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Tetra­aqua­(18-crown-6)cerium(III) hexa­cyano­ferrate(III) di­hydrate, [Ce(C12H24O6)(H2O)4][Fe(CN)6]·2H2O, and tetra­aqua­(18-crown-6)neodymium(III) hexa­cyano­ferrate(III) dihydrate, [Nd(C12H24O6)(H2O)4][Fe(CN)6]·2H2O, are iso­morphous and isostructural in the C2/c space group, where the cations, which contain ten-coordinate lanthanoid centres, lie across twofold rotation axes and the anions lie across inversion centres. In these compounds, an extensive series of O—H...O and O—H...N hydrogen bonds links the components into a continuous three-dimensional framework. Triaqua­(18-crown-6)lanthanoid(III) hexa­cyano­ferrate(III) di­hydrate, [Ln(C12H24O6)(H2O)3][Fe(CN)6]·2H2O, where Ln = Sm, Eu, Gd or Tb, are all isomorphous and isostructural in the P\overline{1} space group, as are triaqua­(18-crown-6)gadolinium(III) hexa­cyano­chromate(III) dihydrate, [Gd(C12H24O6)(H2O)3][Cr(CN)6]·2H2O, and triaqua­(18-crown-6)gadolinium(III) hexa­cyano­cobaltate(III) dihydrate, [Gd(C12H24O6)(H2O)3][Co(CN)6]·2H2O. In these compounds, there are two independent anions, both lying across inversion centres, and the lanthanoid centres exhibit nine-coordination; in the crystal structures, an extensive series of hydrogen bonds links the components into a three-dimensional framework.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270107040449/gg3119sup1.cif
Contains datablocks global, I, II, III, IV, V, VII

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Structure factor file (CIF format) https://doi.org/10.1107/S0108270107040449/gg3119Isup2.hkl
Contains datablock I

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Structure factor file (CIF format) https://doi.org/10.1107/S0108270107040449/gg3119IIsup3.hkl
Contains datablock II

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Structure factor file (CIF format) https://doi.org/10.1107/S0108270107040449/gg3119IIIsup4.hkl
Contains datablock III

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Structure factor file (CIF format) https://doi.org/10.1107/S0108270107040449/gg3119IVsup5.hkl
Contains datablock IV

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Structure factor file (CIF format) https://doi.org/10.1107/S0108270107040449/gg3119Vsup6.hkl
Contains datablock V

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Structure factor file (CIF format) https://doi.org/10.1107/S0108270107040449/gg3119VIIsup7.hkl
Contains datablock VII

CCDC references: 602734; 602735; 602736; 602737; 602738; 602739; 602740

Comment top

We report here the molecular and supramolecular structures of a number of lanthanoid complexes of the macrocyclic ligand 18-crown-6 (1,4,7,10,13,16-hexaoxacyclooctadecane) as hydrated hexacyanometallate salts, which are formed by the reactions in aqueous solution between 18-crown-6 and the appropriate neutral dinuclear precursor complexes [Ln(DMF)4(H2O)3(µ-CN)M(CN)5].nH2O (DMF is dimethylformamide; Ln = Ce, Nd, Sm, Eu, Gd or Tb; M = Cr, Fe or Co) (see scheme). In these ligand-substitution reactions, the hexadentate macrocyclic ether displaces not only the hexacyanometallate(III) unit, which acts in the dinuclear precursors as a monodentate ligand, but also all of the DMF ligands.

When the lanthanoid is either Ce3+ or Nd3+ and M is Fe3+, the isomorphous hexacyanoferrate(III) salts [Ce(18-crown-6)(H2O)4)][Fe(CN)6]·2H2O, (I), and [Nd(18-crown-6)(H2O)4)][Fe(CN)6]·2H2O, (II), are formed (Fig. 1). When the lanthanoid cation is Sm3+, Eu3+ or Tb3+, and M is again Fe3+, the salts [Ln(18-crown-6)(H2O)3)][Fe(CN)6]·2H2O, with Ln = Sm, (III), Eu, (IV), and Tb, (VIII), are formed, all of which are isomorphous with the Gd analogue, (VI), whose structure was reported recently (Koner et al., 2005). Finally, when the lanthanoid cation is Gd3+ and the metal M is either Cr3+ or Co3+, the salts [Gd(18-crown-6)(H2O)3)][Cr(CN)6]·2H2O, (V), and [Gd(18-crown-6)(H2O)3)]Co(CN)6]·2H2O, (VII), are obtained, and these two salts are also isomorphous with compound (VI). The crystal quality for compound (VIII) was consistently poor, and the quality of the X-ray diffraction data was correspondingly poor; accordingly we do not discuss the metrical properties of this compound.

The isomorphous pair of compounds (I) and (II) crystallize in space group C2/c, with the [Ln(18-crown-6)(H2O)4]3+ unit lying across a twofold rotation axis, selected as that along (0, y, 1/4), and the [Fe(CN)6]3− anion lying across an inversion centre, selected as that at (1/4, 1/4, 0); the composition is completed by a noncoordinated water molecule lying in a general position. The isomorphous set of compounds (III)–(VIII), within which the structure is invariant to changes of either the 4f or the 3d metal, all crystallize in space group P1, with the [Ln(18-crown-6)(H2O)3]3+ cation and two noncoordinated water molecules all lying in general positions, and two independent [M(CN)6]3− anions, where M = Cr in compound (V), Fe in compounds (III), (IV), (VI) and (VIII), and Co in compound (VII), each lying across centres of inversion, selected as those at (0, 1/2, 0) and (1/2, 0, 1/2). These specifications of the special positions provide compact and connected asymmetric units for both types of salt.

In compounds (I) and (II), the lanthanoid cation exhibits ten-coordination with a geometry best described as a bicapped square antiprism, while in each of (III)–(VIII), the lanthanoid cation exhibits nine-coordination, with a monocapped square-antiprismatic geometry (Koner et al., 2005). The patterns of the O—C—C—O torsion angles, beginning at O1 and increasing monotonically, are g+gg+gg+g+ in (I) and (II), and ggg+gg+g in (III)–(VIII), indicative of the folding of the macrocycle around the Ln cation (Forsellini et al., 1985). In compounds (I) and (II), the patterns of the Ln—O bond distances (Table 3) are very similar, with the distances to water O atoms somewhat less than those to the crown ether O atoms. Likewise, within the isomorphous set (III)–(VIII), the patterns of the Ln—O distances (Table 4) are consistent from one compound to another, with again the distances to the water O atoms less than those to the crown ether O atoms. Regardless of whether we consider the mean values of all the Ln—O distances, or just the mean of those involving the crown ether, there is a monotonic decrease from left to right across the 4f series, exactly as expected and consistent with the change in coordination number from ten to nine between Nd [compound (I)] and Sm [compound (III)]. Within the subseries (V)–(VII), where the Ln—O distances are virtually identical, the mean values of the M—C distances in the anions are 2.072 (5) Å when M = Cr, 1.940 (2) Å when M = Fe and 1.893 (2) Å when M = Co; inasmuch as the anions when M = Fe or Co are expected to adopt low-spin configurations, the minimum M—C distance is expected for the d6 anion [Co(CN)6]3−, as observed.

The independent components in each of compounds (I) and (II) are linked into a three-dimensional framework structure by a combination of two O—H···O hydrogen bonds and four O—H···N hydrogen bonds, where each water molecule acts as a double donor of hydrogen bonds, and each N atom acts as an acceptor, with atom N11 acting as a double acceptor (Tables 1 and 2); it may be noted that the O atoms of the crown ether component play no part in the hydrogen bonding. Despite the number of independent hydrogen bonds, which is amplified by the symmetry properties of the ionic components, the formation of the framework structure is readily analysed in terms of simple substructures in one and two dimensions.

The anion and the two symmetry-related water molecules of the cation, those containing atom O19, generate a chain of spiro-fused R66(20) (Bernstein et al., 1995) rings running parallel to the [010] direction. Chains of this type are further linked by O—H···N hydrogen bonds to form a hydrogen-bonded sheet of anions and water molecules lying parallel to (100) and built from alternating ribbons of R55(18) and R66(20) rings (Fig. 2). The reference (100) sheet, of which water atom O20 is a component, contains the Fe atoms lying on centres of inversion at x = 1/4. This sheet is related by the twofold rotation axes at x = 0 and x = 1/2, respectively, to the sheets generated by Fe atoms lying on inversion centres at x = −1/4 and x = 3/4, respectively. Since atoms O20 and O20i [symmetry code: (i) −x, y, 1/2 − z] are both coordinated to the reference Ln atom at x = 0, these two water molecules are components of adjacent sheets which are thereby linked. In addition, adjacent sheets are also linked by a further O—H···O hydrogen bond, and these two interactions combine to generate a continuous three-dimensional framework.

The supramolecular structure of compound (VI) has already been described (Koner et al., 2005), so that the structures of the isomorphous analogues (III), (V), (VII) and (VIII) need little further discussion. However, we may note here that the one-dimensional substructures in (VI) were described erroneously (Koner et al., 2005) as double helices; they are, in fact, chains of spiro fused rings, with the points of ring fusion lying on centres of inversion, thus precluding the development of any helical structures which are necessarily chiral.

Related literature top

For related literature, see: Bernstein et al. (1995); Figuerola et al. (2003); Forsellini et al. (1985); Koner et al. (2005).

Experimental top

The dinuclear precursor compounds [Ln(DMF)4(H2O)3(µ-CN)M(CN)5].nH2O (Ln = Ce, Nd, Sm, Eu, Gd or Tb; M = Cr, Fe or Co) were prepared using a published method (Figuerola et al., 2003). For the synthesis of (I), a solution of 18-crown-6 (0.066 g, 0.25 mmol) in water (5 ml) was added dropwise to a solution of [Ce(DMF)4(H2O)3(µ-CN)M(CN)5]·H2O (0.18 g, 0.25 mmol) in water (5 ml). The mixture was stirred for 10 min and then filtered; the yellow filtrate was then set aside to crystallize at ambient temperature. After a few days, golden-yellow crystals suitable for single-crystal X-ray diffraction were deposited and collected by filtration. Compounds (II)–(V), (VII) and (VIII) were prepared in entirely analogous ways by use of the appropriate dinuclear precursor complexes. (I) Golden yellow, yield 85%; analysis found: C 29.6, H 5.1, N 11.7%; C18H36CeFeN6O12 requires: C 29.8, H 5.0, N 11.6%; IR (KBr, cm−1): 2122 m (CN) and 1081 s (CO); µeff (300 K) 3.00 BM. (II) Golden yellow, yield 80%; analysis found: C 29.5, H 4.9, N 11.6%; C18H36FeN6NdO12 requires: C 29.7, H 5.0, N 11.5%; IR (KBr, cm−1): 2122 m (CN) and 1081 s (CO); µeff (300 K) 3.92 BM. (III) Yellow, yield 75%; analysis found: C 30.3, H 4.7, N 11.8%; C18H34FeN6O11Sm requires: C 30.2, H 4.8, N 11.7%; IR (KBr, cm−1): 2124 s (CN) and 1073 s (CO); µeff (300 K) 2.55 BM. (IV) Yellow, yield 88%; analysis found: C 30.2, H 4.7, N 11.6%; C18H34EuFeN6O11 requires: C 30.1, H 4.8, N 11.7%; IR (KBr, cm−1) 2124 m (CN) and 1073 s (CO); µeff (300 K) 3.76 BM. (V) Pale yellow [colourless in CIF?], yield 82%; analysis found: C 29.9, H 4.7, N 11.8%; C18H34CrGdN6O11 requires: C 30.0, H 4.8, N 11.7%; IR (KBr, cm−1) 2138 m (CN) and 1073 s (CO); µeff (300 K) 8.72 BM. (VII) Colourless, yield 90%; analysis found: C 29.9, H 4.6, N 11.6%; C18H34CoGdN6O11 requires: C 29.8, H 4.7, N 11.6%; IR (KBr, cm−1) 2137 s (CN) and 1073 s (CO); µeff (300 K) 7.62 BM. (VIII) Yellow, yield 80%: analysis found: C 29.7, H 4.7, N 11.7%; C18H34FeN6O11Tb requires: C 29.8, H 4.7, N 11.6%; IR (KBr, cm−1) 2125 m (CN) and 1072 s (CO); µeff (300 K) 9.78 BM.

Refinement top

For compounds (I) and (II), the systematic absences permitted Cc and C2/c as possible space groups; C2/c was selected, and confirmed by the subsequent structure analyses. Crystals of compounds (III)–(V), (VII) and (VIII) are all triclinic; space group P1 was selected for each, and confirmed by the subsequent structure analyses. All H atoms were located in difference maps. Those bonded to C atoms were treated as riding atoms with a C—H distance of 0.99 Å and Uiso(H) = 1.2Ueq(C); those bonded to O were allowed to ride at the positions deduced from difference maps, with a common Uiso(H) value for each compound, giving a range of O—H distances of 0.80–0.89 Å. In compounds (II), (IV), (V) and (VII), atoms C2 and C18 bonded to O1 are each disordered over two sites. This was allowed for with both components of these atoms refined isotropically; the final linked occupancy parameters for these disordered atoms are as follows: (III) 0.815 (7):0.185 (7), (IV) 0.762 (14):0.238 (14), (V) 0.542 (7):0.458 (7) and (VII) 0.777 (6):0.223 (6). The maximum difference density in compound (IV), 11.1 e Å−3, is located 0.91 Å from the Eu atom. For compound (VIII), where the unit-cell dimensions are a = 11.1302 (4) Å, b = 11.2341 (4) Å, c = 13.9408 (5) Å, α = 69.778 (2)°, β = 68.585 (3)° and γ = 62.425 (2)°, we were unable to reduce the R factor below 11%, although (VIII) is clearly isostructural with compounds (III)–(VII); no attempt was made to model any disorder of the macrocyclic ligand, and we do not report any further structural details here.

Computing details top

For all compounds, data collection: COLLECT (Hooft, 1999); cell refinement: DENZO (Otwinowski & Minor, 1997) and COLLECT; data reduction: DENZO and COLLECT; program(s) used to solve structure: OSCAIL (McArdle, 2003) and SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: OSCAIL and SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97 and PRPKAPPA (Ferguson, 1999).

