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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 FeII and three FeIII centres. Symmetry relationships between the two space groups and the average supergroup Ia\overline{3} are discussed in detail.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229617018460/qf3003sup1.cif
Contains datablock I

hkl

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)2Mo Kα radiation, λ = 0.71073 Å
Mr = 1469.87Cell parameters from 104201 reflections
Cubic, Pa3θ = 1.3–35.1°
a = 22.0884 (6) ŵ = 2.02 mm1
V = 10776.9 (8) Å3T = 100 K
Z = 8Block, black
F(000) = 60560.22 × 0.09 × 0.08 mm
Dx = 1.812 Mg m3
Data collection top
Bruker Kappa APEXII
diffractometer
6121 reflections with I > 2σ(I)
Radiation source: sealed tubeRint = 0.055
φ and ω scansθmax = 35.1°, θmin = 1.6°
Absorption correction: numerical
(SADABS; Sheldrick, 2014)
h = 3530
Tmin = 0.687, Tmax = 0.887k = 3435
211368 measured reflectionsl = 3331
7962 independent reflections
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028Hydrogen site location: difference Fourier map
wR(F2) = 0.070H atoms treated by a mixture of independent and constrained refinement
S = 1.02 w = 1/[σ2(Fo2) + (0.0318P)2 + 4.712P]
where P = (Fo2 + 2Fc2)/3
7962 reflections(Δ/σ)max = 0.002
236 parametersΔρmax = 0.67 e Å3
0 restraintsΔρmin = 0.47 e Å3
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
xyzUiso*/Ueq
Fe10.25330 (2)0.25330 (2)0.25330 (2)0.00791 (5)
Fe20.22069 (2)0.16731 (2)0.36722 (2)0.00893 (4)
Fe30.33830 (2)0.13764 (2)0.28373 (2)0.00842 (4)
O10.17204 (4)0.21290 (4)0.29115 (4)0.00986 (14)
O20.21869 (4)0.12195 (4)0.45628 (4)0.01637 (17)
H20.2383 (9)0.1233 (11)0.4913 (9)0.048 (7)*
O30.26809 (4)0.10217 (4)0.32397 (4)0.01312 (16)
O40.29956 (4)0.21244 (4)0.32770 (4)0.00978 (14)
O50.37899 (4)0.05905 (4)0.27734 (4)0.01365 (16)
O60.40289 (4)0.18411 (4)0.24104 (4)0.01275 (15)
N10.14858 (4)0.10076 (4)0.35394 (4)0.01091 (17)
N20.40266 (4)0.15008 (4)0.35735 (4)0.01108 (17)
C10.10275 (5)0.13060 (5)0.31484 (5)0.0129 (2)
H1A0.0766400.1569480.3400020.015*
H1B0.0767640.0993740.2959110.015*
C20.13276 (5)0.16854 (5)0.26538 (5)0.01151 (19)
H2A0.1562580.1417640.2381880.014*
H2B0.1011920.1889180.2409480.014*
C30.12445 (5)0.08718 (6)0.41514 (5)0.0146 (2)
H3A0.0971150.0517360.4127970.017*
H3B0.1005420.1221510.4297730.017*
