0.0161 (5)	0.0002 (4)	0.0023 (4)	0.0011 (4)
C7	0.0138 (5)	0.0153 (5)	0.0101 (5)	0.0026 (4)	−0.0014 (4)	−0.0007 (4)
C8	0.0136 (5)	0.0111 (5)	0.0115 (5)	−0.0002 (4)	−0.0018 (4)	−0.0011 (4)
C9	0.0173 (5)	0.0136 (5)	0.0138 (5)	0.0030 (4)	−0.0017 (4)	0.0034 (4)
C10	0.0144 (5)	0.0111 (5)	0.0183 (5)	0.0030 (4)	−0.0020 (4)	0.0002 (4)
C11	0.0102 (5)	0.0159 (5)	0.0152 (5)	−0.0009 (4)	−0.0017 (4)	0.0004 (4)
C12	0.0083 (5)	0.0158 (5)	0.0148 (5)	0.0006 (4)	0.0005 (4)	0.0024 (4)
Cl1	0.01534 (9)	0.01534 (9)	0.01534 (9)	0.00135 (10)	0.00135 (10)	0.00135 (10)
O7	0.0310 (6)	0.0320 (6)	0.0166 (5)	0.0077 (4)	0.0056 (4)	0.0051 (4)
O8	0.0304 (4)	0.0304 (4)	0.0304 (4)	−0.0074 (4)	−0.0074 (4)	−0.0074 (4)
Cl2	0.01490 (9)	0.01490 (9)	0.01490 (9)	0.00088 (10)	0.00088 (10)	0.00088 (10)
O9	0.0321 (6)	0.0161 (4)	0.0278 (5)	0.0056 (4)	0.0044 (4)	0.0032 (4)
O10	0.0281 (4)	0.0281 (4)	0.0281 (4)	−0.0057 (4)	−0.0057 (4)	−0.0057 (4)

Geometric parameters (Å, º) top

Fe1—O4ⁱ	2.1352 (8)	C2—H2B	0.9900
Fe1—O4ⁱⁱ	2.1352 (8)	C3—C4	1.5159 (17)
Fe1—O4	2.1353 (8)	C3—H3A	0.9900
Fe1—O1	2.1719 (8)	C3—H3B	0.9900
Fe1—O1ⁱ	2.1719 (8)	C4—H4A	0.9900
Fe1—O1ⁱⁱ	2.1719 (8)	C4—H4B	0.9900
Fe2—O6ⁱ	1.9814 (8)	C5—C6	1.5247 (16)
Fe2—O3	2.0198 (8)	C5—H5A	0.9900
Fe2—N1	2.1873 (10)	C5—H5B	0.9900
Fe2—O4	2.1888 (8)	C6—H6A	0.9900
Fe2—O2	2.2081 (9)	C6—H6B	0.9900
Fe2—O1	2.2342 (8)	C7—C8	1.5233 (16)
Fe3—O3	1.9516 (8)	C7—H7A	0.9900
Fe3—O5	1.9600 (8)	C7—H7B	0.9900
Fe3—O6	1.9945 (8)	C8—H8A	0.9900
Fe3—O1ⁱⁱ	2.0270 (8)	C8—H8B	0.9900
Fe3—O4	2.0989 (8)	C9—C10	1.5229 (17)
Fe3—N2	2.1774 (10)	C9—H9A	0.9900
O1—C2	1.4271 (13)	C9—H9B	0.9900
O2—C4	1.4345 (15)	C10—H10A	0.9900
O2—H2	0.89 (2)	C10—H10B	0.9900
O3—C6	1.4080 (13)	C11—C12	1.5252 (16)
O4—C8	1.4247 (14)	C11—H11A	0.9900
O5—C10	1.4235 (14)	C11—H11B	0.9900
O6—C12	1.4071 (14)	C12—H12A	0.9900
N1—C3	1.4836 (15)	C12—H12B	0.9900
N1—C1	1.4849 (15)	Cl1—O8	1.4302 (18)
N1—C5	1.4898 (15)	Cl1—O7ⁱ	1.4448 (10)
N2—C7	1.4822 (15)	Cl1—O7ⁱⁱ	1.4448 (10)
N2—C9	1.4839 (15)	Cl1—O7	1.4448 (10)
N2—C11	1.4896 (15)	Cl2—O10	1.4341 (19)
C1—C2	1.5282 (16)	Cl2—O9	1.4435 (10)
C1—H1A	0.9900	Cl2—O9ⁱ	1.4435 (10)
C1—H1B	0.9900	Cl2—O9ⁱⁱ	1.4435 (10)
C2—H2A	0.9900