Figures top
[Figure 1] Fig. 1. The independent components of (I), showing the atom-labelling scheme. Atoms marked a or b are at the symmetry positions (−x, y, 1/2 − z) and (1/2 − x, 1/2 − y, −z), respectively. Displacement ellipsoids are drawn at the 30% probability level. Compound (II) is isomorphous and isostructural with (I).
[Figure 2] Fig. 2. A stereoview of part of the crystal structure of (I), showing the formation of a hydrogen-bonded sheet parallel to (100) and built from hexacyanoferrate(III) anions and water molecules only.
(I) Tetraaqua(18-crown-6)cerium(III) hexacyanoferrate(III) dihydrate top
Crystal data top
[Ce(C12H24O6)(H2O)4][Fe(CN)6]·2H2OF(000) = 1464
Mr = 724.50Dx = 1.627 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 3385 reflections
a = 19.8534 (6) Åθ = 3.4–27.5°
b = 11.5705 (2) ŵ = 2.07 mm1
c = 14.0258 (4) ÅT = 120 K
β = 113.3930 (13)°Block, yellow
V = 2957.09 (13) Å30.20 × 0.10 × 0.10 mm
Z = 4
Data collection top
Bruker–Nonius KappaCCD
diffractometer
3385 independent reflections
Radiation source: Bruker-Nonius FR591 rotating anode3079 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.036
Detector resolution: 9.091 pixels mm-1θmax = 27.5°, θmin = 3.4°
ϕ & ω scansh = 2525
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
k = 1415
Tmin = 0.682, Tmax = 0.820l = 1818
15557 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.023H-atom parameters constrained
wR(F2) = 0.049 w = 1/[σ2(Fo2) + (0.0144P)2 + 2.9468P]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max = 0.001
3385 reflectionsΔρmax = 0.81 e Å3
176 parametersΔρmin = 0.87 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00166 (8)
Crystal data top
[Ce(C12H24O6)(H2O)4][Fe(CN)6]·2H2OV = 2957.09 (13) Å3
Mr = 724.50Z = 4
Monoclinic, C2/cMo Kα radiation
a = 19.8534 (6) ŵ = 2.07 mm1
b = 11.5705 (2) ÅT = 120 K
c = 14.0258 (4) Å0.20 × 0.10 × 0.10 mm
β = 113.3930 (13)°
Data collection top
Bruker–Nonius KappaCCD
diffractometer
3385 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
3079 reflections with I > 2σ(I)
Tmin = 0.682, Tmax = 0.820Rint = 0.036
15557 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0230 restraints
wR(F2) = 0.049H-atom parameters constrained
S = 1.09Δρmax = 0.81 e Å3
3385 reflectionsΔρmin = 0.87 e Å3
176 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ce10.00000.234944 (13)0.25000.01137 (7)
O10.07320 (7)0.42168 (11)0.32310 (10)0.0161 (3)
C20.14240 (11)0.44021 (17)0.31446 (16)0.0179 (4)
C30.18455 (11)0.32906 (17)0.33975 (17)0.0224 (5)
O40.14017 (8)0.24169 (11)0.27090 (11)0.0175 (3)
C50.17858 (12)0.13413 (18)0.28102 (19)0.0253 (5)
C60.12504 (12)0.04820 (18)0.21163 (19)0.0254 (5)
O70.06382 (7)0.04500 (11)0.24187 (11)0.0174 (3)
C80.02244 (12)0.06091 (18)0.21778 (19)0.0269 (5)
C180.02867 (12)0.52538 (16)0.30468 (16)0.0197 (5)
O190.02820 (7)0.31805 (13)0.10237 (10)0.0221 (3)
O200.08468 (8)0.17105 (12)0.42718 (11)0.0229 (3)
Fe10.25000.25000.00000.00981 (9)
N110.14808 (10)0.41328 (15)0.05656 (14)0.0220 (4)
C110.18455 (11)0.35034 (16)0.03461 (15)0.0146 (4)
N120.16334 (10)0.02792 (15)0.00100 (14)0.0222 (4)
C120.19468 (11)0.11178 (17)0.00123 (15)0.0147 (4)
N130.15844 (10)0.27245 (14)0.23566 (13)0.0192 (4)
C130.19222 (11)0.26503 (15)0.14782 (16)0.0135 (4)
O210.09957 (8)0.64744 (12)0.06265 (10)0.0232 (3)
H2A0.17050.50150.36330.022*
H2B0.13390.46500.24300.022*
H3A0.23130.33800.33070.027*
H3B0.19610.30710.41280.027*
H5A0.19780.10720.35400.030*
H5B0.22040.14390.26020.030*
H6A0.10860.07200.13800.030*
H6B0.14810.02910.21990.030*
H8A0.05580.12840.23530.032*
H8B0.00980.06420.14290.032*
H18A0.06030.59450.31580.024*
H18B0.00460.52860.35440.024*
H19A0.00490.33040.04620.046*
H19B0.06770.33400.10110.046*
H20A0.09490.21980.47300.046*
H20B0.11000.11460.45520.046*
H21A0.11570.66660.12420.046*
H21B0.11380.58230.05800.046*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ce10.01244 (10)0.01085 (10)0.01076 (10)0.0000.00456 (7)0.000
O10.0137 (7)0.0141 (7)0.0188 (8)0.0003 (6)0.0047 (6)0.0003 (5)
C20.0154 (11)0.0160 (10)0.0222 (12)0.0064 (8)0.0073 (9)0.0014 (8)
C30.0155 (11)0.0228 (12)0.0260 (12)0.0046 (9)0.0050 (10)0.0006 (9)
O40.0146 (7)0.0150 (7)0.0230 (8)0.0003 (6)0.0076 (6)0.0003 (5)
C50.0206 (12)0.0197 (11)0.0421 (15)0.0069 (9)0.0193 (11)0.0071 (10)
C60.0296 (13)0.0191 (11)0.0386 (14)0.0032 (10)0.0254 (11)0.0014 (10)
O70.0185 (8)0.0127 (7)0.0242 (8)0.0000 (6)0.0119 (7)0.0022 (6)
C80.0212 (12)0.0113 (10)0.0460 (15)0.0011 (9)0.0110 (11)0.0079 (9)
C180.0204 (11)0.0123 (10)0.0253 (12)0.0003 (9)0.0079 (9)0.0029 (8)
O190.0150 (8)0.0337 (9)0.0155 (8)0.0047 (7)0.0038 (6)0.0040 (6)
O200.0315 (9)0.0178 (8)0.0150 (8)0.0099 (7)0.0046 (7)0.0004 (6)
Fe10.0104 (2)0.0101 (2)0.0091 (2)0.00070 (14)0.00391 (16)0.00008 (13)
N110.0239 (10)0.0220 (10)0.0216 (10)0.0036 (8)0.0105 (8)0.0014 (7)
C110.0169 (11)0.0129 (10)0.0125 (10)0.0019 (8)0.0042 (9)0.0030 (7)
N120.0289 (11)0.0193 (10)0.0201 (10)0.0089 (8)0.0115 (8)0.0037 (7)
C120.0164 (10)0.0160 (10)0.0115 (10)0.0016 (9)0.0054 (8)0.0008 (8)
N130.0222 (10)0.0176 (9)0.0151 (10)0.0036 (8)0.0045 (8)0.0009 (7)
C130.0155 (10)0.0097 (9)0.0173 (11)0.0017 (8)0.0087 (9)0.0005 (7)
O210.0330 (9)0.0183 (8)0.0126 (8)0.0039 (7)0.0030 (7)0.0009 (6)
Geometric parameters (Å, º) top
Ce1—O20i2.4962 (14)C6—H6B0.99
Ce1—O202.4962 (14)O7—C81.439 (2)
Ce1—O19i2.5389 (14)C8—C8i1.500 (5)
Ce1—O192.5389 (14)C8—H8A0.99
Ce1—O7i2.5619 (13)C8—H8B0.99
Ce1—O72.5619 (13)C18—C18i1.504 (4)
Ce1—O12.5784 (13)C18—H18A0.99
Ce1—O1i2.5784 (13)C18—H18B0.99
Ce1—O4i2.6811 (14)O19—H19A0.81
Ce1—O42.6811 (14)O19—H19B0.81
O1—C21.442 (2)O20—H20A0.82
O1—C181.451 (2)O20—H20B0.82
C2—C31.498 (3)Fe1—C13ii1.938 (2)
C2—H2A0.99Fe1—C131.938 (2)
C2—H2B0.99Fe1—C11ii1.942 (2)
C3—O41.434 (2)Fe1—C111.942 (2)
C3—H3A0.99Fe1—C12ii1.944 (2)
C3—H3B0.99Fe1—C121.944 (2)
O4—C51.437 (2)N11—C111.152 (3)
C5—C61.498 (3)N12—C121.146 (2)
C5—H5A0.99N13—C131.148 (3)
C5—H5B0.99O21—H21A0.82
C6—O71.438 (2)O21—H21B0.82
C6—H6A0.99
O20i—Ce1—O20145.54 (6)C2—C3—H3B110.1
O20i—Ce1—O19i130.14 (5)H3A—C3—H3B108.4
O20—Ce1—O19i65.14 (4)C3—O4—C5112.58 (16)
O20i—Ce1—O1965.14 (4)C3—O4—Ce1115.33 (11)
O20—Ce1—O19130.14 (5)C5—O4—Ce1118.21 (11)
O19i—Ce1—O19135.49 (7)O4—C5—C6107.39 (17)
O20i—Ce1—O7i68.95 (4)O4—C5—H5A110.2
O20—Ce1—O7i81.44 (5)C6—C5—H5A110.2
O19i—Ce1—O7i90.89 (5)O4—C5—H5B110.2
O19—Ce1—O7i129.37 (5)C6—C5—H5B110.2
O20i—Ce1—O781.44 (5)H5A—C5—H5B108.5
O20—Ce1—O768.95 (4)O7—C6—C5106.88 (17)
O19i—Ce1—O7129.37 (5)O7—C6—H6A110.3
O19—Ce1—O790.89 (5)C5—C6—H6A110.3
O7i—Ce1—O761.85 (6)O7—C6—H6B110.3
O20i—Ce1—O1133.99 (4)C5—C6—H6B110.3
O20—Ce1—O178.57 (4)H6A—C6—H6B108.6
O19i—Ce1—O168.30 (5)C6—O7—C8115.05 (15)
O19—Ce1—O174.63 (4)C6—O7—Ce1118.81 (11)
O7i—Ce1—O1155.75 (4)C8—O7—Ce1119.65 (11)
O7—Ce1—O1121.73 (4)O7—C8—C8i106.20 (15)
O20i—Ce1—O1i78.57 (4)O7—C8—H8A110.5
O20—Ce1—O1i133.99 (4)C8i—C8—H8A110.5
O19i—Ce1—O1i74.63 (4)O7—C8—H8B110.5
O19—Ce1—O1i68.30 (5)C8i—C8—H8B110.5
O7i—Ce1—O1i121.73 (4)H8A—C8—H8B108.7
O7—Ce1—O1i155.75 (4)O1—C18—C18i110.03 (14)
O1—Ce1—O1i66.15 (6)O1—C18—H18A109.7
O20i—Ce1—O4i68.92 (5)C18i—C18—H18A109.7
O20—Ce1—O4i112.15 (5)O1—C18—H18B109.7
O19i—Ce1—O4i61.50 (4)C18i—C18—H18B109.7
O19—Ce1—O4i117.08 (4)H18A—C18—H18B108.2
O7i—Ce1—O4i61.29 (4)Ce1—O19—H19A120.1
O7—Ce1—O4i122.03 (4)Ce1—O19—H19B129.1
O1—Ce1—O4i114.57 (4)H19A—O19—H19B110.8
O1i—Ce1—O4i62.32 (4)Ce1—O20—H20A115.9
O20i—Ce1—O4112.15 (5)Ce1—O20—H20B138.9
O20—Ce1—O468.92 (5)H20A—O20—H20B105.0
O19i—Ce1—O4117.08 (4)C13ii—Fe1—C13180.00 (10)
O19—Ce1—O461.50 (4)C13ii—Fe1—C11ii92.48 (8)
O7i—Ce1—O4122.03 (4)C13—Fe1—C11ii87.52 (8)
O7—Ce1—O461.29 (4)C13ii—Fe1—C1187.52 (8)
O1—Ce1—O462.32 (4)C13—Fe1—C1192.48 (8)
O1i—Ce1—O4114.57 (4)C11ii—Fe1—C11180.00 (11)
O4i—Ce1—O4176.66 (5)C13ii—Fe1—C12ii89.24 (8)
C2—O1—C18113.28 (15)C13—Fe1—C12ii90.76 (8)
C2—O1—Ce1119.76 (11)C11ii—Fe1—C12ii93.04 (8)
C18—O1—Ce1114.50 (11)C11—Fe1—C12ii86.96 (8)
O1—C2—C3108.28 (16)C13ii—Fe1—C1290.76 (8)
O1—C2—H2A110.0C13—Fe1—C1289.24 (8)
C3—C2—H2A110.0C11ii—Fe1—C1286.96 (8)
O1—C2—H2B110.0C11—Fe1—C1293.04 (8)
C3—C2—H2B110.0C12ii—Fe1—C12180.00 (12)
H2A—C2—H2B108.4N11—C11—Fe1177.10 (18)
O4—C3—C2108.04 (16)N12—C12—Fe1176.85 (18)
O4—C3—H3A110.1N13—C13—Fe1178.99 (19)
C2—C3—H3A110.1H21A—O21—H21B109.3
O4—C3—H3B110.1
O20i—Ce1—O1—C281.07 (14)O19i—Ce1—O4—C5113.47 (14)
O20—Ce1—O1—C285.86 (13)O19—Ce1—O4—C5117.20 (15)
O19i—Ce1—O1—C2153.46 (13)O7i—Ce1—O4—C53.57 (15)
O19—Ce1—O1—C251.68 (13)O7—Ce1—O4—C58.69 (13)
O7i—Ce1—O1—C2120.90 (14)O1—Ce1—O4—C5155.99 (15)
O7—Ce1—O1—C229.64 (14)O1i—Ce1—O4—C5161.90 (13)
O1i—Ce1—O1—C2124.35 (15)C3—O4—C5—C6175.74 (17)
O4i—Ce1—O1—C2164.84 (12)Ce1—O4—C5—C637.2 (2)
O4—Ce1—O1—C213.82 (12)O4—C5—C6—O755.8 (2)
O20i—Ce1—O1—C1858.48 (14)C5—C6—O7—C8155.13 (18)
O20—Ce1—O1—C18134.59 (13)C5—C6—O7—Ce153.2 (2)
O19i—Ce1—O1—C1866.99 (12)O20i—Ce1—O7—C696.62 (14)
O19—Ce1—O1—C1887.88 (13)O20—Ce1—O7—C6101.31 (14)
O7i—Ce1—O1—C1899.55 (15)O19i—Ce1—O7—C6127.35 (14)
O7—Ce1—O1—C18169.19 (12)O19—Ce1—O7—C631.92 (14)
O1i—Ce1—O1—C1815.20 (10)O7i—Ce1—O7—C6167.26 (17)
O4i—Ce1—O1—C1825.29 (13)O1—Ce1—O7—C640.50 (15)
O4—Ce1—O1—C18153.37 (14)O1i—Ce1—O7—C661.93 (18)
C18—O1—C2—C3177.45 (16)O4i—Ce1—O7—C6155.06 (13)
Ce1—O1—C2—C342.55 (19)O4—Ce1—O7—C624.53 (13)
O1—C2—C3—O456.6 (2)O20i—Ce1—O7—C853.73 (15)
C2—C3—O4—C5173.73 (17)O20—Ce1—O7—C8108.34 (15)
C2—C3—O4—Ce146.52 (19)O19i—Ce1—O7—C882.30 (15)
O20i—Ce1—O4—C3147.88 (12)O19—Ce1—O7—C8118.43 (15)
O20—Ce1—O4—C369.25 (13)O7i—Ce1—O7—C816.91 (12)
O19i—Ce1—O4—C323.93 (14)O1—Ce1—O7—C8169.16 (14)
O19—Ce1—O4—C3105.40 (13)O1i—Ce1—O7—C888.42 (17)
O7i—Ce1—O4—C3133.82 (12)O4i—Ce1—O7—C84.71 (16)
O7—Ce1—O4—C3146.08 (14)O4—Ce1—O7—C8174.87 (16)
O1—Ce1—O4—C318.59 (12)C6—O7—C8—C8i163.3 (2)
O1i—Ce1—O4—C360.70 (13)Ce1—O7—C8—C8i45.3 (3)
O20i—Ce1—O4—C574.72 (14)C2—O1—C18—C18i99.3 (2)
O20—Ce1—O4—C568.14 (14)Ce1—O1—C18—C18i42.9 (2)
Symmetry codes: (i) x, y, z+1/2; (ii) x+1/2, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O19—H19A···O21iii0.811.912.700 (2)163
O19—H19B···N110.812.142.917 (2)161
O20—H20A···O21iv0.821.962.768 (2)168
O20—H20B···N12v0.821.922.739 (2)171
O21—H21A···N13iv0.821.942.757 (2)173
O21—H21B···N110.822.072.888 (2)175
Symmetry codes: (iii) x, y+1, z; (iv) x, y+1, z+1/2; (v) x, y, z+1/2.
(II) Tetraaqua(18-crown-6)neodymium(III) hexacyanoferrate(III) dihydrate top
Crystal data top
[Nd(C12H24O6)(H2O)4][Fe(CN)6]·2H2OF(000) = 1472
Mr = 728.62Dx = 1.644 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 3360 reflections
a = 19.9552 (6) Åθ = 3.4–27.5°
b = 11.5063 (2) ŵ = 2.30 mm1
c = 13.9706 (3) ÅT = 120 K
β = 113.4189 (11)°Block, yellow
V = 2943.55 (12) Å30.34 × 0.34 × 0.25 mm
Z = 4
Data collection top
Bruker–Nonius KappaCCD
diffractometer
3360 independent reflections
Radiation source: Bruker-Nonius FR591 rotating anode3168 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
Detector resolution: 9.091 pixels mm-1θmax = 27.5°, θmin = 3.4°
ϕ & ω scansh = 2525
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
k = 1414
Tmin = 0.478, Tmax = 0.561l = 1718
21701 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.018H-atom parameters constrained
wR(F2) = 0.043 w = 1/[σ2(Fo2) + (0.0166P)2 + 4.6543P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.001
3360 reflectionsΔρmax = 0.83 e Å3
176 parametersΔρmin = 1.07 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00110 (7)
Crystal data top
[Nd(C12H24O6)(H2O)4][Fe(CN)6]·2H2OV = 2943.55 (12) Å3
Mr = 728.62Z = 4
Monoclinic, C2/cMo Kα radiation
a = 19.9552 (6) ŵ = 2.30 mm1
b = 11.5063 (2) ÅT = 120 K
c = 13.9706 (3) Å0.34 × 0.34 × 0.25 mm
β = 113.4189 (11)°
Data collection top
Bruker–Nonius KappaCCD
diffractometer
3360 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
3168 reflections with I > 2σ(I)
Tmin = 0.478, Tmax = 0.561Rint = 0.031
21701 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0180 restraints
wR(F2) = 0.043H-atom parameters constrained
S = 1.06Δρmax = 0.83 e Å3
3360 reflectionsΔρmin = 1.07 e Å3
176 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Nd10.00000.235995 (11)0.25000.01047 (6)
O10.07244 (6)0.42143 (10)0.32299 (9)0.0147 (3)
C20.14156 (10)0.44074 (16)0.31489 (15)0.0184 (4)
C30.18301 (10)0.32854 (16)0.33869 (15)0.0210 (4)
O40.13804 (7)0.24246 (10)0.26887 (10)0.0171 (3)
C50.17568 (10)0.13461 (16)0.27458 (17)0.0235 (4)
C60.12105 (11)0.05085 (17)0.20432 (17)0.0252 (4)
O70.06155 (7)0.04755 (11)0.23773 (10)0.0174 (3)
C80.02092 (11)0.05890 (16)0.21581 (18)0.0265 (5)
C180.02852 (10)0.52602 (15)0.30506 (15)0.0190 (4)
O190.02701 (7)0.31846 (12)0.10311 (10)0.0208 (3)
O200.08381 (7)0.17143 (11)0.42465 (10)0.0208 (3)
Fe10.25000.25000.00000.00844 (8)
N110.14676 (9)0.40933 (14)0.05722 (13)0.0209 (3)
C110.18383 (9)0.34807 (15)0.03506 (13)0.0140 (3)
N120.16593 (9)0.02424 (14)0.00129 (12)0.0214 (3)
C120.19654 (9)0.10940 (15)0.00127 (13)0.0135 (3)
N130.15783 (9)0.27066 (14)0.23642 (12)0.0194 (3)
C130.19176 (9)0.26363 (14)0.14838 (14)0.0126 (3)
O210.10008 (7)0.64648 (11)0.06217 (10)0.0225 (3)
H2A0.16970.50140.36500.022*
H2B0.13330.46710.24360.022*
H3A0.22930.33730.32910.025*
H3B0.19480.30540.41180.025*
H5A0.19610.10510.34710.028*
H5B0.21620.14570.25160.028*
H6A0.10360.07700.13090.030*
H6B0.14310.02730.20990.030*
H8A0.05430.12650.23180.032*
H8B0.01280.06250.14140.032*
H18A0.06010.59540.31640.023*
H18B0.00450.52930.35490.023*
H19A0.00490.33040.04620.046*
H19B0.06770.33400.10110.046*
H20A0.09490.21980.47300.046*
H20B0.11000.11460.45520.046*
H21A0.11570.66660.12420.046*
H21B0.11380.58230.05800.046*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nd10.01103 (8)0.01016 (8)0.00979 (8)0.0000.00369 (5)0.000
O10.0128 (6)0.0130 (6)0.0169 (6)0.0010 (4)0.0044 (5)0.0001 (5)
C20.0153 (9)0.0184 (9)0.0210 (10)0.0055 (7)0.0068 (8)0.0009 (7)
C30.0125 (9)0.0228 (10)0.0246 (10)0.0037 (7)0.0040 (8)0.0003 (8)
O40.0134 (6)0.0160 (7)0.0216 (7)0.0010 (4)0.0065 (5)0.0011 (5)
C50.0186 (9)0.0200 (10)0.0381 (12)0.0047 (7)0.0179 (9)0.0050 (8)
C60.0289 (11)0.0215 (10)0.0357 (12)0.0039 (8)0.0238 (10)0.0008 (8)
O70.0180 (6)0.0128 (6)0.0240 (7)0.0001 (5)0.0112 (6)0.0029 (5)
C80.0202 (10)0.0123 (9)0.0453 (13)0.0006 (7)0.0111 (9)0.0070 (8)
C180.0188 (9)0.0114 (9)0.0235 (10)0.0004 (7)0.0050 (8)0.0021 (7)
O190.0158 (6)0.0315 (8)0.0137 (6)0.0044 (5)0.0043 (5)0.0044 (5)
O200.0299 (7)0.0156 (7)0.0126 (6)0.0098 (5)0.0039 (6)0.0009 (5)
Fe10.00896 (16)0.00895 (17)0.00733 (16)0.00085 (11)0.00316 (13)0.00016 (11)
N110.0225 (8)0.0214 (8)0.0215 (8)0.0037 (6)0.0118 (7)0.0008 (7)
C110.0157 (8)0.0141 (8)0.0113 (8)0.0015 (6)0.0045 (7)0.0023 (6)
N120.0270 (9)0.0198 (8)0.0194 (8)0.0086 (7)0.0114 (7)0.0032 (6)
C120.0151 (8)0.0160 (9)0.0090 (8)0.0001 (7)0.0044 (7)0.0017 (6)
N130.0232 (8)0.0185 (8)0.0133 (8)0.0043 (6)0.0039 (7)0.0012 (6)