C40.17503 (6)0.07400 (5)0.45961 (5)0.0152 (2)
H4A0.1585070.0712140.5011780.018*
H4B0.1944650.0348910.4495120.018*
C50.17540 (5)0.04711 (5)0.32310 (6)0.0134 (2)
H5A0.1664430.0492530.2792320.016*
H5B0.1565140.0097970.3392300.016*
C60.24374 (5)0.04385 (5)0.33227 (5)0.0126 (2)
H6A0.2529650.0291350.3735820.015*
H6B0.2618120.0153640.3027650.015*
C70.37356 (5)0.18936 (5)0.40332 (5)0.0130 (2)
H7A0.4047490.2071730.4301250.016*
H7B0.3454970.1651430.4285250.016*
C80.33886 (5)0.23950 (5)0.37111 (5)0.0121 (2)
H8A0.3149860.2631360.4007760.014*
H8B0.3674870.2672730.3506690.014*
C90.41247 (6)0.08692 (5)0.37804 (5)0.0149 (2)
H9A0.3767600.0727620.4011310.018*
H9B0.4482380.0851290.4049900.018*
C100.42245 (5)0.04634 (5)0.32320 (6)0.0146 (2)
H10A0.4637060.0529640.3069830.018*
H10B0.4190810.0033890.3355400.018*
C110.45825 (5)0.17931 (6)0.33281 (5)0.0137 (2)
H11A0.4944550.1602610.3511230.016*
H11B0.4583640.2227570.3438070.016*
C120.46122 (5)0.17298 (5)0.26411 (5)0.0130 (2)
H12A0.4904190.2024350.2471360.016*
H12B0.4746090.1316820.2529740.016*
Cl10.09580 (2)0.09580 (2)0.09580 (2)0.01534 (9)
O70.08074 (5)0.08564 (5)0.15863 (5)0.0266 (2)
O80.05841 (5)0.05841 (5)0.05841 (5)0.0304 (4)
Cl20.41017 (2)0.41017 (2)0.41017 (2)0.01490 (9)
O90.42281 (5)0.34728 (5)0.42264 (5)0.0253 (2)
O100.44765 (5)0.44765 (5)0.44765 (5)0.0281 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.00791 (5)0.00791 (5)0.00791 (5)0.00099 (5)0.00099 (5)0.00099 (5)
Fe20.00892 (7)0.00825 (7)0.00963 (7)0.00067 (5)0.00126 (5)0.00061 (5)
Fe30.00793 (7)0.00863 (7)0.00871 (7)0.00104 (5)0.00021 (5)0.00058 (5)
O10.0105 (3)0.0091 (3)0.0101 (3)0.0005 (3)0.0005 (3)0.0005 (3)
O20.0209 (4)0.0160 (4)0.0123 (4)0.0039 (3)0.0032 (3)0.0034 (3)
O30.0131 (4)0.0087 (3)0.0176 (4)0.0000 (3)0.0047 (3)0.0006 (3)
O40.0096 (3)0.0099 (3)0.0098 (3)0.0005 (3)0.0010 (3)0.0001 (3)
O50.0129 (4)0.0120 (4)0.0161 (4)0.0025 (3)0.0014 (3)0.0013 (3)
O60.0079 (3)0.0176 (4)0.0127 (4)0.0008 (3)0.0002 (3)0.0042 (3)
N10.0105 (4)0.0106 (4)0.0117 (4)0.0003 (3)0.0015 (3)0.0007 (3)
N20.0106 (4)0.0115 (4)0.0111 (4)0.0018 (3)0.0005 (3)0.0009 (3)
C10.0101 (5)0.0132 (5)0.0153 (5)0.0011 (4)0.0004 (4)0.0016 (4)
C20.0114 (5)0.0119 (5)0.0112 (5)0.0016 (4)0.0015 (4)0.0007 (4)
C30.0138 (5)0.0161 (5)0.0138 (5)0.0016 (4)0.0033 (4)0.0027 (4)
C40.0204 (6)0.0133 (5)0.0118 (5)0.0028 (4)0.0011 (4)0.0025 (4)