O4ⁱ—Fe1—O4ⁱⁱ	99.17 (3)	N1—C1—H1B	109.4
O4ⁱ—Fe1—O4	99.16 (3)	C2—C1—H1B	109.4
O4ⁱⁱ—Fe1—O4	99.16 (3)	H1A—C1—H1B	108.0
O4ⁱ—Fe1—O1	77.45 (3)	O1—C2—C1	110.80 (9)
O4ⁱⁱ—Fe1—O1	174.49 (3)	O1—C2—H2A	109.5
O4—Fe1—O1	85.73 (3)	C1—C2—H2A	109.5
O4ⁱ—Fe1—O1ⁱ	85.73 (3)	O1—C2—H2B	109.5
O4ⁱⁱ—Fe1—O1ⁱ	77.44 (3)	C1—C2—H2B	109.5
O4—Fe1—O1ⁱ	174.49 (3)	H2A—C2—H2B	108.1
O1—Fe1—O1ⁱ	97.86 (3)	N1—C3—C4	111.37 (10)
O4ⁱ—Fe1—O1ⁱⁱ	174.49 (3)	N1—C3—H3A	109.4
O4ⁱⁱ—Fe1—O1ⁱⁱ	85.73 (3)	C4—C3—H3A	109.4
O4—Fe1—O1ⁱⁱ	77.45 (3)	N1—C3—H3B	109.4
O1—Fe1—O1ⁱⁱ	97.86 (3)	C4—C3—H3B	109.4
O1ⁱ—Fe1—O1ⁱⁱ	97.86 (3)	H3A—C3—H3B	108.0
O6ⁱ—Fe2—O3	170.08 (4)	O2—C4—C3	108.69 (9)
O6ⁱ—Fe2—N1	107.99 (4)	O2—C4—H4A	110.0
O3—Fe2—N1	80.52 (4)	C3—C4—H4A	110.0
O6ⁱ—Fe2—O4	96.25 (3)	O2—C4—H4B	110.0
O3—Fe2—O4	73.93 (3)	C3—C4—H4B	110.0
N1—Fe2—O4	146.33 (3)	H4A—C4—H4B	108.3
O6ⁱ—Fe2—O2	90.60 (3)	N1—C5—C6	111.74 (9)
O3—Fe2—O2	96.23 (4)	N1—C5—H5A	109.3
N1—Fe2—O2	78.46 (4)	C6—C5—H5A	109.3
O4—Fe2—O2	125.30 (3)	N1—C5—H5B	109.3
O6ⁱ—Fe2—O1	74.48 (3)	C6—C5—H5B	109.3
O3—Fe2—O1	102.40 (3)	H5A—C5—H5B	107.9
N1—Fe2—O1	81.48 (3)	O3—C6—C5	108.54 (9)
O4—Fe2—O1	82.97 (3)	O3—C6—H6A	110.0
O2—Fe2—O1	149.87 (3)	C5—C6—H6A	110.0
O3—Fe3—O5	92.38 (4)	O3—C6—H6B	110.0
O3—Fe3—O6	172.02 (4)	C5—C6—H6B	110.0
O5—Fe3—O6	95.38 (4)	H6A—C6—H6B	108.4
O3—Fe3—O1ⁱⁱ	95.38 (3)	N2—C7—C8	108.89 (9)
O5—Fe3—O1ⁱⁱ	120.80 (3)	N2—C7—H7A	109.9
O6—Fe3—O1ⁱⁱ	79.04 (3)	C8—C7—H7A	109.9
O3—Fe3—O4	77.37 (3)	N2—C7—H7B	109.9
O5—Fe3—O4	156.56 (3)	C8—C7—H7B	109.9
O6—Fe3—O4	96.05 (3)	H7A—C7—H7B	108.3
O1ⁱⁱ—Fe3—O4	81.53 (3)	O4—C8—C7	108.41 (9)
O3—Fe3—N2	103.25 (4)	O4—C8—H8A	110.0
O5—Fe3—N2	82.31 (4)	C7—C8—H8A	110.0
O6—Fe3—N2	79.70 (4)	O4—C8—H8B	110.0
O1ⁱⁱ—Fe3—N2	149.83 (4)	C7—C8—H8B	110.0
O4—Fe3—N2	79.70 (3)	H8A—C8—H8B	108.4
C2—O1—Fe3ⁱ	120.46 (7)	N2—C9—C10	109.24 (9)
C2—O1—Fe1	129.12 (7)	N2—C9—H9A	109.8
Fe3ⁱ—O1—Fe1	100.98 (3)	C10—C9—H9A	109.8
C2—O1—Fe2	106.43 (6)	N2—C9—H9B	109.8
Fe3ⁱ—O1—Fe2	98.15 (3)	C10—C9—H9B	109.8
Fe1—O1—Fe2	94.43 (3)	H9A—C9—H9B	108.3
C4—O2—Fe2	113.21 (7)	O5—C10—C9	110.63 (9)
C4—O2—H2	108.0 (15)	O5—C10—H10A	109.5
Fe2—O2—H2	138.7 (14)	C9—C10—H10A	109.5
C6—O3—Fe3	136.90 (7)	O5—C10—H10B	109.5
C6—O3—Fe2	113.09 (7)	C9—C10—H10B	109.5
Fe3—O3—Fe2	109.96 (4)	H10A—C10—H10B	108.1
C8—O4—Fe3	113.16 (6)	N2—C11—C12	110.96 (9)
C8—O4—Fe1	129.21 (7)	N2—C11—H11A	109.4
Fe3—O4—Fe1	99.88 (3)	C12—C11—H11A	109.4
C8—O4—Fe2	114.05 (7)	N2—C11—H11B	109.4
Fe3—O4—Fe2	98.66 (3)	C12—C11—H11B	109.4
Fe1—O4—Fe2	96.80 (3)	H11A—C11—H11B	108.0
C10—O5—Fe3	115.63 (7)	O6—C12—C11	107.76 (9)
C12—O6—Fe2ⁱⁱ	137.14 (7)	O6—C12—H12A	110.2
C12—O6—Fe3	113.19 (7)	C11—C12—H12A	110.2
Fe2ⁱⁱ—O6—Fe3	108.30 (4)	O6—C12—H12B	110.2
C3—N1—C1	112.01 (9)	C11—C12—H12B	110.2
C3—N1—C5	113.50 (9)	H12A—C12—H12B	108.5
C1—N1—C5	110.99 (9)	O8—Cl1—O7ⁱ	109.39 (5)
C3—N1—Fe2	105.98 (7)	O8—Cl1—O7ⁱⁱ	109.39 (5)
C1—N1—Fe2	106.02 (7)	O7ⁱ—Cl1—O7ⁱⁱ	109.55 (5)
C5—N1—Fe2	107.84 (7)	O8—Cl1—O7	109.40 (5)
C7—N2—C9	113.75 (9)	O7ⁱ—Cl1—O7	109.55 (5)
C7—N2—C11	110.68 (9)	O7ⁱⁱ—Cl1—O7	109.55 (5)
C9—N2—C11	113.53 (9)	O10—Cl2—O9	109.50 (5)
C7—N2—Fe3	107.60 (7)	O10—Cl2—O9ⁱ	109.50 (5)
C9—N2—Fe3	101.93 (7)	O9—Cl2—O9ⁱ	109.45 (5)
C11—N2—Fe3	108.73 (7)	O10—Cl2—O9ⁱⁱ	109.50 (5)
N1—C1—C2	111.32 (9)	O9—Cl2—O9ⁱⁱ	109.44 (5)
N1—C1—H1A	109.4	O9ⁱ—Cl2—O9ⁱⁱ	109.45 (5)
C2—C1—H1A	109.4