C130.0143 (8)0.0097 (8)0.0148 (9)0.0013 (6)0.0067 (7)0.0005 (6)
O210.0320 (8)0.0181 (7)0.0110 (6)0.0047 (5)0.0019 (6)0.0009 (5)
Geometric parameters (Å, º) top
Nd1—O20i2.4615 (12)C6—H6B0.99
Nd1—O202.4615 (12)O7—C81.433 (2)
Nd1—O19i2.5062 (12)C8—C8i1.498 (4)
Nd1—O192.5062 (12)C8—H8A0.99
Nd1—O7i2.5312 (12)C8—H8B0.99
Nd1—O72.5312 (12)C18—C18i1.507 (4)
Nd1—O12.5515 (12)C18—H18A0.99
Nd1—O1i2.5515 (12)C18—H18B0.99
Nd1—O4i2.6620 (13)O19—H19A0.81
Nd1—O42.6620 (13)O19—H19B0.84
O1—C21.445 (2)O20—H20A0.83
O1—C181.451 (2)O20—H20B0.84
C2—C31.498 (3)Fe1—C131.9384 (18)
C2—H2A0.99Fe1—C13ii1.9384 (18)
C2—H2B0.99Fe1—C121.9418 (17)
C3—O41.429 (2)Fe1—C12ii1.9418 (17)
C3—H3A0.99Fe1—C11ii1.9419 (18)
C3—H3B0.99Fe1—C111.9419 (18)
O4—C51.436 (2)N11—C111.150 (2)
C5—C61.493 (3)N12—C121.148 (2)
C5—H5A0.99N13—C131.147 (2)
C5—H5B0.99O21—H21A0.83
C6—O71.439 (2)O21—H21B0.80
C6—H6A0.99
O20i—Nd1—O20144.86 (6)C2—C3—H3B110.2
O20i—Nd1—O19i130.05 (4)H3A—C3—H3B108.5
O20—Nd1—O19i65.49 (4)C3—O4—C5112.85 (14)
O20i—Nd1—O1965.49 (4)C3—O4—Nd1115.55 (10)
O20—Nd1—O19130.05 (4)C5—O4—Nd1118.62 (10)
O19i—Nd1—O19135.51 (6)O4—C5—C6106.99 (15)
O20i—Nd1—O7i69.62 (4)O4—C5—H5A110.3
O20—Nd1—O7i80.28 (4)C6—C5—H5A110.3
O19i—Nd1—O7i90.05 (4)O4—C5—H5B110.3
O19—Nd1—O7i130.38 (4)C6—C5—H5B110.3
O20i—Nd1—O780.28 (4)H5A—C5—H5B108.6
O20—Nd1—O769.62 (4)O7—C6—C5106.54 (15)
O19i—Nd1—O7130.38 (4)O7—C6—H6A110.4
O19—Nd1—O790.05 (4)C5—C6—H6A110.4
O7i—Nd1—O762.11 (6)O7—C6—H6B110.4
O20i—Nd1—O1134.62 (4)C5—C6—H6B110.4
O20—Nd1—O178.60 (4)H6A—C6—H6B108.6
O19i—Nd1—O168.18 (4)C8—O7—C6115.02 (14)
O19—Nd1—O174.85 (4)C8—O7—Nd1119.88 (10)
O7i—Nd1—O1154.47 (4)C6—O7—Nd1118.99 (10)
O7—Nd1—O1122.03 (4)O7—C8—C8i105.96 (14)
O20i—Nd1—O1i78.60 (4)O7—C8—H8A110.5
O20—Nd1—O1i134.62 (4)C8i—C8—H8A110.5
O19i—Nd1—O1i74.85 (4)O7—C8—H8B110.5
O19—Nd1—O1i68.18 (4)C8i—C8—H8B110.5
O7i—Nd1—O1i122.03 (4)H8A—C8—H8B108.7
O7—Nd1—O1i154.47 (4)O1—C18—C18i109.61 (12)
O1—Nd1—O1i66.51 (5)O1—C18—H18A109.7
O20i—Nd1—O4i69.00 (4)C18i—C18—H18A109.7
O20—Nd1—O4i112.04 (4)O1—C18—H18B109.7
O19i—Nd1—O4i61.29 (4)C18i—C18—H18B109.7
O19—Nd1—O4i117.33 (4)H18A—C18—H18B108.2
O7i—Nd1—O4i61.30 (4)Nd1—O19—H19A121.8
O7—Nd1—O4i121.88 (4)Nd1—O19—H19B129.1
O1—Nd1—O4i114.57 (4)H19A—O19—H19B109.0
O1i—Nd1—O4i62.45 (4)Nd1—O20—H20A117.3
O20i—Nd1—O4112.04 (4)Nd1—O20—H20B141.2
O20—Nd1—O469.00 (4)H20A—O20—H20B101.4
O19i—Nd1—O4117.33 (4)C13—Fe1—C13ii180.00 (11)
O19—Nd1—O461.29 (4)C13—Fe1—C1288.80 (7)
O7i—Nd1—O4121.88 (4)C13ii—Fe1—C1291.20 (7)
O7—Nd1—O461.30 (4)C13—Fe1—C12ii91.20 (7)
O1—Nd1—O462.45 (4)C13ii—Fe1—C12ii88.80 (7)
O1i—Nd1—O4114.57 (4)C12—Fe1—C12ii180.00 (11)
O4i—Nd1—O4176.80 (5)C13—Fe1—C11ii87.48 (7)
C2—O1—C18112.88 (13)C13ii—Fe1—C11ii92.52 (7)
C2—O1—Nd1120.27 (10)C12—Fe1—C11ii87.09 (7)
C18—O1—Nd1114.66 (9)C12ii—Fe1—C11ii92.91 (7)
O1—C2—C3108.07 (14)C13—Fe1—C1192.52 (7)
O1—C2—H2A110.1C13ii—Fe1—C1187.48 (7)
C3—C2—H2A110.1C12—Fe1—C1192.91 (7)
O1—C2—H2B110.1C12ii—Fe1—C1187.09 (7)
C3—C2—H2B110.1C11ii—Fe1—C11180.00 (9)
H2A—C2—H2B108.4N11—C11—Fe1177.35 (16)
O4—C3—C2107.72 (14)N12—C12—Fe1176.93 (16)
O4—C3—H3A110.2N13—C13—Fe1179.14 (17)
C2—C3—H3A110.2H21A—O21—H21B109.7
O4—C3—H3B110.2
O20i—Nd1—O1—C281.42 (13)O19i—Nd1—O4—C5115.81 (13)
O20—Nd1—O1—C285.26 (12)O19—Nd1—O4—C5114.95 (14)
O19i—Nd1—O1—C2153.22 (12)O7i—Nd1—O4—C57.00 (14)
O19—Nd1—O1—C252.01 (11)O7—Nd1—O4—C57.44 (12)
O7i—Nd1—O1—C2119.99 (13)O1—Nd1—O4—C5157.94 (14)
O7—Nd1—O1—C228.29 (13)O1i—Nd1—O4—C5159.19 (12)
O1i—Nd1—O1—C2124.42 (13)C3—O4—C5—C6175.73 (15)
O4i—Nd1—O1—C2165.54 (11)Nd1—O4—C5—C635.97 (19)
O4—Nd1—O1—C213.15 (11)O4—C5—C6—O755.2 (2)
O20i—Nd1—O1—C1858.33 (13)C5—C6—O7—C8153.11 (16)
O20—Nd1—O1—C18134.98 (12)C5—C6—O7—Nd154.39 (18)
O19i—Nd1—O1—C1867.02 (11)O20i—Nd1—O7—C855.06 (14)
O19—Nd1—O1—C1887.74 (11)O20—Nd1—O7—C8106.52 (14)
O7i—Nd1—O1—C18100.25 (13)O19i—Nd1—O7—C880.28 (14)
O7—Nd1—O1—C18168.05 (10)O19—Nd1—O7—C8120.16 (14)
O1i—Nd1—O1—C1815.34 (9)O7i—Nd1—O7—C816.94 (11)
O4i—Nd1—O1—C1825.79 (12)O1—Nd1—O7—C8167.77 (13)
O4—Nd1—O1—C18152.91 (12)O1i—Nd1—O7—C889.58 (16)
C18—O1—C2—C3177.91 (14)O4i—Nd1—O7—C82.61 (15)
Nd1—O1—C2—C341.69 (17)O4—Nd1—O7—C8176.92 (15)
O1—C2—C3—O455.92 (19)O20i—Nd1—O7—C696.09 (13)
C2—C3—O4—C5172.09 (15)O20—Nd1—O7—C6102.33 (13)
C2—C3—O4—Nd146.86 (17)O19i—Nd1—O7—C6128.58 (12)
O20i—Nd1—O4—C3149.28 (11)O19—Nd1—O7—C630.99 (13)
O20—Nd1—O4—C368.57 (12)O7i—Nd1—O7—C6168.08 (16)
O19i—Nd1—O4—C322.89 (13)O1—Nd1—O7—C641.08 (14)
O19—Nd1—O4—C3106.34 (12)O1i—Nd1—O7—C661.57 (16)
O7i—Nd1—O4—C3131.71 (11)O4i—Nd1—O7—C6153.76 (12)
O7—Nd1—O4—C3146.15 (13)O4—Nd1—O7—C625.78 (12)
O1—Nd1—O4—C319.23 (11)C6—O7—C8—C8i162.68 (18)
O1i—Nd1—O4—C362.10 (12)Nd1—O7—C8—C8i45.1 (2)
O20i—Nd1—O4—C572.01 (13)C2—O1—C18—C18i99.72 (19)
O20—Nd1—O4—C570.14 (13)Nd1—O1—C18—C18i43.0 (2)
Symmetry codes: (i) x, y, z+1/2; (ii) x+1/2, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O19—H19A···O21iii0.811.922.697 (2)161
O19—H19B···N110.842.092.904 (2)161
O20—H20A···O21iv0.831.962.773 (2)166
O20—H20B···N12v0.841.902.734 (2)169
O21—H21A···N13iv0.831.932.753 (2)173
O21—H21B···N110.802.102.893 (2)175
Symmetry codes: (iii) x, y+1, z; (iv) x, y+1, z+1/2; (v) x, y, z+1/2.
(III) Triaqua(18-crown-6)samarium(III) hexacyanoferrate(III) dihydrate top
Crystal data top
[Sm(C12H24O6)(H2O)3][Fe(CN)6]·2H2OZ = 2
Mr = 716.71F(000) = 720
Triclinic, P1Dx = 1.694 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.9324 (2) ÅCell parameters from 6393 reflections
b = 11.0996 (2) Åθ = 2.9–27.5°
c = 14.0119 (4) ŵ = 2.65 mm1
α = 67.9012 (13)°T = 120 K
β = 70.7291 (13)°Block, yellow
γ = 65.7231 (14)°0.10 × 0.06 × 0.04 mm
V = 1404.77 (6) Å3
Data collection top
Bruker–Nonius KappaCCD
diffractometer
6453 independent reflections
Radiation source: Bruker–Nonius FR591 rotating anode5624 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.050
Detector resolution: 9.091 pixels mm-1θmax = 27.5°, θmin = 3.4°
ϕ & ω scansh = 1414
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
k = 1414
Tmin = 0.836, Tmax = 0.900l = 1818
28348 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.067H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0254P)2 + 2.0082P]
where P = (Fo2 + 2Fc2)/3
6453 reflections(Δ/σ)max = 0.001
334 parametersΔρmax = 0.95 e Å3
8 restraintsΔρmin = 0.91 e Å3
Crystal data top
[Sm(C12H24O6)(H2O)3][Fe(CN)6]·2H2Oγ = 65.7231 (14)°
Mr = 716.71V = 1404.77 (6) Å3
Triclinic, P1Z = 2
a = 10.9324 (2) ÅMo Kα radiation
b = 11.0996 (2) ŵ = 2.65 mm1
c = 14.0119 (4) ÅT = 120 K
α = 67.9012 (13)°0.10 × 0.06 × 0.04 mm
β = 70.7291 (13)°
Data collection top
Bruker–Nonius KappaCCD
diffractometer
6453 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
5624 reflections with I > 2σ(I)
Tmin = 0.836, Tmax = 0.900Rint = 0.050
28348 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0308 restraints
wR(F2) = 0.067H-atom parameters constrained
S = 1.01Δρmax = 0.95 e Å3
6453 reflectionsΔρmin = 0.91 e Å3
334 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sm10.205433 (16)0.728591 (16)0.277416 (13)0.01394 (6)
O10.0588 (2)0.5655 (2)0.36656 (17)0.0189 (5)
C20.0921 (4)0.4542 (4)0.3228 (4)0.0279 (12)*0.815 (7)
C2A0.1295 (12)0.4229 (6)0.3844 (7)0.010 (4)*0.185 (7)
C30.2417 (3)0.3963 (3)0.2901 (3)0.0275 (8)
O40.2921 (2)0.5070 (2)0.2303 (2)0.0275 (6)
C50.4238 (3)0.4739 (4)0.1590 (3)0.0254 (8)
C60.5228 (3)0.4977 (3)0.1954 (3)0.0246 (8)
O70.4633 (2)0.6364 (2)0.20323 (17)0.0181 (5)
C80.5484 (3)0.6729 (3)0.2401 (3)0.0233 (7)
C90.4956 (3)0.8257 (3)0.2162 (3)0.0248 (8)
O100.3491 (2)0.8688 (2)0.25898 (18)0.0200 (5)
C110.2963 (4)1.0173 (3)0.2268 (3)0.0280 (8)
C120.1440 (3)1.0625 (3)0.2628 (3)0.0246 (8)
O130.0962 (2)0.9900 (2)0.22425 (17)0.0186 (5)
C140.0485 (3)1.0509 (3)0.2243 (3)0.0219 (7)
C150.0818 (3)0.9621 (3)0.1857 (3)0.0219 (7)
O160.0338 (2)0.8226 (2)0.25158 (18)0.0205 (5)
C170.1292 (3)0.7491 (3)0.2942 (3)0.0273 (8)
C180.0848 (3)0.6330 (4)0.3879 (3)0.0270 (12)*0.815 (7)
C18A0.0590 (12)0.5983 (6)0.3272 (14)0.018 (4)*0.185 (7)
O190.2297 (2)0.7930 (2)0.09554 (17)0.0196 (5)
O200.3158 (2)0.5735 (2)0.42200 (17)0.0195 (5)
O210.0801 (2)0.8005 (2)0.43465 (17)0.0189 (5)
Fe20.00000.50000.00000.01376 (13)
N210.0581 (3)0.7292 (3)0.0340 (2)0.0285 (7)
N220.1331 (3)0.5978 (3)0.2337 (2)0.0230 (6)
N230.2919 (3)0.3143 (3)0.0375 (3)0.0321 (7)
C210.0333 (3)0.6454 (3)0.0226 (2)0.0188 (7)
C220.0823 (3)0.5611 (3)0.1474 (3)0.0174 (7)
C230.1822 (3)0.3810 (3)0.0247 (3)0.0209 (7)
Fe30.50000.00000.50000.01334 (13)
N310.4328 (3)0.1013 (3)0.7432 (2)0.0250 (6)
N320.1950 (3)0.0809 (3)0.4967 (2)0.0255 (7)
N330.4472 (3)0.2968 (3)0.4966 (2)0.0261 (7)
C310.4565 (3)0.0631 (3)0.6529 (3)0.0177 (7)
C320.3086 (3)0.0499 (3)0.4966 (3)0.0177 (7)
C330.4666 (3)0.1848 (3)0.5010 (3)0.0183 (7)
O410.2522 (2)0.7061 (2)0.56604 (18)0.0237 (5)
O420.4350 (2)0.8550 (3)0.04449 (19)0.0297 (6)
H2A0.04900.48870.26130.033*0.815 (7)
H2B0.05560.38160.37610.033*0.815 (7)
H2C0.06480.37420.39730.012*0.185 (7)
H2D0.16940.38740.44760.012*0.185 (7)
H3A0.28360.34350.35270.033*0.815 (7)
H3B0.26480.33360.24720.033*0.815 (7)
H3C0.31880.31430.31430.033*0.185 (7)
H3D0.20660.37470.24390.033*0.185 (7)
H5A0.41620.53290.08650.030*
H5B0.45530.37650.15910.030*
H6A0.53840.43190.26480.029*
H6B0.61180.48560.14450.029*
H8A0.64540.64130.20360.028*
H8B0.54250.62990.31680.028*
H9A0.54240.85600.24810.030*
H9B0.51380.86780.13910.030*
H11A0.32101.05190.14920.034*
H11B0.33671.05490.25820.034*
H12A0.11841.03910.34070.030*
H12B0.10381.16320.23390.030*
H14A0.06931.14610.17720.026*
H14B0.10251.05340.29620.026*
H15A0.18190.99210.19120.026*
H15B0.03530.96770.11120.026*
H17A0.13140.71250.24060.033*0.815 (7)
H17B0.22240.81130.31560.033*0.815 (7)
H17C0.18150.77110.24060.033*0.185 (7)
H17D0.19520.77900.35560.033*0.185 (7)
H18A0.11040.66950.44880.032*0.815 (7)
H18B0.13290.56620.40650.032*0.815 (7)
H18C0.12360.55390.38250.021*0.185 (7)
H18D0.03090.56120.26620.021*0.185 (7)
H19A0.17850.77620.06880.044 (4)*
H19B0.29490.80610.04670.044 (4)*
H20A0.30820.60230.47490.044 (4)*
H20B0.36740.48660.43720.044 (4)*
H21A0.11680.78920.48500.044 (4)*
H21B0.00570.84690.45440.044 (4)*
H41A0.22060.67760.62910.044 (4)*
H41B0.31020.73490.56360.044 (4)*
H42A0.42960.86760.10600.044 (4)*
H42B0.50930.79510.04210.044 (4)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sm10.01185 (9)0.01500 (9)0.01319 (9)0.00443 (6)0.00128 (6)0.00318 (6)
O10.0195 (12)0.0219 (12)0.0169 (12)0.0102 (9)0.0028 (9)0.0042 (9)
C30.039 (2)0.0166 (17)0.027 (2)0.0138 (16)0.0002 (17)0.0061 (15)
O40.0218 (13)0.0224 (12)0.0390 (16)0.0116 (10)0.0066 (11)0.0155 (11)
C50.0240 (18)0.0256 (18)0.026 (2)0.0066 (15)0.0030 (15)0.0156 (15)
C60.0166 (17)0.0216 (17)0.030 (2)0.0016 (14)0.0007 (15)0.0099 (15)
O70.0126 (11)0.0182 (11)0.0222 (12)0.0035 (9)0.0014 (9)0.0079 (10)
C80.0125 (16)0.0306 (19)0.029 (2)0.0067 (14)0.0031 (14)0.0127 (16)
C90.0116 (16)0.0295 (19)0.032 (2)0.0086 (14)0.0015 (14)0.0109 (16)
O100.0123 (11)0.0157 (11)0.0305 (14)0.0039 (9)0.0032 (10)0.0066 (10)
C110.0242 (19)0.0158 (16)0.043 (2)0.0084 (14)0.0071 (17)0.0054 (16)
C120.0260 (19)0.0148 (16)0.034 (2)0.0053 (14)0.0100 (16)0.0064 (15)
O130.0157 (11)0.0165 (11)0.0222 (13)0.0037 (9)0.0056 (10)0.0045 (9)
C140.0149 (16)0.0196 (16)0.0232 (19)0.0004 (13)0.0050 (14)0.0025 (14)
C150.0186 (17)0.0208 (17)0.0194 (18)0.0010 (14)0.0073 (14)0.0014 (14)
O160.0136 (11)0.0183 (11)0.0279 (13)0.0050 (9)0.0070 (10)0.0026 (10)
C170.0170 (17)0.037 (2)0.025 (2)0.0140 (15)0.0020 (15)0.0019 (16)
O190.0154 (11)0.0297 (13)0.0144 (12)0.0105 (10)0.0003 (9)0.0058 (10)
O200.0219 (12)0.0166 (11)0.0165 (12)0.0009 (9)0.0076 (10)0.0038 (9)
O210.0106 (11)0.0264 (12)0.0155 (12)0.0006 (9)0.0027 (9)0.0087 (10)
Fe20.0117 (3)0.0164 (3)0.0127 (3)0.0058 (2)0.0023 (2)0.0024 (2)
N210.0381 (18)0.0305 (17)0.0238 (17)0.0184 (14)0.0072 (14)0.0063 (13)
N220.0219 (15)0.0260 (15)0.0203 (16)0.0094 (12)0.0024 (13)0.0056 (13)
N230.0206 (17)0.0287 (16)0.0364 (19)0.0058 (13)0.0087 (14)0.0019 (14)
C210.0186 (17)0.0221 (17)0.0129 (16)0.0070 (14)0.0023 (13)0.0024 (13)
C220.0149 (16)0.0186 (16)0.0180 (18)0.0058 (13)0.0038 (14)0.0038 (13)
C230.0210 (18)0.0202 (16)0.0182 (17)0.0099 (14)0.0018 (14)0.0004 (14)
Fe30.0096 (3)0.0130 (3)0.0141 (3)0.0025 (2)0.0010 (2)0.0029 (2)
N310.0193 (15)0.0305 (16)0.0184 (16)0.0052 (13)0.0026 (12)0.0040 (13)
N320.0169 (15)0.0305 (16)0.0245 (17)0.0054 (12)0.0019 (12)0.0075 (13)
N330.0284 (17)0.0187 (15)0.0309 (18)0.0059 (13)0.0095 (14)0.0057 (13)
C310.0100 (15)0.0161 (15)0.0225 (19)0.0015 (12)0.0026 (13)0.0044 (14)
C320.0153 (17)0.0183 (16)0.0161 (17)0.0051 (13)0.0002 (13)0.0046 (13)
C330.0104 (15)0.0235 (18)0.0167 (17)0.0048 (13)0.0022 (13)0.0025 (14)
O410.0240 (13)0.0361 (14)0.0150 (12)0.0184 (11)0.0015 (10)0.0040 (10)
O420.0149 (12)0.0450 (15)0.0194 (13)0.0065 (11)0.0021 (10)0.0038 (11)
Geometric parameters (Å, º) top
Sm1—O192.327 (2)C14—C151.491 (5)
Sm1—O212.408 (2)C14—H14A0.99
Sm1—O202.409 (2)C14—H14B0.99
Sm1—O162.481 (2)C15—O161.450 (4)
Sm1—O42.505 (2)C15—H15A0.99
Sm1—O102.529 (2)C15—H15B0.99
Sm1—O132.552 (2)O16—C171.425 (4)
Sm1—O72.563 (2)C17—C18A1.484 (5)
Sm1—O12.602 (2)C17—C181.501 (4)
O1—C2A1.410 (5)C17—H17A0.99
O1—C181.416 (3)C17—H17B0.99
O1—C18A1.424 (5)C17—H17C0.99
O1—C21.445 (3)C17—H17D0.99
C2—C31.471 (4)C18—H18A0.99
C2—H2A0.99C18—H18B0.99
C2—H2B0.99C18A—H18C0.99
C2A—C31.505 (5)C18A—H18D0.99
C2A—H2C0.99O19—H19A0.87
C2A—H2D0.99O19—H19B0.83
C3—O41.411 (4)O20—H20A0.88
C3—H3A0.99O20—H20B0.88
C3—H3B0.99O21—H21A0.87
C3—H3C0.99O21—H21B0.87
C3—H3D0.99Fe2—C221.939 (3)
O4—C51.449 (4)Fe2—C22i1.939 (3)
C5—C61.484 (5)Fe2—C23i1.945 (3)
C5—H5A0.99Fe2—C231.945 (3)
C5—H5B0.99Fe2—C211.945 (3)
C6—O71.436 (4)Fe2—C21i1.945 (3)
C6—H6A0.99N21—C211.146 (4)
C6—H6B0.99N22—C221.143 (4)
O7—C81.442 (4)N23—C231.153 (4)
C8—C91.489 (5)Fe3—C331.934 (3)
C8—H8A0.99Fe3—C33ii1.934 (3)
C8—H8B0.99Fe3—C321.944 (3)
C9—O101.451 (4)Fe3—C32ii1.944 (3)
C9—H9A0.99Fe3—C311.944 (3)
C9—H9B0.99Fe3—C31ii1.944 (3)
O10—C111.443 (4)N31—C311.147 (4)
C11—C121.492 (5)N32—C321.144 (4)
C11—H11A0.99N33—C331.153 (4)
C11—H11B0.99O41—H41A0.82
C12—O131.440 (4)O41—H41B0.80
C12—H12A0.99O42—H42A0.84
C12—H12B0.99O42—H42B0.81
O13—C141.442 (4)
O19—Sm1—O21144.30 (7)O10—C11—H11A109.9
O19—Sm1—O20144.23 (7)C12—C11—H11A109.9
O21—Sm1—O2070.41 (7)O10—C11—H11B109.9
O19—Sm1—O1676.07 (8)C12—C11—H11B109.9
O21—Sm1—O1678.51 (7)H11A—C11—H11B108.3
O20—Sm1—O16134.35 (7)O13—C12—C11106.0 (3)
O19—Sm1—O474.97 (8)O13—C12—H12A110.5
O21—Sm1—O4135.03 (8)C11—C12—H12A110.5
O20—Sm1—O479.77 (8)O13—C12—H12B110.5
O16—Sm1—O4101.33 (8)C11—C12—H12B110.5
O19—Sm1—O1090.85 (8)H12A—C12—H12B108.7
O21—Sm1—O1084.05 (7)C12—O13—C14112.8 (2)
O20—Sm1—O1083.84 (7)C12—O13—Sm1115.11 (17)
O16—Sm1—O10125.77 (7)C14—O13—Sm1119.85 (18)
O4—Sm1—O10125.99 (7)O13—C14—C15106.0 (2)