C50.0141 (5)0.0096 (5)0.0164 (5)0.0009 (4)0.0006 (4)0.0010 (4)
C60.0139 (5)0.0079 (4)0.0161 (5)0.0002 (4)0.0023 (4)0.0011 (4)
C70.0138 (5)0.0153 (5)0.0101 (5)0.0026 (4)0.0014 (4)0.0007 (4)
C80.0136 (5)0.0111 (5)0.0115 (5)0.0002 (4)0.0018 (4)0.0011 (4)
C90.0173 (5)0.0136 (5)0.0138 (5)0.0030 (4)0.0017 (4)0.0034 (4)
C100.0144 (5)0.0111 (5)0.0183 (5)0.0030 (4)0.0020 (4)0.0002 (4)
C110.0102 (5)0.0159 (5)0.0152 (5)0.0009 (4)0.0017 (4)0.0004 (4)
C120.0083 (5)0.0158 (5)0.0148 (5)0.0006 (4)0.0005 (4)0.0024 (4)
Cl10.01534 (9)0.01534 (9)0.01534 (9)0.00135 (10)0.00135 (10)0.00135 (10)
O70.0310 (6)0.0320 (6)0.0166 (5)0.0077 (4)0.0056 (4)0.0051 (4)
O80.0304 (4)0.0304 (4)0.0304 (4)0.0074 (4)0.0074 (4)0.0074 (4)
Cl20.01490 (9)0.01490 (9)0.01490 (9)0.00088 (10)0.00088 (10)0.00088 (10)
O90.0321 (6)0.0161 (4)0.0278 (5)0.0056 (4)0.0044 (4)0.0032 (4)
O100.0281 (4)0.0281 (4)0.0281 (4)0.0057 (4)0.0057 (4)0.0057 (4)
Geometric parameters (Å, º) top
Fe1—O4i2.1352 (8)C2—H2B0.9900
Fe1—O4ii2.1352 (8)C3—C41.5159 (17)
Fe1—O42.1353 (8)C3—H3A0.9900
Fe1—O12.1719 (8)C3—H3B0.9900
Fe1—O1i2.1719 (8)C4—H4A0.9900
Fe1—O1ii2.1719 (8)C4—H4B0.9900
Fe2—O6i1.9814 (8)C5—C61.5247 (16)
Fe2—O32.0198 (8)C5—H5A0.9900
Fe2—N12.1873 (10)C5—H5B0.9900
Fe2—O42.1888 (8)C6—H6A0.9900
Fe2—O22.2081 (9)C6—H6B0.9900
Fe2—O12.2342 (8)C7—C81.5233 (16)
Fe3—O31.9516 (8)C7—H7A0.9900
Fe3—O51.9600 (8)C7—H7B0.9900
Fe3—O61.9945 (8)C8—H8A0.9900
Fe3—O1ii2.0270 (8)C8—H8B0.9900
Fe3—O42.0989 (8)C9—C101.5229 (17)
Fe3—N22.1774 (10)C9—H9A0.9900
O1—C21.4271 (13)C9—H9B0.9900
O2—C41.4345 (15)C10—H10A0.9900
O2—H20.89 (2)C10—H10B0.9900
O3—C61.4080 (13)C11—C121.5252 (16)
O4—C81.4247 (14)C11—H11A0.9900
O5—C101.4235 (14)C11—H11B0.9900
O6—C121.4071 (14)C12—H12A0.9900
N1—C31.4836 (15)C12—H12B0.9900
N1—C11.4849 (15)Cl1—O81.4302 (18)
N1—C51.4898 (15)Cl1—O7i1.4448 (10)
N2—C71.4822 (15)Cl1—O7ii1.4448 (10)
N2—C91.4839 (15)Cl1—O71.4448 (10)
N2—C111.4896 (15)Cl2—O101.4341 (19)
C1—C21.5282 (16)Cl2—O91.4435 (10)
C1—H1A0.9900Cl2—O9i1.4435 (10)
C1—H1B0.9900Cl2—O9ii1.4435 (10)
C2—H2A0.9900
O4i—Fe1—O4ii99.17 (3)N1—C1—H1B109.4
O4i—Fe1—O499.16 (3)C2—C1—H1B109.4
O4ii—Fe1—O499.16 (3)H1A—C1—H1B108.0
O4i—Fe1—O177.45 (3)O1—C2—C1110.80 (9)
O4ii—Fe1—O1174.49 (3)O1—C2—H2A109.5
O4—Fe1—O185.73 (3)C1—C2—H2A109.5
O4i—Fe1—O1i85.73 (3)O1—C2—H2B109.5
O4ii—Fe1—O1i77.44 (3)C1—C2—H2B109.5
O4—Fe1—O1i174.49 (3)H2A—C2—H2B108.1