C3—N1—C1—C2	154.85 (10)	C9—N2—C7—C8	−152.83 (10)
C5—N1—C1—C2	−77.15 (12)	C11—N2—C7—C8	77.95 (11)
Fe2—N1—C1—C2	39.70 (10)	Fe3—N2—C7—C8	−40.72 (10)
Fe3ⁱ—O1—C2—C1	−69.16 (10)	Fe3—O4—C8—C7	−38.20 (10)
Fe1—O1—C2—C1	151.10 (7)	Fe1—O4—C8—C7	−164.36 (7)
Fe2—O1—C2—C1	41.01 (10)	Fe2—O4—C8—C7	73.53 (9)
N1—C1—C2—O1	−57.29 (12)	N2—C7—C8—O4	52.65 (12)
C1—N1—C3—C4	−163.54 (10)	C7—N2—C9—C10	161.48 (10)
C5—N1—C3—C4	69.81 (12)	C11—N2—C9—C10	−70.76 (12)
Fe2—N1—C3—C4	−48.36 (11)	Fe3—N2—C9—C10	45.98 (10)
Fe2—O2—C4—C3	−26.94 (12)	Fe3—O5—C10—C9	19.09 (12)
N1—C3—C4—O2	51.07 (13)	N2—C9—C10—O5	−45.53 (13)
C3—N1—C5—C6	−95.22 (11)	C7—N2—C11—C12	−135.90 (10)
C1—N1—C5—C6	137.60 (10)	C9—N2—C11—C12	94.76 (11)
Fe2—N1—C5—C6	21.87 (11)	Fe3—N2—C11—C12	−17.93 (11)
Fe3—O3—C6—C5	−137.18 (9)	Fe2ⁱⁱ—O6—C12—C11	146.42 (9)
Fe2—O3—C6—C5	45.75 (11)	Fe3—O6—C12—C11	−49.03 (11)
N1—C5—C6—O3	−43.95 (13)	N2—C11—C12—O6	42.43 (13)