O19—Sm1—O1374.59 (7)O13—C14—H14A110.5
O21—Sm1—O1371.66 (7)C15—C14—H14A110.5
O20—Sm1—O13131.34 (7)O13—C14—H14B110.5
O16—Sm1—O1362.89 (7)C15—C14—H14B110.5
O4—Sm1—O13148.36 (8)H14A—C14—H14B108.7
O10—Sm1—O1362.89 (7)O16—C15—C14106.8 (3)
O19—Sm1—O774.23 (7)O16—C15—H15A110.4
O21—Sm1—O7131.71 (7)C14—C15—H15A110.4
O20—Sm1—O771.91 (7)O16—C15—H15B110.4
O16—Sm1—O7149.21 (7)C14—C15—H15B110.4
O4—Sm1—O763.15 (7)H15A—C15—H15B108.6
O10—Sm1—O762.83 (7)C17—O16—C15116.1 (2)
O13—Sm1—O7115.60 (7)C17—O16—Sm1125.34 (17)
O19—Sm1—O1109.70 (7)C15—O16—Sm1118.51 (18)
O21—Sm1—O179.51 (7)O16—C17—C18A111.5 (5)
O20—Sm1—O179.10 (7)O16—C17—C18108.2 (3)
O16—Sm1—O162.70 (7)O16—C17—H17A110.1
O4—Sm1—O162.01 (7)C18—C17—H17A110.1
O10—Sm1—O1159.45 (7)O16—C17—H17B110.1
O13—Sm1—O1122.01 (7)C18—C17—H17B110.1
O7—Sm1—O1121.17 (6)H17A—C17—H17B108.4
C2A—O1—C18A108.6 (7)O16—C17—H17C109.3
C18—O1—C2110.9 (3)C18A—C17—H17C109.3
C2A—O1—Sm1117.2 (5)O16—C17—H17D109.3
C18—O1—Sm1114.9 (2)C18A—C17—H17D109.3
C18A—O1—Sm1118.1 (5)H17C—C17—H17D108.0
C2—O1—Sm1117.6 (2)O1—C18—C17111.0 (3)
O1—C2—C3109.7 (3)O1—C18—H18A109.4
O1—C2—H2A109.7C17—C18—H18A109.4
C3—C2—H2A109.7O1—C18—H18B109.4
O1—C2—H2B109.7C17—C18—H18B109.4
C3—C2—H2B109.7H18A—C18—H18B108.0
H2A—C2—H2B108.2O1—C18A—C17111.6 (5)
O1—C2A—C3109.7 (4)O1—C18A—H18C109.3
O1—C2A—H2C109.7C17—C18A—H18C109.3
C3—C2A—H2C109.7O1—C18A—H18D109.3
O1—C2A—H2D109.7C17—C18A—H18D109.3
C3—C2A—H2D109.7H18C—C18A—H18D108.0
H2C—C2A—H2D108.2Sm1—O19—H19A119.5
O4—C3—C2107.7 (3)Sm1—O19—H19B131.6
O4—C3—C2A114.3 (4)H19A—O19—H19B105.3
O4—C3—H3A110.2Sm1—O20—H20A120.4
C2—C3—H3A110.2Sm1—O20—H20B134.6
O4—C3—H3B110.2H20A—O20—H20B105.0
C2—C3—H3B110.2Sm1—O21—H21A124.6
H3A—C3—H3B108.5Sm1—O21—H21B132.2
O4—C3—H3C108.7H21A—O21—H21B103.0
C2A—C3—H3C108.7C22—Fe2—C22i180.0 (2)
O4—C3—H3D108.7C22—Fe2—C23i91.64 (13)
C2A—C3—H3D108.7C22i—Fe2—C23i88.36 (13)
H3C—C3—H3D107.6C22—Fe2—C2388.36 (13)
C3—O4—C5116.0 (2)C22i—Fe2—C2391.64 (13)
C3—O4—Sm1123.26 (19)C23i—Fe2—C23180.0 (2)
C5—O4—Sm1118.28 (18)C22—Fe2—C2187.90 (13)
O4—C5—C6107.9 (3)C22i—Fe2—C2192.10 (13)
O4—C5—H5A110.1C23i—Fe2—C2191.97 (13)
C6—C5—H5A110.1C23—Fe2—C2188.03 (13)
O4—C5—H5B110.1C22—Fe2—C21i92.10 (13)
C6—C5—H5B110.1C22i—Fe2—C21i87.90 (13)
H5A—C5—H5B108.4C23i—Fe2—C21i88.03 (13)
O7—C6—C5106.6 (3)C23—Fe2—C21i91.97 (13)
O7—C6—H6A110.4C21—Fe2—C21i180.00 (17)
C5—C6—H6A110.4N21—C21—Fe2177.3 (3)
O7—C6—H6B110.4N22—C22—Fe2178.3 (3)
C5—C6—H6B110.4N23—C23—Fe2177.6 (3)
H6A—C6—H6B108.6C33—Fe3—C33ii180.0 (2)
C6—O7—C8112.5 (2)C33—Fe3—C3289.79 (13)
C6—O7—Sm1118.97 (18)C33ii—Fe3—C3290.21 (13)
C8—O7—Sm1114.86 (17)C33—Fe3—C32ii90.21 (13)
O7—C8—C9106.4 (3)C33ii—Fe3—C32ii89.79 (13)
O7—C8—H8A110.5C32—Fe3—C32ii180.0 (2)
C9—C8—H8A110.5C33—Fe3—C3192.14 (13)
O7—C8—H8B110.5C33ii—Fe3—C3187.86 (13)
C9—C8—H8B110.5C32—Fe3—C3190.21 (13)
H8A—C8—H8B108.6C32ii—Fe3—C3189.79 (13)
O10—C9—C8108.7 (3)C33—Fe3—C31ii87.86 (13)
O10—C9—H9A110.0C33ii—Fe3—C31ii92.14 (13)
C8—C9—H9A110.0C32—Fe3—C31ii89.79 (13)
O10—C9—H9B110.0C32ii—Fe3—C31ii90.21 (13)
C8—C9—H9B110.0C31—Fe3—C31ii180.000 (1)
H9A—C9—H9B108.3N31—C31—Fe3179.1 (3)
C11—O10—C9108.4 (2)N32—C32—Fe3178.2 (3)
C11—O10—Sm1120.66 (18)N33—C33—Fe3176.8 (3)
C9—O10—Sm1120.97 (18)H41A—O41—H41B105.7
O10—C11—C12108.8 (3)H42A—O42—H42B100.3
O19—Sm1—O1—C2A91.0 (6)O10—Sm1—O7—C829.4 (2)
O21—Sm1—O1—C2A124.8 (6)O13—Sm1—O7—C864.9 (2)
O20—Sm1—O1—C2A53.0 (6)O1—Sm1—O7—C8127.5 (2)
O16—Sm1—O1—C2A152.8 (6)C6—O7—C8—C9164.6 (3)
O4—Sm1—O1—C2A31.1 (6)Sm1—O7—C8—C955.0 (3)
O10—Sm1—O1—C2A87.4 (6)O7—C8—C9—O1052.3 (4)
O13—Sm1—O1—C2A174.7 (6)C8—C9—O10—C11174.5 (3)
O7—Sm1—O1—C2A7.9 (6)C8—C9—O10—Sm128.8 (4)
O19—Sm1—O1—C1886.9 (2)O19—Sm1—O10—C1170.7 (2)
O21—Sm1—O1—C1857.3 (2)O21—Sm1—O10—C1173.9 (2)
O20—Sm1—O1—C18129.2 (2)O20—Sm1—O10—C11144.7 (2)
O16—Sm1—O1—C1825.1 (2)O16—Sm1—O10—C112.7 (3)
O4—Sm1—O1—C18146.7 (3)O4—Sm1—O10—C11142.7 (2)
O10—Sm1—O1—C1894.7 (3)O13—Sm1—O10—C111.5 (2)
O13—Sm1—O1—C183.1 (3)O7—Sm1—O10—C11142.5 (3)
O7—Sm1—O1—C18169.9 (2)O1—Sm1—O10—C11110.8 (3)
O19—Sm1—O1—C18A41.9 (8)O19—Sm1—O10—C970.8 (2)
O21—Sm1—O1—C18A102.3 (7)O21—Sm1—O10—C9144.6 (2)
O20—Sm1—O1—C18A174.1 (7)O20—Sm1—O10—C973.7 (2)
O16—Sm1—O1—C18A19.9 (7)O16—Sm1—O10—C9144.2 (2)
O4—Sm1—O1—C18A101.7 (8)O4—Sm1—O10—C91.2 (3)
O10—Sm1—O1—C18A139.7 (8)O13—Sm1—O10—C9143.0 (2)
O13—Sm1—O1—C18A41.9 (8)O7—Sm1—O10—C90.9 (2)
O7—Sm1—O1—C18A124.9 (7)O1—Sm1—O10—C9107.7 (3)
O19—Sm1—O1—C246.4 (2)C9—O10—C11—C12175.4 (3)
O21—Sm1—O1—C2169.4 (2)Sm1—O10—C11—C1229.6 (4)
O20—Sm1—O1—C297.5 (2)O10—C11—C12—O1352.7 (4)
O16—Sm1—O1—C2108.2 (2)C11—C12—O13—C14162.5 (3)
O4—Sm1—O1—C213.4 (2)C11—C12—O13—Sm155.0 (3)
O10—Sm1—O1—C2132.0 (3)O19—Sm1—O13—C12128.5 (2)
O13—Sm1—O1—C2130.2 (2)O21—Sm1—O13—C1263.3 (2)
O7—Sm1—O1—C236.6 (3)O20—Sm1—O13—C1223.0 (2)
C2A—O1—C2—C361.7 (6)O16—Sm1—O13—C12149.6 (2)
C18—O1—C2—C3173.5 (3)O4—Sm1—O13—C12144.7 (2)
C18A—O1—C2—C3153.1 (8)O10—Sm1—O13—C1229.4 (2)
Sm1—O1—C2—C338.5 (4)O7—Sm1—O13—C1264.9 (2)
C18—O1—C2A—C3135.7 (7)O1—Sm1—O13—C12127.6 (2)
C18A—O1—C2A—C395.1 (13)O19—Sm1—O13—C1491.8 (2)
C2—O1—C2A—C359.3 (6)O21—Sm1—O13—C1476.4 (2)
Sm1—O1—C2A—C341.9 (12)O20—Sm1—O13—C14116.7 (2)
O1—C2—C3—O448.3 (4)O16—Sm1—O13—C149.9 (2)
O1—C2—C3—C2A58.8 (6)O4—Sm1—O13—C1475.6 (3)
O1—C2A—C3—O426.5 (13)O10—Sm1—O13—C14169.0 (2)
O1—C2A—C3—C261.2 (7)O7—Sm1—O13—C14155.4 (2)
C2—C3—O4—C5157.6 (3)O1—Sm1—O13—C1412.0 (2)
C2A—C3—O4—C5162.5 (7)C12—O13—C14—C15178.3 (3)
C2—C3—O4—Sm140.7 (4)Sm1—O13—C14—C1537.8 (3)
C2A—C3—O4—Sm10.8 (7)O13—C14—C15—O1653.8 (3)
O19—Sm1—O4—C3138.3 (3)C14—C15—O16—C17130.8 (3)
O21—Sm1—O4—C318.7 (3)C14—C15—O16—Sm150.8 (3)
O20—Sm1—O4—C367.2 (3)O19—Sm1—O16—C17121.3 (3)
O16—Sm1—O4—C366.3 (3)O21—Sm1—O16—C1783.9 (2)
O10—Sm1—O4—C3141.8 (2)O20—Sm1—O16—C1736.6 (3)
O13—Sm1—O4—C3122.2 (3)O4—Sm1—O16—C1750.1 (3)
O7—Sm1—O4—C3142.0 (3)O10—Sm1—O16—C17157.9 (2)
O1—Sm1—O4—C315.8 (2)O13—Sm1—O16—C17159.1 (3)
O19—Sm1—O4—C560.3 (2)O7—Sm1—O16—C17105.8 (3)
O21—Sm1—O4—C5142.6 (2)O1—Sm1—O16—C170.1 (2)
O20—Sm1—O4—C594.1 (2)O19—Sm1—O16—C1556.8 (2)
O16—Sm1—O4—C5132.4 (2)O21—Sm1—O16—C1597.9 (2)
O10—Sm1—O4—C519.5 (3)O20—Sm1—O16—C15145.26 (19)
O13—Sm1—O4—C576.5 (3)O4—Sm1—O16—C15128.0 (2)
O7—Sm1—O4—C519.3 (2)O10—Sm1—O16—C1524.0 (2)
O1—Sm1—O4—C5177.1 (3)O13—Sm1—O16—C1522.8 (2)
C3—O4—C5—C6115.2 (3)O7—Sm1—O16—C1572.3 (2)
Sm1—O4—C5—C647.4 (3)O1—Sm1—O16—C15178.1 (2)
O4—C5—C6—O754.1 (4)C15—O16—C17—C18A160.0 (7)
C5—C6—O7—C8178.9 (3)Sm1—O16—C17—C18A18.2 (8)
C5—C6—O7—Sm140.3 (3)C15—O16—C17—C18159.5 (3)
O19—Sm1—O7—C693.6 (2)Sm1—O16—C17—C1822.3 (4)
O21—Sm1—O7—C6114.9 (2)C2A—O1—C18—C17131.0 (7)
O20—Sm1—O7—C674.7 (2)C18A—O1—C18—C1758.2 (7)
O16—Sm1—O7—C677.9 (3)C2—O1—C18—C1789.8 (4)
O4—Sm1—O7—C612.7 (2)Sm1—O1—C18—C1746.6 (4)
O10—Sm1—O7—C6167.1 (2)O16—C17—C18—O143.5 (4)
O13—Sm1—O7—C6157.4 (2)C18A—C17—C18—O158.4 (7)
O1—Sm1—O7—C610.2 (2)C2A—O1—C18A—C17173.0 (9)
O19—Sm1—O7—C8128.7 (2)C18—O1—C18A—C1759.7 (7)
O21—Sm1—O7—C822.7 (2)C2—O1—C18A—C17150.6 (13)
O20—Sm1—O7—C862.9 (2)Sm1—O1—C18A—C1736.5 (15)
O16—Sm1—O7—C8144.4 (2)O16—C17—C18A—O134.1 (14)
O4—Sm1—O7—C8150.4 (2)C18—C17—C18A—O158.3 (7)
Symmetry codes: (i) x, y+1, z; (ii) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O19—H19A···N210.871.852.717 (4)171
O19—H19B···O420.831.772.590 (3)169
O20—H20A···O410.881.832.682 (3)163
O20—H20B···N330.881.882.745 (3)167
O21—H21A···O410.871.882.691 (3)155
O21—H21B···N32iii0.871.872.737 (3)171
O41—H41A···N22iv0.821.902.712 (4)170
O41—H41B···N33v0.802.423.099 (4)143
O42—H42A···N31vi0.842.002.836 (4)175
O42—H42B···N23vii0.812.022.810 (4)165
Symmetry codes: (iii) x, y+1, z+1; (iv) x, y, z+1; (v) x+1, y+1, z+1; (vi) x, y+1, z1; (vii) x+1, y+1, z.
(IV) Triaqua(18-crown-6)europium(III) hexacyanoferrate(III) dihydrate top
Crystal data top
[Eu(C12H24O6)(H2O)3][Fe(CN)6]·2H2OZ = 2
Mr = 718.32F(000) = 722
Triclinic, P1Dx = 1.703 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.9125 (3) ÅCell parameters from 6139 reflections
b = 11.0947 (4) Åθ = 2.9–27.5°
c = 14.0119 (3) ŵ = 2.80 mm1
α = 67.8201 (18)°T = 120 K
β = 70.635 (2)°Block, yellow
γ = 65.743 (2)°0.25 × 0.20 × 0.20 mm
V = 1400.57 (8) Å3
Data collection top
Bruker–Nonius KappaCCD
diffractometer
6420 independent reflections
Radiation source: Bruker–Nonius FR591 rotating anode5973 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.060
Detector resolution: 9.091 pixels mm-1θmax = 27.6°, θmin = 3.2°
ϕ & ω scansh = 1414
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
k = 1414
Tmin = 0.509, Tmax = 0.568l = 1818
27604 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.077Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.212H-atom parameters constrained
S = 1.10 w = 1/[σ2(Fo2) + (0.1382P)2 + 13.515P]
where P = (Fo2 + 2Fc2)/3
6420 reflections(Δ/σ)max = 0.001
334 parametersΔρmax = 11.43 e Å3
8 restraintsΔρmin = 3.03 e Å3
Crystal data top
[Eu(C12H24O6)(H2O)3][Fe(CN)6]·2H2Oγ = 65.743 (2)°
Mr = 718.32V = 1400.57 (8) Å3
Triclinic, P1Z = 2
a = 10.9125 (3) ÅMo Kα radiation
b = 11.0947 (4) ŵ = 2.80 mm1
c = 14.0119 (3) ÅT = 120 K
α = 67.8201 (18)°0.25 × 0.20 × 0.20 mm
β = 70.635 (2)°
Data collection top
Bruker–Nonius KappaCCD
diffractometer
6420 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
5973 reflections with I > 2σ(I)
Tmin = 0.509, Tmax = 0.568Rint = 0.060
27604 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0778 restraints
wR(F2) = 0.212H-atom parameters constrained
S = 1.10 w = 1/[σ2(Fo2) + (0.1382P)2 + 13.515P]
where P = (Fo2 + 2Fc2)/3
6420 reflectionsΔρmax = 11.43 e Å3
334 parametersΔρmin = 3.03 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Eu10.20539 (3)0.72823 (3)0.27729 (3)0.01553 (16)
O10.0592 (5)0.5655 (5)0.3664 (4)0.0218 (11)
C20.0893 (8)0.4559 (9)0.3237 (9)0.0259 (16)*0.762 (14)
C2A0.127 (2)0.4216 (8)0.3832 (15)0.0259 (16)*0.238 (14)
C30.2416 (8)0.3962 (9)0.2902 (7)0.0300 (18)
O40.2905 (6)0.5068 (6)0.2306 (6)0.0311 (14)
C50.4213 (9)0.4752 (9)0.1589 (7)0.0282 (18)
C60.5221 (8)0.4978 (8)0.1952 (7)0.0275 (17)
O70.4628 (5)0.6361 (6)0.2037 (5)0.0211 (11)
C80.5477 (8)0.6701 (9)0.2423 (8)0.0290 (18)
C90.4951 (8)0.8258 (9)0.2178 (8)0.0288 (18)
O100.3486 (6)0.8667 (6)0.2602 (5)0.0228 (11)
C110.2960 (10)1.0171 (9)0.2273 (8)0.0310 (19)
C120.1435 (10)1.0622 (9)0.2626 (8)0.0296 (18)
O130.0968 (6)0.9897 (5)0.2235 (5)0.0226 (11)
C140.0479 (8)1.0508 (8)0.2224 (7)0.0253 (16)
C150.0800 (8)0.9618 (8)0.1843 (8)0.0282 (17)
O160.0321 (6)0.8222 (6)0.2500 (5)0.0241 (12)
C170.1290 (9)0.7506 (9)0.2938 (7)0.0313 (19)
C180.0847 (7)0.6349 (9)0.3882 (7)0.0259 (16)*0.762 (14)
C18A0.059 (2)0.5983 (11)0.327 (3)0.0259 (16)*0.238 (14)
O190.2303 (6)0.7931 (6)0.0959 (4)0.0227 (11)
O200.3152 (6)0.5729 (6)0.4218 (4)0.0219 (11)
O210.0804 (5)0.8001 (6)0.4333 (4)0.0205 (11)
Fe20.00000.50000.00000.0155 (3)
N210.0612 (9)0.7267 (8)0.0339 (6)0.0339 (17)
N220.1326 (8)0.5989 (8)0.2346 (6)0.0277 (15)
N230.2921 (9)0.3135 (9)0.0374 (8)0.044 (2)
C210.0342 (8)0.6443 (8)0.0230 (6)0.0225 (15)
C220.0817 (8)0.5612 (8)0.1470 (6)0.0196 (14)
C230.1811 (8)0.3802 (9)0.0255 (7)0.0253 (16)
Fe30.50000.00000.50000.0152 (3)
N310.4322 (8)0.1000 (8)0.7428 (6)0.0284 (15)
N320.1927 (7)0.0800 (8)0.4979 (6)0.0290 (16)
N330.4469 (8)0.2961 (7)0.4965 (6)0.0295 (16)
C310.4560 (7)0.0630 (8)0.6526 (6)0.0206 (15)
C320.3083 (8)0.0495 (8)0.4980 (6)0.0205 (14)
C330.4673 (8)0.1848 (8)0.5000 (6)0.0209 (15)
O410.2521 (6)0.7052 (6)0.5656 (4)0.0255 (12)
O420.4345 (6)0.8559 (7)0.0449 (5)0.0327 (14)
H2A0.04580.49100.26240.031*0.762 (14)
H2B0.05210.38380.37740.031*0.762 (14)
H2C0.06060.37620.39220.031*0.238 (14)
H2D0.16380.38240.44810.031*0.238 (14)
H3A0.28390.34350.35270.036*0.762 (14)
H3B0.26430.33350.24740.036*0.762 (14)
H3C0.31900.31560.31580.036*0.238 (14)
H3D0.20960.37220.24360.036*0.238 (14)
H5A0.41300.53550.08670.034*
H5B0.45270.37820.15790.034*
H6A0.53800.43130.26430.033*
H6B0.61090.48610.14380.033*
H8A0.64520.63760.20670.035*
H8B0.53990.62700.31920.035*
H9A0.54110.85590.25050.035*
H9B0.51400.86830.14060.035*
H11A0.32171.05170.14970.037*
H11B0.33601.05450.25920.037*
H12A0.11691.03880.34050.035*
H12B0.10331.16300.23350.035*
H14A0.06811.14570.17470.030*
H14B0.10301.05400.29410.030*
H15A0.18030.99150.18950.034*
H15B0.03310.96760.10970.034*
H17A0.13240.71340.24100.038*0.762 (14)
H17B0.22170.81380.31510.038*0.762 (14)
H17C0.18220.77270.24080.038*0.238 (14)
H17D0.19400.78120.35530.038*0.238 (14)
H18A0.10880.67220.44840.031*0.762 (14)
H18B0.13420.56870.40820.031*0.762 (14)
H18C0.12380.55430.38310.031*0.238 (14)
H18D0.03100.56090.26670.031*0.238 (14)
H19A0.17910.77630.06920.045 (11)*
H19B0.29540.80620.04700.045 (11)*
H20A0.30770.60160.47470.045 (11)*
H20B0.36680.48600.43700.045 (11)*
H21A0.11710.78890.48360.045 (11)*
H21B0.00540.84650.45300.045 (11)*
H41A0.22050.67660.62860.045 (11)*
H41B0.31010.73390.56320.045 (11)*
H42A0.42910.86850.10650.045 (11)*
H42B0.50880.79600.04250.045 (11)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Eu10.0163 (2)0.0170 (2)0.0140 (2)0.00982 (16)0.00108 (14)0.00214 (14)
O10.025 (3)0.025 (3)0.020 (3)0.018 (2)0.000 (2)0.003 (2)
C30.042 (5)0.023 (4)0.028 (4)0.019 (4)0.001 (4)0.006 (3)
O40.026 (3)0.026 (3)0.046 (4)0.015 (2)0.006 (3)0.019 (3)
C50.028 (4)0.028 (4)0.033 (4)0.015 (3)0.006 (3)0.017 (4)
C60.019 (4)0.022 (4)0.037 (5)0.003 (3)0.001 (3)0.012 (3)
O70.017 (2)0.022 (3)0.026 (3)0.009 (2)0.002 (2)0.008 (2)
C80.016 (3)0.033 (4)0.042 (5)0.008 (3)0.005 (3)0.016 (4)
C90.019 (4)0.033 (4)0.041 (5)0.018 (3)0.000 (3)0.014 (4)
O100.019 (3)0.019 (3)0.034 (3)0.014 (2)0.002 (2)0.007 (2)
C110.034 (5)0.022 (4)0.042 (5)0.018 (4)0.008 (4)0.004 (4)
C120.032 (4)0.021 (4)0.038 (5)0.008 (3)0.009 (4)0.010 (3)
O130.022 (3)0.017 (2)0.029 (3)0.007 (2)0.007 (2)0.005 (2)
C140.020 (4)0.015 (3)0.033 (4)0.002 (3)0.008 (3)0.001 (3)
C150.020 (4)0.022 (4)0.036 (5)0.002 (3)0.011 (3)0.002 (3)
O160.018 (3)0.019 (3)0.035 (3)0.010 (2)0.009 (2)0.001 (2)
C170.021 (4)0.044 (5)0.028 (4)0.018 (4)0.003 (3)0.002 (4)
O190.021 (3)0.034 (3)0.015 (2)0.015 (2)0.000 (2)0.006 (2)
O200.029 (3)0.020 (2)0.014 (2)0.009 (2)0.007 (2)0.001 (2)
O210.017 (2)0.026 (3)0.018 (3)0.007 (2)0.003 (2)0.007 (2)
Fe20.0163 (7)0.0181 (7)0.0139 (7)0.0113 (6)0.0022 (5)0.0008 (5)
N210.049 (5)0.033 (4)0.028 (4)0.022 (4)0.010 (3)0.006 (3)
N220.030 (4)0.033 (4)0.020 (3)0.016 (3)0.001 (3)0.005 (3)
N230.027 (4)0.036 (4)0.053 (6)0.004 (3)0.014 (4)0.001 (4)
C210.027 (4)0.027 (4)0.015 (3)0.015 (3)0.002 (3)0.002 (3)
C220.021 (3)0.022 (3)0.020 (4)0.013 (3)0.004 (3)0.003 (3)
C230.020 (4)0.027 (4)0.029 (4)0.010 (3)0.003 (3)0.006 (3)
Fe30.0134 (6)0.0155 (6)0.0154 (7)0.0077 (5)0.0008 (5)0.0016 (5)
N310.027 (3)0.035 (4)0.017 (3)0.009 (3)0.004 (3)0.003 (3)
N320.019 (3)0.036 (4)0.029 (4)0.008 (3)0.005 (3)0.008 (3)
N330.034 (4)0.022 (3)0.029 (4)0.009 (3)0.006 (3)0.005 (3)