O1—Fe1—O1i97.86 (3)N1—C3—C4111.37 (10)
O4i—Fe1—O1ii174.49 (3)N1—C3—H3A109.4
O4ii—Fe1—O1ii85.73 (3)C4—C3—H3A109.4
O4—Fe1—O1ii77.45 (3)N1—C3—H3B109.4
O1—Fe1—O1ii97.86 (3)C4—C3—H3B109.4
O1i—Fe1—O1ii97.86 (3)H3A—C3—H3B108.0
O6i—Fe2—O3170.08 (4)O2—C4—C3108.69 (9)
O6i—Fe2—N1107.99 (4)O2—C4—H4A110.0
O3—Fe2—N180.52 (4)C3—C4—H4A110.0
O6i—Fe2—O496.25 (3)O2—C4—H4B110.0
O3—Fe2—O473.93 (3)C3—C4—H4B110.0
N1—Fe2—O4146.33 (3)H4A—C4—H4B108.3
O6i—Fe2—O290.60 (3)N1—C5—C6111.74 (9)
O3—Fe2—O296.23 (4)N1—C5—H5A109.3
N1—Fe2—O278.46 (4)C6—C5—H5A109.3
O4—Fe2—O2125.30 (3)N1—C5—H5B109.3
O6i—Fe2—O174.48 (3)C6—C5—H5B109.3
O3—Fe2—O1102.40 (3)H5A—C5—H5B107.9
N1—Fe2—O181.48 (3)O3—C6—C5108.54 (9)
O4—Fe2—O182.97 (3)O3—C6—H6A110.0
O2—Fe2—O1149.87 (3)C5—C6—H6A110.0
O3—Fe3—O592.38 (4)O3—C6—H6B110.0
O3—Fe3—O6172.02 (4)C5—C6—H6B110.0
O5—Fe3—O695.38 (4)H6A—C6—H6B108.4
O3—Fe3—O1ii95.38 (3)N2—C7—C8108.89 (9)
O5—Fe3—O1ii120.80 (3)N2—C7—H7A109.9
O6—Fe3—O1ii79.04 (3)C8—C7—H7A109.9
O3—Fe3—O477.37 (3)N2—C7—H7B109.9
O5—Fe3—O4156.56 (3)C8—C7—H7B109.9
O6—Fe3—O496.05 (3)H7A—C7—H7B108.3
O1ii—Fe3—O481.53 (3)O4—C8—C7108.41 (9)
O3—Fe3—N2103.25 (4)O4—C8—H8A110.0
O5—Fe3—N282.31 (4)C7—C8—H8A110.0
O6—Fe3—N279.70 (4)O4—C8—H8B110.0
O1ii—Fe3—N2149.83 (4)C7—C8—H8B110.0
O4—Fe3—N279.70 (3)H8A—C8—H8B108.4
C2—O1—Fe3i120.46 (7)N2—C9—C10109.24 (9)
C2—O1—Fe1129.12 (7)N2—C9—H9A109.8
Fe3i—O1—Fe1100.98 (3)C10—C9—H9A109.8
C2—O1—Fe2106.43 (6)N2—C9—H9B109.8
Fe3i—O1—Fe298.15 (3)C10—C9—H9B109.8
Fe1—O1—Fe294.43 (3)H9A—C9—H9B108.3
C4—O2—Fe2113.21 (7)O5—C10—C9110.63 (9)
C4—O2—H2108.0 (15)O5—C10—H10A109.5
Fe2—O2—H2138.7 (14)C9—C10—H10A109.5
C6—O3—Fe3136.90 (7)O5—C10—H10B109.5
C6—O3—Fe2113.09 (7)C9—C10—H10B109.5
Fe3—O3—Fe2109.96 (4)H10A—C10—H10B108.1
C8—O4—Fe3113.16 (6)N2—C11—C12110.96 (9)
C8—O4—Fe1129.21 (7)N2—C11—H11A109.4
Fe3—O4—Fe199.88 (3)C12—C11—H11A109.4
C8—O4—Fe2114.05 (7)N2—C11—H11B109.4
Fe3—O4—Fe298.66 (3)C12—C11—H11B109.4
Fe1—O4—Fe296.80 (3)H11A—C11—H11B108.0
C10—O5—Fe3115.63 (7)O6—C12—C11107.76 (9)
C12—O6—Fe2ii137.14 (7)O6—C12—H12A110.2
C12—O6—Fe3113.19 (7)C11—C12—H12A110.2
Fe2ii—O6—Fe3108.30 (4)O6—C12—H12B110.2
C3—N1—C1112.01 (9)C11—C12—H12B110.2
C3—N1—C5113.50 (9)H12A—C12—H12B108.5
C1—N1—C5110.99 (9)O8—Cl1—O7i109.39 (5)
C3—N1—Fe2105.98 (7)O8—Cl1—O7ii109.39 (5)
C1—N1—Fe2106.02 (7)O7i—Cl1—O7ii109.55 (5)
C5—N1—Fe2107.84 (7)O8—Cl1—O7109.40 (5)
C7—N2—C9113.75 (9)O7i—Cl1—O7109.55 (5)