Symmetry codes: (i) y, z, x; (ii) z, x, y.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O2—H2···O5ⁱⁱⁱ	0.89 (2)	1.73 (2)	2.6137 (13)	176 (2)

Symmetry code: (iii) z, −x+1/2, y+1/2.

Reflection statistics for the strong substructure and the weak superstructure reflections.
Agreement factors R1 and wR2 were calculated according to the SHELXL manual (Sheldrick, 2015b). top

h+k+l	#	<I>	<σ>	<I>/<σ>	<I/σ>	wR2 (all reflections)	R1 [I > 2σ(I)]	# I > 2σ(I)
2n	3990	12721.86	495.31	25.68	46.01	0.0621	0.0233	84.29 %
2n+1	3972	1654.41	131.84	12.55	15.64	0.0894	0.0412	69.44 %
Total	7962	7198.77	313.97	22.93	30.85	0.0701	0.0282	76.88 %

Results of the leverage analysis performed with the program HATTIE (Parsons et al., 2012)
The normalized value T² is a measure of the influence of a specific reflection on a refined parameter. top

	h	k	l	T²
x coordinate (H2)	3	1	5	10000
	3	3	3	7629.49
	3	5	7	7353.62
	5	1	7	7175.33

y coordinate (H2)	0	2	6	10000
	0	6	10	7304.21
	5	1	8	5936.25
	6	4	10	5243.41

z coordinate (H2)	5	0	6	10000
	4	6	7	5790.49
	1	0	8	5227.58
	3	4	6	4357.97

Bond lengths (Å) from different refinements top

	Literature structure at room temperature (Liu et al., 2008))	Present study at 100 K
	I2₁3	I2₁3	Ia3	Pa3
Fe1—O	2.122 (7)–2.182 (7)	2.140 (5)–2.164 (5)	2.1515 (8)	2.1353 (10)–2.1719 (10)
Fe2—O	1.977 (7)–2.184 (6)	1.976 (5)–2.188 (6)	1.9666 (10)–2.1811 (10)	1.9814 (10)–2.2343 (10)
Fe3—O	1.954 (6)–2.151 (6)	1.955 (5)–2.176 (6)	-	1.9517 (10)–2.0989 (10)

Bond-valence sums (BVS)
Entries for the literature structure were taken from the original publication. Entries for the present study were calculated using the ToposPro software (Version 5.3.0.3; Blatov et al., 2014) with parameters from Brown (2016b): R₀(Fe³⁺—O) 1.759 Å; R₀(Fe²⁺—O) 1.734 Å; R₀(Fe³⁺—N) 1.82 Å; R₀(Fe²⁺—N) 1.76 Å. A b value of 0.37 was used for all bonds. top

	Assumed state	Literature structure at room temperature (Liu et al., 2008)	Present study at 100 K
		I2₁3	I2₁3	Ia3	Pa3
Fe1	+2	1.82	1.94	1.94	1.93
	+3		2.08	2.08	2.07
Fe2	+2		2.40	2.40	2.11
	+3	2.53	2.60	2.61	2.30
Fe3	+2		2.40		2.75
	+3	2.73	2.61		2.97

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Tri­ethano­laminate iron perchlorate revisited: change of space group, chemical composition and oxidation states in [Fe7(tea)3(tea-H)3](ClO4)2 (tea-H3 is tri­ethano­lamine)

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Triethanolaminate iron perchlorate revisited: change of space group, chemical composition and oxidation states in [Fe₇(tea)₃(tea-H)₃](ClO₄)₂ (tea-H₃ is triethanolamine)