C310.014 (3)0.019 (3)0.026 (4)0.008 (3)0.002 (3)0.003 (3)
C320.021 (4)0.023 (3)0.017 (3)0.014 (3)0.001 (3)0.002 (3)
C330.018 (3)0.023 (4)0.018 (3)0.007 (3)0.002 (3)0.003 (3)
O410.028 (3)0.037 (3)0.017 (3)0.022 (3)0.000 (2)0.004 (2)
O420.023 (3)0.050 (4)0.018 (3)0.014 (3)0.003 (2)0.001 (3)
Geometric parameters (Å, º) top
Eu1—O192.318 (5)C14—C151.479 (12)
Eu1—O212.392 (5)C14—H14A0.99
Eu1—O202.405 (5)C14—H14B0.99
Eu1—O162.467 (5)C15—O161.448 (10)
Eu1—O42.502 (6)C15—H15A0.99
Eu1—O102.511 (5)C15—H15B0.99
Eu1—O132.550 (5)O16—C171.421 (10)
Eu1—O72.553 (5)C17—C18A1.496 (5)
Eu1—O12.590 (5)C17—C181.505 (5)
O1—C2A1.418 (5)C17—H17A0.99
O1—C18A1.420 (5)C17—H17B0.99
O1—C181.420 (5)C17—H17C0.99
O1—C21.427 (5)C17—H17D0.99
C2—C31.495 (5)C18—H18A0.99
C2—H2A0.99C18—H18B0.99
C2—H2B0.99C18A—H18C0.99
C2A—C31.501 (5)C18A—H18D0.99
C2A—H2C0.99O19—H19A0.87
C2A—H2D0.99O19—H19B0.82
C3—O41.399 (10)O20—H20A0.88
C3—H3A0.99O20—H20B0.88
C3—H3B0.99O21—H21A0.87
C3—H3C0.99O21—H21B0.87
C3—H3D0.99Fe2—C221.929 (8)
O4—C51.440 (10)Fe2—C22i1.929 (8)
C5—C61.491 (12)Fe2—C231.936 (8)
C5—H5A0.99Fe2—C23i1.936 (8)
C5—H5B0.99Fe2—C211.941 (8)
C6—O71.435 (9)Fe2—C21i1.941 (8)
C6—H6A0.99N21—C211.141 (11)
C6—H6B0.99N22—C221.159 (11)
O7—C81.437 (10)N23—C231.161 (12)
C8—C91.516 (12)Fe3—C331.932 (8)
C8—H8A0.99Fe3—C33ii1.932 (8)
C8—H8B0.99Fe3—C31ii1.939 (8)
C9—O101.446 (10)Fe3—C311.939 (8)
C9—H9A0.99Fe3—C32ii1.940 (8)
C9—H9B0.99Fe3—C321.940 (8)
O10—C111.461 (10)N31—C311.144 (11)
C11—C121.490 (13)N32—C321.164 (11)
C11—H11A0.99N33—C331.145 (11)
C11—H11B0.99O41—H41A0.82
C12—O131.437 (10)O41—H41B0.80
C12—H12A0.99O42—H42A0.84
C12—H12B0.99O42—H42B0.81
O13—C141.443 (9)
O19—Eu1—O21144.10 (19)O10—C11—H11A110.0
O19—Eu1—O20144.23 (19)C12—C11—H11A110.0
O21—Eu1—O2070.55 (18)O10—C11—H11B110.0
O19—Eu1—O1675.7 (2)C12—C11—H11B110.0
O21—Eu1—O1678.9 (2)H11A—C11—H11B108.4
O20—Eu1—O16134.7 (2)O13—C12—C11105.8 (7)
O19—Eu1—O475.2 (2)O13—C12—H12A110.6
O21—Eu1—O4135.0 (2)C11—C12—H12A110.6
O20—Eu1—O479.8 (2)O13—C12—H12B110.6
O16—Eu1—O4100.8 (2)C11—C12—H12B110.6
O19—Eu1—O1091.0 (2)H12A—C12—H12B108.7
O21—Eu1—O1083.71 (19)C12—O13—C14112.8 (6)
O20—Eu1—O1083.59 (19)C12—O13—Eu1115.2 (5)
O16—Eu1—O10125.90 (18)C14—O13—Eu1119.8 (4)
O4—Eu1—O10126.37 (19)O13—C14—C15105.9 (6)
O19—Eu1—O1374.3 (2)O13—C14—H14A110.6
O21—Eu1—O1371.67 (19)C15—C14—H14A110.6
O20—Eu1—O13131.53 (19)O13—C14—H14B110.6
O16—Eu1—O1362.85 (18)C15—C14—H14B110.6
O4—Eu1—O13148.2 (2)H14A—C14—H14B108.7
O10—Eu1—O1363.05 (18)O16—C15—C14107.2 (7)
O19—Eu1—O774.26 (19)O16—C15—H15A110.3
O21—Eu1—O7131.67 (18)C14—C15—H15A110.3
O20—Eu1—O771.84 (19)O16—C15—H15B110.3
O16—Eu1—O7148.8 (2)C14—C15—H15B110.3
O4—Eu1—O763.50 (19)H15A—C15—H15B108.5
O10—Eu1—O762.88 (18)C17—O16—C15115.8 (6)
O13—Eu1—O7115.53 (18)C17—O16—Eu1125.5 (4)
O19—Eu1—O1109.97 (19)C15—O16—Eu1118.8 (5)
O21—Eu1—O179.60 (18)O16—C17—C18A111.0 (11)
O20—Eu1—O178.89 (18)O16—C17—C18108.0 (7)
O16—Eu1—O163.06 (17)O16—C17—H17A110.1
O4—Eu1—O161.65 (18)C18—C17—H17A110.1
O10—Eu1—O1158.99 (19)O16—C17—H17B110.1
O13—Eu1—O1122.21 (17)C18—C17—H17B110.1
O7—Eu1—O1121.04 (17)H17A—C17—H17B108.4
C2A—O1—C18A106.6 (16)O16—C17—H17C109.4
C18—O1—C2110.7 (7)C18A—C17—H17C109.4
C2A—O1—Eu1118.8 (10)O16—C17—H17D109.4
C18A—O1—Eu1118.0 (10)C18A—C17—H17D109.4
C18—O1—Eu1114.0 (5)H17C—C17—H17D108.0
C2—O1—Eu1118.5 (5)O1—C18—C17111.0 (7)
O1—C2—C3109.0 (6)O1—C18—H18A109.4
O1—C2—H2A109.9C17—C18—H18A109.4
C3—C2—H2A109.9O1—C18—H18B109.4
O1—C2—H2B109.9C17—C18—H18B109.4
C3—C2—H2B109.9H18A—C18—H18B108.0
H2A—C2—H2B108.3O1—C18A—C17111.5 (8)
O1—C2A—C3109.2 (7)O1—C18A—H18C109.3
O1—C2A—H2C109.8C17—C18A—H18C109.3
C3—C2A—H2C109.8O1—C18A—H18D109.3
O1—C2A—H2D109.8C17—C18A—H18D109.3
C3—C2A—H2D109.8H18C—C18A—H18D108.0
H2C—C2A—H2D108.3Eu1—O19—H19A119.4
O4—C3—C2106.9 (7)Eu1—O19—H19B131.9
O4—C3—C2A115.1 (9)H19A—O19—H19B105.2
O4—C3—H3A110.3Eu1—O20—H20A120.3
C2—C3—H3A110.3Eu1—O20—H20B134.6
O4—C3—H3B110.3H20A—O20—H20B105.1
C2—C3—H3B110.3Eu1—O21—H21A124.6
H3A—C3—H3B108.6Eu1—O21—H21B132.3
O4—C3—H3C108.5H21A—O21—H21B103.0
C2A—C3—H3C108.5C22—Fe2—C22i180.0 (5)
O4—C3—H3D108.5C22—Fe2—C2388.9 (3)
C2A—C3—H3D108.5C22i—Fe2—C2391.1 (3)
H3C—C3—H3D107.5C22—Fe2—C23i91.1 (3)
C3—O4—C5116.1 (6)C22i—Fe2—C23i88.9 (3)
C3—O4—Eu1123.7 (5)C23—Fe2—C23i180.0 (6)
C5—O4—Eu1117.6 (5)C22—Fe2—C2188.1 (3)
O4—C5—C6108.2 (7)C22i—Fe2—C2191.9 (3)
O4—C5—H5A110.1C23—Fe2—C2188.0 (4)
C6—C5—H5A110.1C23i—Fe2—C2192.0 (4)
O4—C5—H5B110.1C22—Fe2—C21i91.9 (3)
C6—C5—H5B110.1C22i—Fe2—C21i88.1 (3)
H5A—C5—H5B108.4C23—Fe2—C21i92.0 (4)
O7—C6—C5106.3 (7)C23i—Fe2—C21i88.0 (4)
O7—C6—H6A110.5C21—Fe2—C21i180.0 (4)
C5—C6—H6A110.5N21—C21—Fe2176.4 (8)
O7—C6—H6B110.5N22—C22—Fe2178.5 (7)
C5—C6—H6B110.5N23—C23—Fe2176.7 (8)
H6A—C6—H6B108.7C33—Fe3—C33ii180.0 (5)
C6—O7—C8112.2 (6)C33—Fe3—C31ii87.5 (3)
C6—O7—Eu1119.0 (5)C33ii—Fe3—C31ii92.5 (3)
C8—O7—Eu1114.7 (5)C33—Fe3—C3192.5 (3)
O7—C8—C9105.9 (7)C33ii—Fe3—C3187.5 (3)
O7—C8—H8A110.6C31ii—Fe3—C31180.000 (1)
C9—C8—H8A110.6C33—Fe3—C32ii90.2 (3)
O7—C8—H8B110.6C33ii—Fe3—C32ii89.8 (3)
C9—C8—H8B110.6C31ii—Fe3—C32ii89.6 (3)
H8A—C8—H8B108.7C31—Fe3—C32ii90.4 (3)
O10—C9—C8107.3 (6)C33—Fe3—C3289.8 (3)
O10—C9—H9A110.3C33ii—Fe3—C3290.2 (3)
C8—C9—H9A110.3C31ii—Fe3—C3290.4 (3)
O10—C9—H9B110.3C31—Fe3—C3289.6 (3)
C8—C9—H9B110.2C32ii—Fe3—C32180.0 (5)
H9A—C9—H9B108.5N31—C31—Fe3178.8 (7)
C9—O10—C11107.2 (6)N32—C32—Fe3179.1 (8)
C9—O10—Eu1122.0 (5)N33—C33—Fe3177.6 (7)
C11—O10—Eu1120.7 (5)H41A—O41—H41B105.5
O10—C11—C12108.5 (7)H42A—O42—H42B100.3
O19—Eu1—O1—C2A89.4 (14)O10—Eu1—O7—C830.2 (5)
O21—Eu1—O1—C2A126.6 (14)O13—Eu1—O7—C866.2 (6)
O20—Eu1—O1—C2A54.5 (14)O1—Eu1—O7—C8126.1 (5)
O16—Eu1—O1—C2A150.7 (14)C6—O7—C8—C9164.2 (7)
O4—Eu1—O1—C2A29.8 (14)Eu1—O7—C8—C955.9 (8)
O10—Eu1—O1—C2A88.6 (15)O7—C8—C9—O1052.6 (9)
O13—Eu1—O1—C2A173.0 (14)C8—C9—O10—C11174.4 (7)
O7—Eu1—O1—C2A6.2 (14)C8—C9—O10—Eu129.0 (9)
O19—Eu1—O1—C18A42.1 (14)O19—Eu1—O10—C970.6 (6)
O21—Eu1—O1—C18A102.0 (14)O21—Eu1—O10—C9145.0 (6)
O20—Eu1—O1—C18A174.0 (14)O20—Eu1—O10—C974.0 (6)
O16—Eu1—O1—C18A19.2 (14)O16—Eu1—O10—C9143.6 (6)
O4—Eu1—O1—C18A101.7 (14)O4—Eu1—O10—C91.7 (7)
O10—Eu1—O1—C18A139.9 (14)O13—Eu1—O10—C9142.4 (7)
O13—Eu1—O1—C18A41.5 (14)O7—Eu1—O10—C91.1 (6)
O7—Eu1—O1—C18A125.3 (14)O1—Eu1—O10—C9107.5 (7)
O19—Eu1—O1—C1887.4 (5)O19—Eu1—O10—C1170.4 (6)
O21—Eu1—O1—C1856.6 (5)O21—Eu1—O10—C1174.0 (6)
O20—Eu1—O1—C18128.6 (5)O20—Eu1—O10—C11145.1 (6)
O16—Eu1—O1—C1826.1 (5)O16—Eu1—O10—C112.6 (7)
O4—Eu1—O1—C18147.1 (6)O4—Eu1—O10—C11142.6 (6)
O10—Eu1—O1—C1894.6 (7)O13—Eu1—O10—C111.4 (6)
O13—Eu1—O1—C183.8 (6)O7—Eu1—O10—C11142.1 (7)
O7—Eu1—O1—C18170.7 (5)O1—Eu1—O10—C11111.6 (7)
O19—Eu1—O1—C245.6 (6)C9—O10—C11—C12175.6 (8)
O21—Eu1—O1—C2170.3 (6)Eu1—O10—C11—C1229.6 (10)
O20—Eu1—O1—C298.3 (6)O10—C11—C12—O1352.6 (10)
O16—Eu1—O1—C2106.9 (6)C11—C12—O13—C14162.3 (7)
O4—Eu1—O1—C214.0 (6)C11—C12—O13—Eu155.2 (8)
O10—Eu1—O1—C2132.3 (6)O19—Eu1—O13—C12128.9 (6)
O13—Eu1—O1—C2129.3 (6)O21—Eu1—O13—C1262.7 (6)
O7—Eu1—O1—C237.6 (6)O20—Eu1—O13—C1222.4 (6)
C2A—O1—C2—C362.3 (12)O16—Eu1—O13—C12149.4 (6)
C18A—O1—C2—C3153.2 (16)O4—Eu1—O13—C12145.8 (6)
C18—O1—C2—C3173.5 (7)O10—Eu1—O13—C1229.5 (5)
Eu1—O1—C2—C338.9 (10)O7—Eu1—O13—C1265.4 (6)
C18A—O1—C2A—C398 (3)O1—Eu1—O13—C12127.1 (5)
C18—O1—C2A—C3137.8 (14)O19—Eu1—O13—C1491.4 (6)
C2—O1—C2A—C361.9 (12)O21—Eu1—O13—C1477.0 (6)
Eu1—O1—C2A—C339 (3)O20—Eu1—O13—C14117.3 (6)
O1—C2—C3—O448.5 (10)O16—Eu1—O13—C149.7 (5)
O1—C2—C3—C2A61.1 (12)O4—Eu1—O13—C1474.6 (7)
O1—C2A—C3—O423 (3)O10—Eu1—O13—C14169.2 (6)
O1—C2A—C3—C261.9 (13)O7—Eu1—O13—C14154.9 (5)
C2—C3—O4—C5157.6 (8)O1—Eu1—O13—C1412.6 (6)
C2A—C3—O4—C5164.5 (16)C12—O13—C14—C15178.0 (7)
C2—C3—O4—Eu141.1 (9)Eu1—O13—C14—C1537.4 (8)
C2A—C3—O4—Eu13.2 (17)O13—C14—C15—O1653.2 (8)
O19—Eu1—O4—C3139.4 (7)C14—C15—O16—C17129.4 (8)
O21—Eu1—O4—C317.6 (8)C14—C15—O16—Eu150.6 (8)
O20—Eu1—O4—C366.4 (7)O19—Eu1—O16—C17123.1 (7)
O16—Eu1—O4—C367.5 (7)O21—Eu1—O16—C1782.5 (7)
O10—Eu1—O4—C3140.5 (6)O20—Eu1—O16—C1734.7 (8)
O13—Eu1—O4—C3122.6 (7)O4—Eu1—O16—C1751.6 (7)
O7—Eu1—O4—C3141.1 (7)O10—Eu1—O16—C17156.3 (6)
O1—Eu1—O4—C316.4 (6)O13—Eu1—O16—C17157.5 (7)
O19—Eu1—O4—C559.6 (6)O7—Eu1—O16—C17107.5 (7)
O21—Eu1—O4—C5143.4 (6)O1—Eu1—O16—C171.4 (6)
O20—Eu1—O4—C594.6 (7)O19—Eu1—O16—C1557.0 (6)
O16—Eu1—O4—C5131.5 (6)O21—Eu1—O16—C1597.4 (6)
O10—Eu1—O4—C520.4 (7)O20—Eu1—O16—C15145.2 (6)
O13—Eu1—O4—C576.4 (7)O4—Eu1—O16—C15128.5 (6)
O7—Eu1—O4—C519.9 (6)O10—Eu1—O16—C1523.6 (7)
O1—Eu1—O4—C5177.4 (7)O13—Eu1—O16—C1522.4 (6)
C3—O4—C5—C6114.3 (8)O7—Eu1—O16—C1572.6 (7)
Eu1—O4—C5—C648.1 (9)O1—Eu1—O16—C15178.7 (6)
O4—C5—C6—O754.4 (9)C15—O16—C17—C18A160.5 (14)
C5—C6—O7—C8177.7 (7)Eu1—O16—C17—C18A19.6 (16)
C5—C6—O7—Eu139.7 (8)C15—O16—C17—C18158.8 (8)
O19—Eu1—O7—C693.3 (6)Eu1—O16—C17—C1821.1 (10)
O21—Eu1—O7—C6115.6 (6)C2A—O1—C18—C17129.0 (16)
O20—Eu1—O7—C675.1 (6)C18A—O1—C18—C1758.2 (13)
O16—Eu1—O7—C677.6 (7)C2—O1—C18—C1789.1 (10)
O4—Eu1—O7—C612.3 (6)Eu1—O1—C18—C1747.6 (9)
O10—Eu1—O7—C6167.2 (6)O16—C17—C18—O143.6 (11)
O13—Eu1—O7—C6156.8 (5)C18A—C17—C18—O157.8 (13)
O1—Eu1—O7—C610.9 (6)C2A—O1—C18A—C17172.8 (18)
O19—Eu1—O7—C8129.7 (6)C18—O1—C18A—C1759.0 (13)
O21—Eu1—O7—C821.4 (6)C2—O1—C18A—C17151 (3)
O20—Eu1—O7—C861.8 (5)Eu1—O1—C18A—C1736 (3)
O16—Eu1—O7—C8145.4 (5)O16—C17—C18A—O135 (3)
O4—Eu1—O7—C8149.3 (6)C18—C17—C18A—O158.1 (13)
Symmetry codes: (i) x, y+1, z; (ii) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O19—H19A···N210.871.852.713 (10)171
O19—H19B···O420.831.772.582 (8)169
O20—H20A···O410.881.822.677 (8)163
O20—H20B···N330.881.882.745 (9)167
O21—H21A···O410.871.882.695 (8)155
O21—H21B···N32iii0.871.852.718 (9)171
O41—H41A···N22iv0.821.882.698 (9)170
O41—H41B···N33v0.802.423.102 (10)143
O42—H42A···N31vi0.842.002.834 (10)175
O42—H42B···N23vii0.812.022.810 (10)165
Symmetry codes: (iii) x, y+1, z+1; (iv) x, y, z+1; (v) x+1, y+1, z+1; (vi) x, y+1, z1; (vii) x+1, y+1, z.
(V) triaqua(18-crown-6)gadolinium(III) hexacyanochromate(III) dihydrate top
Crystal data top
[Gd(C12H24O6)(H2O)3][Cr(CN)6]·2H2OZ = 2
Mr = 719.76F(000) = 720
Triclinic, P1Dx = 1.647 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 11.0563 (2) ÅCell parameters from 6595 reflections
b = 11.1562 (2) Åθ = 2.9–27.5°
c = 14.2127 (3) ŵ = 2.70 mm1
α = 68.3494 (11)°T = 120 K
β = 70.0959 (12)°Prism, colourless
γ = 66.0299 (12)°0.16 × 0.15 × 0.04 mm
V = 1450.92 (5) Å3
Data collection top
Bruker–Nonius KappaCCD
diffractometer
6646 independent reflections
Radiation source: Bruker–Nonius FR591 rotating anode6382 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
Detector resolution: 9.091 pixels mm-1θmax = 27.5°, θmin = 3.4°
ϕ & ω scansh = 1414
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
k = 1414
Tmin = 0.672, Tmax = 0.899l = 1818
34884 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.108H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0507P)2 + 9.2124P]
where P = (Fo2 + 2Fc2)/3
6646 reflections(Δ/σ)max = 0.001
334 parametersΔρmax = 3.60 e Å3
8 restraintsΔρmin = 1.63 e Å3
Crystal data top
[Gd(C12H24O6)(H2O)3][Cr(CN)6]·2H2Oγ = 66.0299 (12)°
Mr = 719.76V = 1450.92 (5) Å3
Triclinic, P1Z = 2
a = 11.0563 (2) ÅMo Kα radiation
b = 11.1562 (2) ŵ = 2.70 mm1
c = 14.2127 (3) ÅT = 120 K
α = 68.3494 (11)°0.16 × 0.15 × 0.04 mm
β = 70.0959 (12)°
Data collection top
Bruker–Nonius KappaCCD
diffractometer
6646 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
6382 reflections with I > 2σ(I)
Tmin = 0.672, Tmax = 0.899Rint = 0.038
34884 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0408 restraints
wR(F2) = 0.108H-atom parameters constrained
S = 1.04Δρmax = 3.60 e Å3
6646 reflectionsΔρmin = 1.63 e Å3
334 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Gd10.21115 (2)0.72456 (2)0.279303 (15)0.01806 (8)
O10.0618 (3)0.5681 (3)0.3682 (2)0.0249 (7)
C20.0899 (7)0.4598 (8)0.3253 (8)0.0297 (10)*0.458 (7)
C2A0.1330 (8)0.4262 (5)0.3896 (5)0.0297 (10)*0.542 (7)
C30.2388 (5)0.3941 (5)0.2941 (4)0.0353 (12)
O40.2990 (4)0.4985 (4)0.2432 (4)0.0461 (11)
C50.4264 (6)0.4663 (6)0.1679 (5)0.0403 (13)
C60.5252 (5)0.4964 (5)0.1965 (4)0.0322 (11)
O70.4652 (3)0.6338 (3)0.2047 (3)0.0242 (7)
C80.5504 (5)0.6713 (6)0.2388 (5)0.0338 (11)
C90.4962 (5)0.8220 (6)0.2185 (5)0.0339 (11)
O100.3519 (3)0.8611 (3)0.2652 (3)0.0305 (8)
C110.2994 (8)1.0077 (7)0.2354 (8)0.065 (2)
C120.1618 (9)1.0583 (7)0.2497 (10)0.090 (4)
O130.1098 (4)0.9822 (4)0.2203 (3)0.0293 (7)
C140.0342 (7)1.0460 (7)0.2218 (6)0.0511 (16)
C150.0738 (6)0.9580 (5)0.1922 (5)0.0359 (12)
O160.0223 (3)0.8180 (3)0.2506 (3)0.0261 (7)
C170.1214 (5)0.7500 (5)0.2998 (4)0.0320 (11)
C180.0795 (6)0.6364 (9)0.3917 (6)0.0297 (10)*0.458 (7)
C18A0.0495 (7)0.6003 (6)0.3241 (7)0.0297 (10)*0.542 (7)
O190.2388 (4)0.7767 (5)0.1020 (3)0.0364 (9)
O200.3150 (3)0.5812 (3)0.4216 (3)0.0264 (7)
O210.0845 (3)0.8050 (3)0.4289 (2)0.0241 (7)
Cr20.00000.50000.00000.01807 (19)
N210.0580 (7)0.7365 (6)0.0374 (4)0.0495 (13)
N220.1309 (5)0.6085 (5)0.2423 (3)0.0334 (10)
N230.3003 (5)0.3136 (6)0.0358 (4)0.0466 (13)
C210.0315 (6)0.6548 (6)0.0254 (4)0.0311 (10)
C220.0827 (5)0.5693 (5)0.1566 (4)0.0240 (9)
C230.1922 (5)0.3776 (5)0.0238 (4)0.0305 (10)
Cr30.50000.00000.50000.01763 (19)
N310.4262 (4)0.0966 (5)0.7500 (3)0.0322 (9)
N320.1859 (4)0.0726 (5)0.5029 (4)0.0348 (10)
N330.4356 (5)0.3094 (4)0.4976 (4)0.0346 (10)
C310.4518 (4)0.0627 (5)0.6612 (4)0.0235 (9)
C320.2989 (5)0.0460 (5)0.4989 (4)0.0245 (9)
C330.4588 (5)0.1976 (5)0.5018 (4)0.0240 (9)
O410.2465 (4)0.7199 (4)0.5609 (3)0.0310 (8)
O420.4314 (4)0.8577 (5)0.0406 (3)0.0414 (10)
H2A0.04960.49600.26400.036*0.458 (7)
H2B0.04820.39140.37740.036*0.458 (7)
H2C0.06860.37520.41040.036*0.542 (7)
H2D0.17730.39800.44770.036*0.542 (7)
H3A0.27570.33370.35610.042*0.458 (7)
H3B0.25860.33860.24680.042*0.458 (7)
H3C0.30930.30580.31420.042*0.542 (7)
H3D0.19600.38670.24640.042*0.542 (7)
H5A0.41470.52220.09700.048*
H5B0.45830.36900.16950.048*
H6A0.54540.43270.26360.039*
H6B0.61100.48660.14270.039*
H8A0.64570.64250.19980.041*
H8B0.54710.62750.31380.041*
H9A0.54340.85270.24860.041*
H9B0.51150.86520.14270.041*
H11A0.32761.04290.27620.078*
H11B0.34031.04140.16110.078*
H12A0.13541.15450.20810.108*
H12B0.12081.05630.32380.108*
H14A0.05131.13760.17220.061*
H14B0.08661.05540.29220.061*
H15A0.17410.98670.20600.043*
H15B0.03730.96600.11700.043*
H17A0.13070.71320.25000.038*0.458 (7)
H17B0.21050.81530.32260.038*0.458 (7)
H17C0.18220.77570.25320.038*0.542 (7)
H17D0.17710.77650.36460.038*0.542 (7)
H18A0.10280.67340.45140.036*0.458 (7)
H18B0.12930.57130.41150.036*0.458 (7)
H18C0.11330.55160.37360.036*0.542 (7)
H18D0.01570.57030.25970.036*0.542 (7)
H19A0.18760.75990.07530.055 (7)*
H19B0.30400.78980.05310.055 (7)*
H20A0.30750.61000.47450.055 (7)*
H20B0.36660.49430.43690.055 (7)*
H21A0.12110.79380.47920.055 (7)*
H21B0.00140.85140.44870.055 (7)*
H41A0.21490.69130.62400.055 (7)*