C7—N2—C11110.68 (9)O7ii—Cl1—O7109.55 (5)
C9—N2—C11113.53 (9)O10—Cl2—O9109.50 (5)
C7—N2—Fe3107.60 (7)O10—Cl2—O9i109.50 (5)
C9—N2—Fe3101.93 (7)O9—Cl2—O9i109.45 (5)
C11—N2—Fe3108.73 (7)O10—Cl2—O9ii109.50 (5)
N1—C1—C2111.32 (9)O9—Cl2—O9ii109.44 (5)
N1—C1—H1A109.4O9i—Cl2—O9ii109.45 (5)
C2—C1—H1A109.4
C3—N1—C1—C2154.85 (10)C9—N2—C7—C8152.83 (10)
C5—N1—C1—C277.15 (12)C11—N2—C7—C877.95 (11)
Fe2—N1—C1—C239.70 (10)Fe3—N2—C7—C840.72 (10)
Fe3i—O1—C2—C169.16 (10)Fe3—O4—C8—C738.20 (10)
Fe1—O1—C2—C1151.10 (7)Fe1—O4—C8—C7164.36 (7)
Fe2—O1—C2—C141.01 (10)Fe2—O4—C8—C773.53 (9)
N1—C1—C2—O157.29 (12)N2—C7—C8—O452.65 (12)
C1—N1—C3—C4163.54 (10)C7—N2—C9—C10161.48 (10)
C5—N1—C3—C469.81 (12)C11—N2—C9—C1070.76 (12)
Fe2—N1—C3—C448.36 (11)Fe3—N2—C9—C1045.98 (10)
Fe2—O2—C4—C326.94 (12)Fe3—O5—C10—C919.09 (12)
N1—C3—C4—O251.07 (13)N2—C9—C10—O545.53 (13)
C3—N1—C5—C695.22 (11)C7—N2—C11—C12135.90 (10)
C1—N1—C5—C6137.60 (10)C9—N2—C11—C1294.76 (11)
Fe2—N1—C5—C621.87 (11)Fe3—N2—C11—C1217.93 (11)
Fe3—O3—C6—C5137.18 (9)Fe2ii—O6—C12—C11146.42 (9)
Fe2—O3—C6—C545.75 (11)Fe3—O6—C12—C1149.03 (11)
N1—C5—C6—O343.95 (13)N2—C11—C12—O642.43 (13)
Symmetry codes: (i) y, z, x; (ii) z, x, y.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H2···O5iii0.89 (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)
2n399012721.86495.3125.6846.010.06210.023384.29 %
2n+139721654.41131.8412.5515.640.08940.041269.44 %
Total79627198.77313.9722.9330.850.07010.028276.88 %
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
hklT2
x coordinate (H2)31510000
3337629.49
3577353.62
5177175.33
y coordinate (H2)02610000
06107304.21
5185936.25
64105243.41
z coordinate (H2)50610000
4675790.49
1085227.58
3464357.97
Bond lengths (Å) from different refinements top
Literature structure at room temperature (Liu et al., 2008))Present study at 100 K
I213I213Ia3Pa3
Fe1—O2.122 (7)–2.182 (7)2.140 (5)–2.164 (5)2.1515 (8)2.1353 (10)–2.1719 (10)
Fe2—O1.977 (7)–2.184 (6)1.976 (5)–2.188 (6)1.9666 (10)–2.1811 (10)1.9814 (10)–2.2343 (10)
Fe3—O1.954 (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 stateLiterature structure at room temperature (Liu et al., 2008)Present study at 100 K
I213I213Ia3Pa3
Fe1+21.821.941.941.93
+32.082.082.07
Fe2+22.402.402.11
+32.532.602.612.30
Fe3+22.402.75
+32.732.612.97
 

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