H41B0.30450.74860.55850.055 (7)*
H42A0.42600.87040.10210.055 (7)*
H42B0.50570.79780.03810.055 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Gd10.01794 (12)0.02037 (12)0.01745 (12)0.00866 (8)0.00270 (8)0.00512 (8)
O10.0286 (17)0.0291 (17)0.0229 (15)0.0176 (14)0.0049 (13)0.0048 (13)
C30.046 (3)0.025 (2)0.039 (3)0.016 (2)0.004 (2)0.011 (2)
O40.035 (2)0.041 (2)0.072 (3)0.0248 (18)0.018 (2)0.039 (2)
C50.036 (3)0.039 (3)0.049 (3)0.013 (2)0.006 (2)0.029 (3)
C60.028 (2)0.025 (2)0.038 (3)0.0043 (19)0.001 (2)0.013 (2)
O70.0202 (15)0.0237 (16)0.0299 (17)0.0069 (13)0.0048 (13)0.0095 (13)
C80.019 (2)0.039 (3)0.047 (3)0.009 (2)0.006 (2)0.019 (2)
C90.026 (2)0.036 (3)0.046 (3)0.015 (2)0.003 (2)0.016 (2)
O100.0209 (16)0.0234 (17)0.052 (2)0.0061 (13)0.0084 (15)0.0165 (16)
C110.052 (4)0.029 (3)0.137 (8)0.003 (3)0.047 (5)0.033 (4)
C120.077 (6)0.024 (3)0.193 (12)0.018 (3)0.088 (7)0.001 (5)
O130.0304 (18)0.0252 (17)0.0312 (18)0.0129 (14)0.0113 (14)0.0019 (14)
C140.047 (4)0.034 (3)0.064 (4)0.009 (3)0.020 (3)0.001 (3)
C150.029 (3)0.026 (2)0.048 (3)0.001 (2)0.021 (2)0.003 (2)
O160.0185 (15)0.0235 (16)0.0333 (18)0.0080 (13)0.0078 (13)0.0011 (13)
C170.020 (2)0.040 (3)0.035 (3)0.016 (2)0.0051 (19)0.003 (2)
O190.0254 (17)0.064 (3)0.0199 (16)0.0144 (17)0.0040 (13)0.0128 (17)
O200.0306 (17)0.0216 (16)0.0218 (16)0.0027 (13)0.0092 (13)0.0038 (12)
O210.0194 (15)0.0303 (17)0.0214 (15)0.0039 (13)0.0046 (12)0.0100 (13)
Cr20.0183 (4)0.0221 (5)0.0163 (4)0.0111 (4)0.0034 (3)0.0031 (4)
N210.071 (4)0.054 (3)0.043 (3)0.038 (3)0.012 (3)0.015 (2)
N220.040 (2)0.040 (2)0.024 (2)0.023 (2)0.0050 (18)0.0031 (18)
N230.028 (2)0.049 (3)0.051 (3)0.013 (2)0.013 (2)0.003 (2)
C210.038 (3)0.036 (3)0.026 (2)0.019 (2)0.007 (2)0.008 (2)
C220.026 (2)0.027 (2)0.023 (2)0.0125 (18)0.0064 (17)0.0067 (18)
C230.024 (2)0.032 (3)0.030 (2)0.010 (2)0.0068 (19)0.001 (2)
Cr30.0155 (4)0.0174 (4)0.0186 (4)0.0067 (3)0.0033 (3)0.0022 (3)
N310.028 (2)0.040 (2)0.025 (2)0.0118 (19)0.0052 (16)0.0050 (18)
N320.022 (2)0.047 (3)0.037 (2)0.0090 (19)0.0059 (17)0.017 (2)
N330.037 (2)0.021 (2)0.045 (3)0.0082 (18)0.015 (2)0.0052 (18)
C310.0164 (19)0.023 (2)0.027 (2)0.0046 (16)0.0048 (17)0.0050 (17)
C320.022 (2)0.027 (2)0.024 (2)0.0083 (18)0.0033 (17)0.0077 (18)
C330.021 (2)0.024 (2)0.026 (2)0.0085 (17)0.0059 (17)0.0032 (17)
O410.040 (2)0.045 (2)0.0179 (15)0.0294 (17)0.0045 (14)0.0031 (14)
O420.0292 (19)0.060 (3)0.0216 (17)0.0061 (18)0.0053 (14)0.0065 (17)
Geometric parameters (Å, º) top
Gd1—O192.307 (3)C14—C151.453 (9)
Gd1—O212.377 (3)C14—H14A0.99
Gd1—O202.381 (3)C14—H14B0.99
Gd1—O162.476 (3)C15—O161.448 (6)
Gd1—O42.489 (4)C15—H15A0.99
Gd1—O102.504 (3)C15—H15B0.99
Gd1—O132.543 (3)O16—C171.423 (6)
Gd1—O72.548 (3)C17—C18A1.491 (5)
Gd1—O12.581 (3)C17—C181.497 (5)
O1—C181.413 (5)C17—H17A0.99
O1—C2A1.419 (5)C17—H17B0.99
O1—C18A1.426 (5)C17—H17C0.99
O1—C21.427 (5)C17—H17D0.99
C2—C31.485 (5)C18—H18A0.99
C2—H2A0.99C18—H18B0.99
C2—H2B0.99C18A—H18C0.99
C2A—C31.509 (5)C18A—H18D0.99
C2A—H2C0.99O19—H19A0.89
C2A—H2D0.99O19—H19B0.83
C3—O41.415 (6)O20—H20A0.89
C3—H3A0.99O20—H20B0.89
C3—H3B0.99O21—H21A0.88
C3—H3C0.99O21—H21B0.88
C3—H3D0.99Cr2—C212.066 (5)
O4—C51.450 (6)Cr2—C21i2.066 (5)
C5—C61.473 (8)Cr2—C232.070 (5)
C5—H5A0.99Cr2—C23i2.070 (5)
C5—H5B0.99Cr2—C22i2.075 (5)
C6—O71.435 (6)Cr2—C222.075 (5)
C6—H6A0.99N21—C211.145 (7)
C6—H6B0.99N22—C221.146 (6)
O7—C81.441 (6)N23—C231.150 (7)
C8—C91.486 (8)Cr3—C332.071 (5)
C8—H8A0.99Cr3—C33ii2.071 (5)
C8—H8B0.99Cr3—C32ii2.074 (5)
C9—O101.450 (6)Cr3—C322.074 (5)
C9—H9A0.99Cr3—C31ii2.076 (5)
C9—H9B0.99Cr3—C312.076 (5)
O10—C111.441 (7)N31—C311.143 (6)
C11—C121.360 (11)N32—C321.147 (6)
C11—H11A0.99N33—C331.149 (7)
C11—H11B0.99O41—H41A0.83
C12—O131.432 (8)O41—H41B0.81
C12—H12A0.99O42—H42A0.85
C12—H12B0.99O42—H42B0.82
O13—C141.453 (7)
O19—Gd1—O21144.08 (13)C12—C11—H11A108.8
O19—Gd1—O20144.24 (13)O10—C11—H11A108.8
O21—Gd1—O2070.73 (11)C12—C11—H11B108.8
O19—Gd1—O1675.00 (12)O10—C11—H11B108.8
O21—Gd1—O1678.66 (11)H11A—C11—H11B107.7
O20—Gd1—O16135.57 (12)C11—C12—O13111.9 (8)
O19—Gd1—O476.01 (16)C11—C12—H12A109.2
O21—Gd1—O4134.26 (14)O13—C12—H12A109.2
O20—Gd1—O478.39 (15)C11—C12—H12B109.2
O16—Gd1—O4102.87 (13)O13—C12—H12B109.2
O19—Gd1—O1093.87 (14)H12A—C12—H12B107.9
O21—Gd1—O1082.15 (12)C12—O13—C14112.4 (5)
O20—Gd1—O1081.39 (12)C12—O13—Gd1115.8 (3)
O16—Gd1—O10125.86 (11)C14—O13—Gd1120.5 (3)
O4—Gd1—O10125.97 (12)O13—C14—C15106.7 (5)
O19—Gd1—O1374.60 (14)O13—C14—H14A110.4
O21—Gd1—O1371.80 (12)C15—C14—H14A110.4
O20—Gd1—O13130.99 (12)O13—C14—H14B110.4
O16—Gd1—O1362.80 (11)C15—C14—H14B110.4
O4—Gd1—O13149.82 (15)H14A—C14—H14B108.6
O10—Gd1—O1363.16 (11)O16—C15—C14110.1 (5)
O19—Gd1—O773.45 (12)O16—C15—H15A109.6
O21—Gd1—O7132.65 (11)C14—C15—H15A109.6
O20—Gd1—O772.82 (11)O16—C15—H15B109.6
O16—Gd1—O7147.74 (11)C14—C15—H15B109.6
O4—Gd1—O762.94 (11)H15A—C15—H15B108.2
O10—Gd1—O763.30 (11)C17—O16—C15114.4 (4)
O13—Gd1—O7113.99 (11)C17—O16—Gd1124.6 (3)
O19—Gd1—O1108.29 (13)C15—O16—Gd1120.4 (3)
O21—Gd1—O179.92 (11)O16—C17—C18A108.4 (5)
O20—Gd1—O180.48 (11)O16—C17—C18109.7 (5)
O16—Gd1—O162.74 (10)O16—C17—H17A109.7
O4—Gd1—O162.02 (11)C18—C17—H17A109.7
O10—Gd1—O1157.84 (12)O16—C17—H17B109.7
O13—Gd1—O1122.13 (11)C18—C17—H17B109.7
O7—Gd1—O1122.25 (10)H17A—C17—H17B108.2
C2A—O1—C18A110.6 (5)O16—C17—H17C110.0
C18—O1—C2110.6 (6)C18A—C17—H17C110.0
C18A—O1—C272.8 (4)O16—C17—H17D110.0
C18—O1—Gd1115.1 (4)C18A—C17—H17D110.0
C2A—O1—Gd1115.6 (4)H17C—C17—H17D108.4
C18A—O1—Gd1116.4 (4)O1—C18—C17110.3 (5)
C2—O1—Gd1117.8 (4)O1—C18—H18A109.6
O1—C2—C3110.5 (5)C17—C18—H18A109.6
O1—C2—H2A109.5O1—C18—H18B109.6
C3—C2—H2A109.5C17—C18—H18B109.6
O1—C2—H2B109.5H18A—C18—H18B108.1
C3—C2—H2B109.5O1—C18A—C17109.9 (5)
H2A—C2—H2B108.1O1—C18A—H18C109.7
O1—C2A—C3109.6 (5)C17—C18A—H18C109.7
O1—C2A—H2C109.8O1—C18A—H18D109.7
C3—C2A—H2C109.8C17—C18A—H18D109.7
O1—C2A—H2D109.8H18C—C18A—H18D108.2
C3—C2A—H2D109.8Gd1—O19—H19A121.1
H2C—C2A—H2D108.2Gd1—O19—H19B131.4
O4—C3—C2107.8 (5)H19A—O19—H19B105.1
O4—C3—C2A109.6 (5)Gd1—O20—H20A122.9
O4—C3—H3A110.1Gd1—O20—H20B133.1
C2—C3—H3A110.1H20A—O20—H20B104.1
O4—C3—H3B110.1Gd1—O21—H21A123.2
C2—C3—H3B110.1Gd1—O21—H21B133.1
H3A—C3—H3B108.5H21A—O21—H21B103.7
O4—C3—H3C109.7C21—Cr2—C21i180.0 (3)
C2A—C3—H3C109.7C21—Cr2—C2388.2 (2)
O4—C3—H3D109.7C21i—Cr2—C2391.8 (2)
C2A—C3—H3D109.7C21—Cr2—C23i91.8 (2)
H3C—C3—H3D108.2C21i—Cr2—C23i88.2 (2)
C3—O4—C5116.3 (4)C23—Cr2—C23i180.00 (18)
C3—O4—Gd1125.5 (3)C21—Cr2—C22i91.82 (19)
C5—O4—Gd1118.1 (3)C21i—Cr2—C22i88.18 (19)
O4—C5—C6107.1 (4)C23—Cr2—C22i90.10 (19)
O4—C5—H5A110.3C23i—Cr2—C22i89.90 (19)
C6—C5—H5A110.3C21—Cr2—C2288.18 (19)
O4—C5—H5B110.3C21i—Cr2—C2291.82 (19)
C6—C5—H5B110.3C23—Cr2—C2289.90 (19)
H5A—C5—H5B108.6C23i—Cr2—C2290.10 (19)
O7—C6—C5107.2 (4)C22i—Cr2—C22180.0 (4)
O7—C6—H6A110.3N21—C21—Cr2175.5 (6)
C5—C6—H6A110.3N22—C22—Cr2178.1 (4)
O7—C6—H6B110.3N23—C23—Cr2177.6 (5)
C5—C6—H6B110.3C33—Cr3—C33ii180.0
H6A—C6—H6B108.5C33—Cr3—C32ii90.41 (18)
C6—O7—C8111.8 (4)C33ii—Cr3—C32ii89.59 (18)
C6—O7—Gd1119.6 (3)C33—Cr3—C3289.59 (18)
C8—O7—Gd1115.4 (3)C33ii—Cr3—C3290.41 (18)
O7—C8—C9106.4 (4)C32ii—Cr3—C32180.000 (1)
O7—C8—H8A110.5C33—Cr3—C31ii88.76 (18)
C9—C8—H8A110.5C33ii—Cr3—C31ii91.24 (18)
O7—C8—H8B110.5C32ii—Cr3—C31ii89.76 (18)
C9—C8—H8B110.5C32—Cr3—C31ii90.24 (18)
H8A—C8—H8B108.6C33—Cr3—C3191.24 (18)
O10—C9—C8108.6 (4)C33ii—Cr3—C3188.76 (18)
O10—C9—H9A110.0C32ii—Cr3—C3190.24 (18)
C8—C9—H9A110.0C32—Cr3—C3189.76 (18)
O10—C9—H9B110.0C31ii—Cr3—C31180.0
C8—C9—H9B110.0N31—C31—Cr3179.2 (4)
H9A—C9—H9B108.3N32—C32—Cr3176.7 (4)
C11—O10—C9107.5 (5)N33—C33—Cr3176.5 (4)
C11—O10—Gd1120.0 (3)H41A—O41—H41B105.1
C9—O10—Gd1120.8 (3)H42A—O42—H42B101.4
C12—C11—O10113.8 (6)
O19—Gd1—O1—C1889.6 (5)O10—Gd1—O7—C827.2 (3)
O21—Gd1—O1—C1854.2 (4)O13—Gd1—O7—C866.2 (3)
O20—Gd1—O1—C18126.2 (5)O1—Gd1—O7—C8128.1 (3)
O16—Gd1—O1—C1828.1 (4)C6—O7—C8—C9165.9 (4)
O4—Gd1—O1—C18152.0 (5)Gd1—O7—C8—C952.8 (5)
O10—Gd1—O1—C1890.7 (5)O7—C8—C9—O1052.4 (6)
O13—Gd1—O1—C186.7 (5)C8—C9—O10—C11174.2 (5)
O7—Gd1—O1—C18171.2 (4)C8—C9—O10—Gd131.3 (6)
O19—Gd1—O1—C2A92.5 (4)O19—Gd1—O10—C1172.5 (6)
O21—Gd1—O1—C2A123.7 (4)O21—Gd1—O10—C1171.6 (6)
O20—Gd1—O1—C2A51.7 (4)O20—Gd1—O10—C11143.1 (6)
O16—Gd1—O1—C2A154.0 (4)O16—Gd1—O10—C111.7 (6)
O4—Gd1—O1—C2A30.1 (4)O4—Gd1—O10—C11148.0 (5)
O10—Gd1—O1—C2A87.2 (5)O13—Gd1—O10—C112.0 (5)
O13—Gd1—O1—C2A175.4 (4)O7—Gd1—O10—C11141.8 (6)
O7—Gd1—O1—C2A10.9 (4)O1—Gd1—O10—C11107.8 (6)
O19—Gd1—O1—C18A39.9 (4)O19—Gd1—O10—C965.9 (4)
O21—Gd1—O1—C18A104.0 (4)O21—Gd1—O10—C9150.1 (4)
O20—Gd1—O1—C18A175.9 (4)O20—Gd1—O10—C978.5 (4)
O16—Gd1—O1—C18A21.6 (4)O16—Gd1—O10—C9140.1 (4)
O4—Gd1—O1—C18A102.2 (4)O4—Gd1—O10—C99.7 (4)
O10—Gd1—O1—C18A140.4 (4)O13—Gd1—O10—C9136.4 (4)
O13—Gd1—O1—C18A43.1 (4)O7—Gd1—O10—C93.4 (4)
O7—Gd1—O1—C18A121.5 (4)O1—Gd1—O10—C9113.8 (4)
O19—Gd1—O1—C243.8 (5)C9—O10—C11—C12163.5 (9)
O21—Gd1—O1—C2172.4 (5)Gd1—O10—C11—C1220.2 (11)
O20—Gd1—O1—C2100.4 (5)O10—C11—C12—O1340.9 (13)
O16—Gd1—O1—C2105.3 (5)C11—C12—O13—C14172.2 (8)
O4—Gd1—O1—C218.6 (5)C11—C12—O13—Gd143.8 (11)
O10—Gd1—O1—C2135.9 (5)O19—Gd1—O13—C12125.8 (6)
O13—Gd1—O1—C2126.7 (5)O21—Gd1—O13—C1267.1 (6)
O7—Gd1—O1—C237.8 (5)O20—Gd1—O13—C1225.3 (7)
C18—O1—C2—C3176.2 (6)O16—Gd1—O13—C12153.4 (7)
C2A—O1—C2—C357.9 (6)O4—Gd1—O13—C12139.3 (6)
C18A—O1—C2—C3152.2 (9)O10—Gd1—O13—C1223.2 (6)
Gd1—O1—C2—C340.9 (9)O7—Gd1—O13—C1262.3 (6)
C18—O1—C2A—C3134.2 (7)O1—Gd1—O13—C12132.0 (6)
C18A—O1—C2A—C386.7 (7)O19—Gd1—O13—C1493.2 (4)
C2—O1—C2A—C356.0 (6)O21—Gd1—O13—C1473.9 (4)
Gd1—O1—C2A—C348.3 (7)O20—Gd1—O13—C14115.6 (4)
O1—C2—C3—O443.4 (9)O16—Gd1—O13—C1412.5 (4)
O1—C2—C3—C2A56.3 (6)O4—Gd1—O13—C1479.8 (5)
O1—C2A—C3—O438.6 (8)O10—Gd1—O13—C14164.2 (5)
O1—C2A—C3—C256.3 (6)O7—Gd1—O13—C14156.7 (4)
C2—C3—O4—C5153.2 (6)O1—Gd1—O13—C149.0 (5)
C2A—C3—O4—C5163.5 (6)C12—O13—C14—C15179.1 (7)
C2—C3—O4—Gd130.3 (7)Gd1—O13—C14—C1536.9 (7)
C2A—C3—O4—Gd113.0 (7)O13—C14—C15—O1647.7 (7)
O19—Gd1—O4—C3127.8 (5)C14—C15—O16—C17129.5 (5)
O21—Gd1—O4—C329.5 (6)C14—C15—O16—Gd142.1 (6)
O20—Gd1—O4—C377.4 (5)O19—Gd1—O16—C17125.3 (4)
O16—Gd1—O4—C357.1 (5)O21—Gd1—O16—C1779.3 (4)
O10—Gd1—O4—C3147.7 (4)O20—Gd1—O16—C1732.6 (4)
O13—Gd1—O4—C3114.4 (5)O4—Gd1—O16—C1753.9 (4)
O7—Gd1—O4—C3153.9 (5)O10—Gd1—O16—C17150.9 (4)
O1—Gd1—O4—C37.9 (4)O13—Gd1—O16—C17154.6 (4)
O19—Gd1—O4—C555.8 (4)O7—Gd1—O16—C17113.0 (4)
O21—Gd1—O4—C5146.9 (4)O1—Gd1—O16—C175.1 (4)
O20—Gd1—O4—C599.0 (5)O19—Gd1—O16—C1564.0 (4)
O16—Gd1—O4—C5126.5 (4)O21—Gd1—O16—C1591.3 (4)
O10—Gd1—O4—C528.8 (5)O20—Gd1—O16—C15138.1 (4)
O13—Gd1—O4—C569.2 (5)O4—Gd1—O16—C15135.5 (4)
O7—Gd1—O4—C522.5 (4)O10—Gd1—O16—C1519.8 (4)
O1—Gd1—O4—C5175.7 (5)O13—Gd1—O16—C1516.1 (4)
C3—O4—C5—C6126.7 (5)O7—Gd1—O16—C1576.3 (4)
Gd1—O4—C5—C650.0 (6)O1—Gd1—O16—C15175.8 (4)
O4—C5—C6—O753.2 (6)C15—O16—C17—C18A160.4 (5)
C5—C6—O7—C8176.4 (4)Gd1—O16—C17—C18A28.4 (6)
C5—C6—O7—Gd137.0 (5)C15—O16—C17—C18154.9 (6)
O19—Gd1—O7—C691.6 (4)Gd1—O16—C17—C1816.3 (7)
O21—Gd1—O7—C6117.4 (3)C2A—O1—C18—C17135.0 (7)
O20—Gd1—O7—C676.4 (3)C18A—O1—C18—C1755.6 (6)
O16—Gd1—O7—C679.2 (4)C2—O1—C18—C1789.3 (9)
O4—Gd1—O7—C69.1 (3)Gd1—O1—C18—C1747.4 (8)
O10—Gd1—O7—C6165.2 (4)O16—C17—C18—O140.4 (9)
O13—Gd1—O7—C6155.8 (3)C18A—C17—C18—O155.5 (6)
O1—Gd1—O7—C69.9 (4)C18—O1—C18A—C1755.7 (6)
O19—Gd1—O7—C8130.4 (4)C2A—O1—C18A—C17178.7 (5)
O21—Gd1—O7—C820.7 (4)C2—O1—C18A—C17157.2 (8)
O20—Gd1—O7—C861.7 (3)Gd1—O1—C18A—C1744.1 (7)
O16—Gd1—O7—C8142.8 (3)O16—C17—C18A—O144.9 (8)
O4—Gd1—O7—C8147.2 (4)C18—C17—C18A—O154.5 (6)
Symmetry codes: (i) x, y+1, z; (ii) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O19—H19A···N210.891.832.706 (7)170
O19—H19B···O420.831.782.594 (6)165
O20—H20A···O410.891.832.679 (5)160
O20—H20B···N330.891.852.723 (5)165
O21—H21A···O410.881.852.688 (5)158
O21—H21B···N32iii0.881.852.725 (5)173
O41—H41A···N22iv0.831.882.701 (5)169
O41—H41B···N33v0.812.573.230 (6)139
O42—H42A···N31vi0.851.992.846 (6)176
O42—H42B···N23vii0.822.002.809 (6)167
Symmetry codes: (iii) x, y+1, z+1; (iv) x, y, z+1; (v) x+1, y+1, z+1; (vi) x, y+1, z1; (vii) x+1, y+1, z.
(VII) triaqua(18-crown-6)gadolinium(III) hexacyanocobaltate(III) dihydrate top
Crystal data top
[Gd(C12H24O6)(H2O)3][Co(CN)6]·2H2OZ = 2
Mr = 726.69F(000) = 726
Triclinic, P1Dx = 1.742 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.8604 (2) ÅCell parameters from 6164 reflections
b = 11.0724 (3) Åθ = 2.9–27.5°
c = 13.9909 (2) ŵ = 3.03 mm1
α = 67.5857 (10)°T = 120 K
β = 70.5870 (8)°Block, colourless
γ = 65.5666 (9)°0.60 × 0.54 × 0.42 mm
V = 1385.20 (5) Å3
Data collection top
Bruker–Nonius KappaCCD
diffractometer
6348 independent reflections
Radiation source: Bruker–Nonius FR591 rotating anode6022 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
Detector resolution: 9.091 pixels mm-1θmax = 27.6°, θmin = 3.2°
ϕ & ω scansh = 1414
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
k = 1414
Tmin = 0.187, Tmax = 0.280l = 1818
27907 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.020Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.047H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.0144P)2 + 1.6153P]
where P = (Fo2 + 2Fc2)/3
6348 reflections(Δ/σ)max = 0.001
334 parametersΔρmax = 1.00 e Å3
8 restraintsΔρmin = 0.91 e Å3
Crystal data top
[Gd(C12H24O6)(H2O)3][Co(CN)6]·2H2Oγ = 65.5666 (9)°
Mr = 726.69V = 1385.20 (5) Å3
Triclinic, P1Z = 2
a = 10.8604 (2) ÅMo Kα radiation
b = 11.0724 (3) ŵ = 3.03 mm1
c = 13.9909 (2) ÅT = 120 K
α = 67.5857 (10)°0.60 × 0.54 × 0.42 mm
β = 70.5870 (8)°
Data collection top
Bruker–Nonius KappaCCD
diffractometer
6348 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
6022 reflections with I > 2σ(I)
Tmin = 0.187, Tmax = 0.280Rint = 0.033
27907 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0208 restraints
wR(F2) = 0.047H-atom parameters constrained
S = 1.09Δρmax = 1.00 e Å3
6348 reflectionsΔρmin = 0.91 e Å3
334 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Gd10.204535 (10)0.727652 (10)0.276475 (8)0.00822 (4)
O10.05822 (16)0.56550 (15)0.36672 (12)0.0145 (3)
C20.0911 (3)0.4532 (3)0.3232 (3)0.0196 (8)*0.777 (6)
C2A0.1288 (8)0.4225 (5)0.3849 (5)0.015 (3)*0.223 (6)
C30.2409 (3)0.3959 (2)0.2899 (2)0.0230 (5)
O40.29066 (18)0.50784 (17)0.22885 (15)0.0239 (4)
C50.4213 (3)0.4760 (3)0.1564 (2)0.0228 (5)
C60.5233 (2)0.4976 (2)0.1919 (2)0.0211 (5)
O70.46241 (15)0.63674 (16)0.20197 (12)0.0139 (3)
C80.5485 (3)0.6706 (3)0.2393 (2)0.0223 (5)
C90.4943 (2)0.8238 (3)0.2179 (2)0.0241 (5)
O100.34693 (16)0.86517 (16)0.26154 (14)0.0178 (3)
C110.2942 (3)1.0150 (2)0.2307 (2)0.0250 (6)
C120.1410 (3)1.0610 (2)0.2646 (2)0.0210 (5)
O130.09491 (16)0.98866 (15)0.22438 (12)0.0143 (3)
C140.0504 (2)1.0504 (2)0.22211 (19)0.0182 (5)
C150.0819 (2)0.9613 (2)0.18275 (19)0.0183 (5)
O160.03335 (16)0.82085 (16)0.24904 (13)0.0158 (3)
C170.1311 (2)0.7489 (3)0.29388 (19)0.0236 (5)
C180.0862 (3)0.6340 (3)0.3892 (2)0.0189 (8)*0.777 (6)
C18A0.0618 (8)0.5992 (6)0.3289 (9)0.023 (3)*0.223 (6)
O190.22824 (16)0.79333 (17)0.09573 (12)0.0155 (3)
O200.31546 (16)0.57135 (16)0.41987 (12)0.0154 (3)
O210.07935 (16)0.79714 (16)0.43348 (12)0.0145 (3)
Co20.00000.50000.00000.00891 (8)
N210.0594 (2)0.7237 (2)0.03509 (16)0.0240 (5)
N220.1318 (2)0.5971 (2)0.23171 (15)0.0191 (4)
N230.2878 (2)0.3122 (2)0.03837 (18)0.0276 (5)
C210.0338 (2)0.6403 (2)0.02316 (17)0.0150 (4)
C220.0807 (2)0.5597 (2)0.14435 (17)0.0125 (4)
C230.1778 (2)0.3806 (2)0.02529 (17)0.0156 (5)
Co30.50000.00000.50000.00877 (8)
N310.4334 (2)0.0968 (2)0.74058 (15)0.0203 (4)
N320.1966 (2)0.0807 (2)0.49815 (16)0.0206 (4)
N330.4513 (2)0.2934 (2)0.49433 (17)0.0219 (4)
C310.4576 (2)0.0594 (2)0.64972 (18)0.0138 (4)
C320.3116 (2)0.0495 (2)0.49810 (17)0.0128 (4)
C330.4692 (2)0.1811 (2)0.49969 (17)0.0138 (4)
O410.25167 (17)0.70080 (18)0.56594 (12)0.0196 (4)
O420.43567 (18)0.8541 (2)0.04606 (13)0.0263 (4)
H2A0.04700.48810.26190.023*0.777 (6)
H2B0.05490.38020.37720.023*0.777 (6)
H2C0.06320.37400.39860.018*0.223 (6)
H2D0.16990.38650.44780.018*0.223 (6)
H3A0.28380.34300.35240.028*0.777 (6)
H3B0.26380.33280.24730.028*0.777 (6)
H3C0.31910.31370.31390.028*0.223 (6)
H3D0.20490.37400.24430.028*0.223 (6)
H5A0.41210.53710.08410.027*
H5B0.45230.37880.15540.027*
H6A0.54110.42960.26060.025*
H6B0.61180.48740.13940.025*
H8A0.64590.64020.20150.027*
H8B0.54400.62480.31590.027*
H9A0.54130.85260.25090.029*
H9B0.51200.86870.14080.029*
H11A0.32101.05160.15310.030*
H11B0.33371.05070.26450.030*
H12A0.11321.03730.34260.025*
H12B0.10101.16220.23510.025*
H14A0.07041.14590.17430.022*
H14B0.10661.05330.29380.022*
H15A0.18260.99100.18750.022*
H15B0.03410.96740.10810.022*
H17A0.13430.71050.24170.028*0.777 (6)
H17B0.22440.81270.31470.028*0.777 (6)
H17C0.18400.76990.24070.028*0.223 (6)
H17D0.19710.78090.35480.028*0.223 (6)
H18A0.11040.67240.44890.023*0.777 (6)
H18B0.13550.56700.41030.023*0.777 (6)
H18C0.12710.55620.38590.028*0.223 (6)
H18D0.03530.56020.26920.028*0.223 (6)
H19A0.17700.77650.06900.042 (3)*
H19B0.29340.80640.04690.042 (3)*
H20A0.30790.60010.47280.042 (3)*
H20B0.36700.48450.43510.042 (3)*
H21A0.11600.78590.48380.042 (3)*
H21B0.00650.84350.45320.042 (3)*
H41A0.22010.67220.62900.042 (3)*
H41B0.30970.72950.56350.042 (3)*
H42A0.43020.86670.10760.042 (3)*
H42B0.51000.79420.04360.042 (3)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Gd10.00784 (6)0.00869 (5)0.00750 (5)0.00356 (4)0.00049 (4)0.00167 (4)
O10.0161 (8)0.0162 (8)0.0137 (7)0.0097 (7)0.0020 (6)0.0029 (6)
C30.0342 (15)0.0135 (11)0.0201 (12)0.0119 (11)0.0009 (11)0.0046 (9)
O40.0192 (9)0.0183 (9)0.0354 (10)0.0109 (7)0.0082 (8)0.0155 (8)
C50.0220 (13)0.0211 (12)0.0252 (13)0.0065 (11)0.0047 (10)0.0152 (10)
C60.0150 (12)0.0176 (12)0.0259 (13)0.0014 (10)0.0010 (10)0.0101 (10)
O70.0098 (7)0.0142 (8)0.0174 (8)0.0024 (6)0.0019 (6)0.0069 (6)
C80.0139 (12)0.0263 (13)0.0301 (14)0.0070 (10)0.0032 (10)0.0123 (11)
C90.0142 (12)0.0278 (13)0.0344 (15)0.0109 (11)0.0002 (10)0.0127 (11)
O100.0109 (8)0.0138 (8)0.0300 (9)0.0040 (6)0.0037 (7)0.0083 (7)
C110.0231 (13)0.0134 (11)0.0407 (16)0.0076 (10)0.0086 (11)0.0066 (11)
C120.0233 (13)0.0112 (11)0.0311 (14)0.0050 (10)0.0085 (11)0.0072 (10)
O130.0135 (8)0.0107 (7)0.0180 (8)0.0028 (6)0.0047 (6)0.0034 (6)
C140.0147 (11)0.0137 (11)0.0194 (12)0.0005 (9)0.0047 (9)0.0014 (9)
C150.0146 (11)0.0165 (11)0.0182 (12)0.0016 (9)0.0077 (9)0.0008 (9)
O160.0103 (8)0.0136 (8)0.0225 (8)0.0050 (6)0.0055 (6)0.0013 (6)
C170.0134 (12)0.0315 (14)0.0214 (12)0.0131 (11)0.0025 (10)0.0025 (10)
O190.0147 (8)0.0252 (9)0.0083 (7)0.0106 (7)0.0003 (6)0.0044 (6)
O200.0191 (8)0.0117 (7)0.0121 (8)0.0011 (7)0.0059 (6)0.0021 (6)
O210.0097 (8)0.0200 (8)0.0124 (7)0.0013 (6)0.0025 (6)0.0069 (6)
Co20.00843 (19)0.01094 (19)0.00770 (18)0.00513 (16)0.00152 (15)0.00100 (15)
N210.0344 (13)0.0270 (11)0.0189 (11)0.0186 (10)0.0061 (9)0.0054 (9)
N220.0199 (11)0.0226 (10)0.0149 (10)0.0105 (9)0.0015 (8)0.0034 (8)
N230.0158 (11)0.0263 (12)0.0317 (12)0.0054 (9)0.0080 (9)0.0020 (10)
C210.0159 (11)0.0184 (11)0.0101 (10)0.0083 (9)0.0017 (8)0.0014 (9)
C220.0114 (10)0.0133 (10)0.0147 (11)0.0048 (9)0.0047 (9)0.0036 (8)
C230.0156 (12)0.0170 (11)0.0123 (10)0.0085 (10)0.0014 (9)0.0000 (9)
Co30.00643 (19)0.00789 (18)0.00924 (19)0.00176 (15)0.00050 (15)0.00120 (15)
N310.0167 (10)0.0264 (11)0.0135 (10)0.0066 (9)0.0012 (8)0.0032 (8)
N320.0135 (10)0.0263 (11)0.0191 (10)0.0052 (9)0.0013 (8)0.0068 (9)
N330.0232 (11)0.0140 (10)0.0272 (11)0.0048 (9)0.0075 (9)0.0039 (8)
C310.0081 (10)0.0126 (10)0.0179 (12)0.0025 (8)0.0006 (8)0.0043 (9)
C320.0140 (11)0.0121 (10)0.0102 (10)0.0055 (9)0.0000 (8)0.0018 (8)
C330.0104 (10)0.0148 (11)0.0130 (10)0.0031 (9)0.0013 (8)0.0026 (8)
O410.0207 (9)0.0316 (10)0.0100 (8)0.0161 (8)0.0014 (6)0.0027 (7)
O420.0134 (9)0.0424 (11)0.0132 (8)0.0070 (8)0.0005 (7)0.0018 (8)
Geometric parameters (Å, º) top
Gd1—O192.3042 (15)C14—C151.488 (3)
Gd1—O212.3883 (15)C14—H14A0.99
Gd1—O202.3887 (15)C14—H14B0.99
Gd1—O162.4573 (15)C15—O161.450 (3)
Gd1—O42.4863 (16)C15—H15A0.99
Gd1—O102.4989 (15)C15—H15B0.99
Gd1—O132.5347 (15)O16—C171.425 (3)
Gd1—O72.5437 (15)C17—C18A1.465 (5)
Gd1—O12.5769 (14)C17—C181.504 (3)
O1—C2A1.406 (5)C17—H17A0.99
O1—C181.416 (3)C17—H17B0.99
O1—C18A1.423 (5)C17—H17C0.99
O1—C21.452 (3)C17—H17D0.99
C2—C31.461 (3)C18—H18A0.99
C2—H2A0.99C18—H18B0.99
C2—H2B0.99C18A—H18C0.99
C2A—C31.504 (5)C18A—H18D0.99
C2A—H2C0.99O19—H19A0.87
C2A—H2D0.99O19—H19B0.82
C3—O41.413 (3)O20—H20A0.88
C3—H3A0.99O20—H20B0.87
C3—H3B0.99O21—H21A0.86
C3—H3C0.99O21—H21B0.87
C3—H3D0.99Co2—C22i1.889 (2)
O4—C51.438 (3)Co2—C221.889 (2)
C5—C61.486 (4)Co2—C23i1.894 (2)
C5—H5A0.99Co2—C231.894 (2)
C5—H5B0.99Co2—C211.894 (2)
C6—O71.446 (3)Co2—C21i1.894 (2)
C6—H6A0.99N21—C211.148 (3)
C6—H6B0.99N22—C221.152 (3)
O7—C81.432 (3)N23—C231.151 (3)
C8—C91.490 (4)Co3—C331.889 (2)
C8—H8A0.99Co3—C33ii1.889 (2)
C8—H8B0.99Co3—C321.894 (2)
C9—O101.450 (3)Co3—C32ii1.894 (2)
C9—H9A0.99Co3—C311.895 (2)
C9—H9B0.99Co3—C31ii1.895 (2)
O10—C111.449 (3)N31—C311.150 (3)
C11—C121.486 (4)N32—C321.150 (3)
C11—H11A0.99N33—C331.153 (3)
C11—H11B0.99O41—H41A0.82
C12—O131.439 (3)O41—H41B0.80
C12—H12A0.99O42—H42A0.84
C12—H12B0.99O42—H42B0.81
O13—C141.443 (3)
O19—Gd1—O21144.40 (6)O10—C11—H11A109.9
O19—Gd1—O20144.12 (6)C12—C11—H11A109.9
O21—Gd1—O2070.48 (5)O10—C11—H11B109.9
O19—Gd1—O1675.42 (5)C12—C11—H11B109.9
O21—Gd1—O1679.20 (5)H11A—C11—H11B108.3
O20—Gd1—O16134.84 (5)O13—C12—C11105.83 (19)
O19—Gd1—O474.85 (6)O13—C12—H12A110.6
O21—Gd1—O4134.90 (6)C11—C12—H12A110.6
O20—Gd1—O479.77 (6)O13—C12—H12B110.6
O16—Gd1—O4100.61 (6)C11—C12—H12B110.6
O19—Gd1—O1091.82 (5)H12A—C12—H12B108.7
O21—Gd1—O1083.42 (5)C12—O13—C14112.82 (17)
O20—Gd1—O1083.16 (5)C12—O13—Gd1115.41 (13)
O16—Gd1—O10126.28 (5)C14—O13—Gd1119.92 (12)
O4—Gd1—O10126.42 (5)O13—C14—C15105.97 (18)
O19—Gd1—O1374.74 (5)O13—C14—H14A110.5
O21—Gd1—O1371.67 (5)C15—C14—H14A110.5
O20—Gd1—O13131.35 (5)O13—C14—H14B110.5
O16—Gd1—O1363.19 (5)C15—C14—H14B110.5
O4—Gd1—O13148.37 (6)H14A—C14—H14B108.7
O10—Gd1—O1363.11 (5)O16—C15—C14106.81 (18)
O19—Gd1—O774.17 (5)O16—C15—H15A110.4
O21—Gd1—O7131.78 (5)C14—C15—H15A110.4
O20—Gd1—O771.91 (5)O16—C15—H15B110.4
O16—Gd1—O7148.47 (5)C14—C15—H15B110.4
O4—Gd1—O763.38 (5)H15A—C15—H15B108.6
O10—Gd1—O763.05 (5)C17—O16—C15115.79 (17)
O13—Gd1—O7115.49 (5)C17—O16—Gd1125.58 (13)
O19—Gd1—O1110.22 (5)C15—O16—Gd1118.62 (12)
O21—Gd1—O178.83 (5)O16—C17—C18A111.0 (4)
O20—Gd1—O178.68 (5)O16—C17—C18107.74 (19)
O16—Gd1—O162.88 (5)O16—C17—H17A110.2
O4—Gd1—O162.32 (5)C18—C17—H17A110.2
O10—Gd1—O1157.96 (5)O16—C17—H17B110.2
O13—Gd1—O1121.95 (5)C18—C17—H17B110.2
O7—Gd1—O1121.47 (5)H17A—C17—H17B108.5
C2A—O1—C18A108.7 (5)O16—C17—H17C109.4
C18—O1—C2111.3 (2)C18A—C17—H17C109.4
C2A—O1—Gd1117.4 (3)O16—C17—H17D109.4
C18—O1—Gd1114.62 (14)C18A—C17—H17D109.4
C18A—O1—Gd1118.2 (4)H17C—C17—H17D108.0
C2—O1—Gd1117.66 (14)O1—C18—C17110.4 (2)
O1—C2—C3109.5 (2)O1—C18—H18A109.6
O1—C2—H2A109.8C17—C18—H18A109.6
C3—C2—H2A109.8O1—C18—H18B109.6
O1—C2—H2B109.8C17—C18—H18B109.6
C3—C2—H2B109.8H18A—C18—H18B108.1
H2A—C2—H2B108.2O1—C18A—C17112.3 (4)
O1—C2A—C3109.6 (4)O1—C18A—H18C109.2
O1—C2A—H2C109.8C17—C18A—H18C109.2
C3—C2A—H2C109.8O1—C18A—H18D109.2
O1—C2A—H2D109.8C17—C18A—H18D109.2
C3—C2A—H2D109.8H18C—C18A—H18D107.9
H2C—C2A—H2D108.2Gd1—O19—H19A119.5
O4—C3—C2107.6 (2)Gd1—O19—H19B131.7
O4—C3—C2A114.1 (3)H19A—O19—H19B105.1
O4—C3—H3A110.2Gd1—O20—H20A120.0
C2—C3—H3A110.2Gd1—O20—H20B134.8
O4—C3—H3B110.2H20A—O20—H20B105.2
C2—C3—H3B110.2Gd1—O21—H21A124.9
H3A—C3—H3B108.5Gd1—O21—H21B132.2
O4—C3—H3C108.7H21A—O21—H21B102.7
C2A—C3—H3C108.7C22i—Co2—C22180.00 (19)
O4—C3—H3D108.7C22i—Co2—C23i88.93 (9)
C2A—C3—H3D108.7C22—Co2—C23i91.07 (9)
H3C—C3—H3D107.6C22i—Co2—C2391.07 (9)
C3—O4—C5116.14 (18)C22—Co2—C2388.93 (9)
C3—O4—Gd1123.01 (14)C23i—Co2—C23180.00 (15)
C5—O4—Gd1118.33 (13)C22i—Co2—C2191.47 (9)
O4—C5—C6108.12 (19)C22—Co2—C2188.53 (9)
O4—C5—H5A110.1C23i—Co2—C2191.72 (10)
C6—C5—H5A110.1C23—Co2—C2188.28 (10)
O4—C5—H5B110.1C22i—Co2—C21i88.53 (9)
C6—C5—H5B110.1C22—Co2—C21i91.47 (9)
H5A—C5—H5B108.4C23i—Co2—C21i88.28 (10)
O7—C6—C5106.04 (19)C23—Co2—C21i91.72 (10)
O7—C6—H6A110.5C21—Co2—C21i180.00 (12)
C5—C6—H6A110.5N21—C21—Co2177.4 (2)
O7—C6—H6B110.5N22—C22—Co2178.45 (19)
C5—C6—H6B110.5N23—C23—Co2177.4 (2)
H6A—C6—H6B108.7C33—Co3—C33ii180.0
C8—O7—C6112.16 (18)C33—Co3—C3290.05 (9)
C8—O7—Gd1115.27 (13)C33ii—Co3—C3289.95 (9)
C6—O7—Gd1119.24 (13)C33—Co3—C32ii89.95 (9)
O7—C8—C9106.1 (2)C33ii—Co3—C32ii90.05 (9)
O7—C8—H8A110.5C32—Co3—C32ii180.00 (14)
C9—C8—H8A110.5C33—Co3—C3191.50 (9)
O7—C8—H8B110.5C33ii—Co3—C3188.50 (9)
C9—C8—H8B110.5C32—Co3—C3189.97 (9)
H8A—C8—H8B108.7C32ii—Co3—C3190.03 (9)
O10—C9—C8108.49 (19)C33—Co3—C31ii88.50 (9)
O10—C9—H9A110.0C33ii—Co3—C31ii91.50 (9)
C8—C9—H9A110.0C32—Co3—C31ii90.03 (9)
O10—C9—H9B110.0C32ii—Co3—C31ii89.97 (9)
C8—C9—H9B110.0C31—Co3—C31ii180.0
H9A—C9—H9B108.4N31—C31—Co3179.1 (2)
C11—O10—C9107.47 (18)N32—C32—Co3178.9 (2)
C11—O10—Gd1121.04 (13)N33—C33—Co3176.7 (2)
C9—O10—Gd1121.22 (13)H41A—O41—H41B105.4
O10—C11—C12108.82 (19)H42A—O42—H42B100.2
O19—Gd1—O1—C2A91.0 (4)O10—Gd1—O7—C6167.04 (17)
O21—Gd1—O1—C2A124.9 (4)O13—Gd1—O7—C6156.53 (15)
O20—Gd1—O1—C2A52.8 (4)O1—Gd1—O7—C611.81 (17)
O16—Gd1—O1—C2A151.6 (4)C6—O7—C8—C9164.81 (19)
O4—Gd1—O1—C2A31.5 (4)Gd1—O7—C8—C954.3 (2)
O10—Gd1—O1—C2A87.9 (4)O7—C8—C9—O1051.8 (3)
O13—Gd1—O1—C2A175.2 (4)C8—C9—O10—C11174.4 (2)
O7—Gd1—O1—C2A7.6 (4)C8—C9—O10—Gd129.0 (3)
O19—Gd1—O1—C1887.30 (17)O19—Gd1—O10—C1170.95 (18)
O21—Gd1—O1—C1856.84 (17)O21—Gd1—O10—C1173.66 (17)
O20—Gd1—O1—C18128.91 (17)O20—Gd1—O10—C11144.70 (18)
O16—Gd1—O1—C1826.65 (16)O16—Gd1—O10—C112.24 (19)
O4—Gd1—O1—C18146.80 (18)O4—Gd1—O10—C11143.41 (17)
O10—Gd1—O1—C1893.8 (2)O13—Gd1—O10—C110.91 (16)
O13—Gd1—O1—C183.09 (18)O7—Gd1—O10—C11142.15 (19)
O7—Gd1—O1—C18170.68 (16)O1—Gd1—O10—C11110.1 (2)
O19—Gd1—O1—C18A42.5 (5)O19—Gd1—O10—C969.81 (17)
O21—Gd1—O1—C18A101.6 (5)O21—Gd1—O10—C9145.58 (17)
O20—Gd1—O1—C18A173.7 (5)O20—Gd1—O10—C974.54 (17)
O16—Gd1—O1—C18A18.2 (5)O16—Gd1—O10—C9143.00 (16)
O4—Gd1—O1—C18A102.0 (5)O4—Gd1—O10—C92.64 (19)
O10—Gd1—O1—C18A138.6 (5)O13—Gd1—O10—C9141.67 (18)
O13—Gd1—O1—C18A41.7 (5)O7—Gd1—O10—C91.39 (16)
O7—Gd1—O1—C18A125.9 (5)O1—Gd1—O10—C9109.1 (2)
O19—Gd1—O1—C246.41 (18)C9—O10—C11—C12174.1 (2)
O21—Gd1—O1—C2169.45 (18)Gd1—O10—C11—C1228.7 (3)
O20—Gd1—O1—C297.38 (17)O10—C11—C12—O1351.5 (3)
O16—Gd1—O1—C2107.06 (18)C11—C12—O13—C14162.51 (19)
O4—Gd1—O1—C213.09 (17)C11—C12—O13—Gd154.5 (2)
O10—Gd1—O1—C2132.48 (18)O19—Gd1—O13—C12129.52 (15)
O13—Gd1—O1—C2130.62 (17)O21—Gd1—O13—C1262.45 (15)
O7—Gd1—O1—C236.97 (18)O20—Gd1—O13—C1221.96 (17)
C2A—O1—C2—C362.0 (5)O16—Gd1—O13—C12149.37 (16)
C18—O1—C2—C3173.5 (2)O4—Gd1—O13—C12145.91 (15)
C18A—O1—C2—C3153.3 (5)O10—Gd1—O13—C1229.43 (14)
Gd1—O1—C2—C338.4 (3)O7—Gd1—O13—C1265.84 (15)
C18—O1—C2A—C3136.0 (4)O1—Gd1—O13—C12125.88 (14)
C18A—O1—C2A—C395.5 (8)O19—Gd1—O13—C1490.24 (15)
C2—O1—C2A—C359.1 (4)O21—Gd1—O13—C1477.79 (15)
Gd1—O1—C2A—C342.0 (8)O20—Gd1—O13—C14118.29 (15)
O1—C2—C3—O448.5 (3)O16—Gd1—O13—C149.13 (14)
O1—C2—C3—C2A58.4 (4)O4—Gd1—O13—C1473.85 (18)
O1—C2A—C3—O426.1 (8)O10—Gd1—O13—C14169.67 (16)
O1—C2A—C3—C261.8 (5)O7—Gd1—O13—C14153.92 (14)
C2—C3—O4—C5157.0 (2)O1—Gd1—O13—C1414.36 (16)
C2A—C3—O4—C5163.0 (5)C12—O13—C14—C15177.99 (18)
C2—C3—O4—Gd141.3 (3)Gd1—O13—C14—C1536.8 (2)
C2A—C3—O4—Gd11.3 (5)O13—C14—C15—O1653.0 (2)
O19—Gd1—O4—C3139.28 (19)C14—C15—O16—C17128.5 (2)
O21—Gd1—O4—C317.6 (2)C14—C15—O16—Gd150.9 (2)
O20—Gd1—O4—C366.33 (18)O19—Gd1—O16—C17123.76 (18)
O16—Gd1—O4—C367.71 (19)O21—Gd1—O16—C1781.42 (18)
O10—Gd1—O4—C3139.86 (17)O20—Gd1—O16—C1733.4 (2)
O13—Gd1—O4—C3122.90 (18)O4—Gd1—O16—C1752.64 (18)
O7—Gd1—O4—C3141.1 (2)O10—Gd1—O16—C17154.88 (17)
O1—Gd1—O4—C316.17 (17)O13—Gd1—O16—C17156.21 (19)
O19—Gd1—O4—C559.44 (17)O7—Gd1—O16—C17108.14 (19)
O21—Gd1—O4—C5143.72 (16)O1—Gd1—O16—C171.46 (17)
O20—Gd1—O4—C594.95 (18)O19—Gd1—O16—C1556.87 (15)
O16—Gd1—O4—C5131.01 (17)O21—Gd1—O16—C1597.94 (15)
O10—Gd1—O4—C521.4 (2)O20—Gd1—O16—C15145.92 (14)
O13—Gd1—O4—C575.8 (2)O4—Gd1—O16—C15128.00 (15)
O7—Gd1—O4—C520.17 (16)O10—Gd1—O16—C1524.48 (17)
O1—Gd1—O4—C5177.45 (19)O13—Gd1—O16—C1523.15 (14)
C3—O4—C5—C6114.3 (2)O7—Gd1—O16—C1572.50 (18)
Gd1—O4—C5—C648.3 (2)O1—Gd1—O16—C15179.18 (16)
O4—C5—C6—O753.6 (2)C15—O16—C17—C18A161.4 (5)
C5—C6—O7—C8178.14 (19)Gd1—O16—C17—C18A19.2 (5)
C5—C6—O7—Gd139.0 (2)C15—O16—C17—C18158.2 (2)
O19—Gd1—O7—C8129.55 (15)Gd1—O16—C17—C1821.2 (3)
O21—Gd1—O7—C822.10 (17)C2A—O1—C18—C17130.0 (5)
O20—Gd1—O7—C862.35 (15)C18A—O1—C18—C1757.1 (5)
O16—Gd1—O7—C8145.26 (14)C2—O1—C18—C1788.5 (3)
O4—Gd1—O7—C8149.76 (16)Gd1—O1—C18—C1748.1 (3)
O10—Gd1—O7—C829.11 (14)O16—C17—C18—O143.6 (3)
O13—Gd1—O7—C865.54 (16)C18A—C17—C18—O158.0 (5)
O1—Gd1—O7—C8126.12 (14)C2A—O1—C18A—C17172.0 (6)
O19—Gd1—O7—C692.52 (15)C18—O1—C18A—C1760.8 (5)
O21—Gd1—O7—C6115.83 (15)C2—O1—C18A—C17149.2 (9)
O20—Gd1—O7—C675.58 (15)Gd1—O1—C18A—C1734.9 (10)
O16—Gd1—O7—C676.81 (18)O16—C17—C18A—O133.6 (9)
O4—Gd1—O7—C611.83 (15)C18—C17—C18A—O158.7 (5)
Symmetry codes: (i) x, y+1, z; (ii) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O19—H19A···N210.871.852.717 (3)170
O19—H19B···O420.821.782.594 (2)169
O20—H20A···O410.881.832.680 (2)163
O20—H20B···N330.871.892.748 (3)168
O21—H21A···O410.861.882.687 (2)155
O21—H21B···N32iii0.871.872.730 (3)172
O41—H41A···N22iv0.821.892.708 (2)172
O41—H41B···N33v0.802.383.072 (3)145
O42—H42A···N31vi0.842.002.830 (3)174
O42—H42B···N23vii0.812.032.813 (3)164
Symmetry codes: (iii) x, y+1, z+1; (iv) x, y, z+1; (v) x+1, y+1, z+1; (vi) x, y+1, z1; (vii) x+1, y+1, z.

Experimental details

(I)(II)(III)(IV)
Crystal data
Chemical formula[Ce(C12H24O6)(H2O)4][Fe(CN)6]·2H2O[Nd(C12H24O6)(H2O)4][Fe(CN)6]·2H2O[Sm(C12H24O6)(H2O)3][Fe(CN)6]·2H2O[Eu(C12H24O6)(H2O)3][Fe(CN)6]·2H2O
Mr724.50728.62716.71718.32
Crystal system, space groupMonoclinic, C2/cMonoclinic, C2/cTriclinic, P1Triclinic, P1
Temperature (K)120120120120
a, b, c (Å)19.8534 (6), 11.5705 (2), 14.0258 (4)19.9552 (6), 11.5063 (2), 13.9706 (3)10.9324 (2), 11.0996 (2), 14.0119 (4)10.9125 (3), 11.0947 (4), 14.0119 (3)
α, β, γ (°)90, 113.3930 (13), 9090, 113.4189 (11), 9067.9012 (13), 70.7291 (13), 65.7231 (14)67.8201 (18), 70.635 (2), 65.743 (2)
V3)2957.09 (13)2943.55 (12)1404.77 (6)1400.57 (8)
Z4422
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)2.072.302.652.80
Crystal size (mm)0.20 × 0.10 × 0.100.34 × 0.34 × 0.250.10 × 0.06 × 0.040.25 × 0.20 × 0.20
Data collection
DiffractometerBruker–Nonius KappaCCD
diffractometer
Bruker–Nonius KappaCCD
diffractometer
Bruker–Nonius KappaCCD
diffractometer
Bruker–Nonius KappaCCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2003)
Multi-scan
(SADABS; Sheldrick, 2003)
Multi-scan
(SADABS; Sheldrick, 2003)
Multi-scan
(SADABS; Sheldrick, 2003)
Tmin, Tmax0.682, 0.8200.478, 0.5610.836, 0.9000.509, 0.568
No. of measured, independent and
observed [I > 2σ(I)] reflections
15557, 3385, 3079 21701, 3360, 3168 28348, 6453, 5624 27604, 6420, 5973
Rint0.0360.0310.0500.060
(sin θ/λ)max1)0.6500.6500.6500.652
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.023, 0.049, 1.09 0.018, 0.043, 1.06 0.030, 0.067, 1.01 0.077, 0.212, 1.10
No. of reflections3385336064536420
No. of parameters176176334334
No. of restraints0088
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0144P)2 + 2.9468P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0166P)2 + 4.6543P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0254P)2 + 2.0082P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.1382P)2 + 13.515P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.81, 0.870.83, 1.070.95, 0.9111.43, 3.03


(V)(VII)
Crystal data
Chemical formula[Gd(C12H24O6)(H2O)3][Cr(CN)6]·2H2O[Gd(C12H24O6)(H2O)3][Co(CN)6]·2H2O
Mr719.76726.69
Crystal system, space groupTriclinic, P1Triclinic, P1
Temperature (K)120120
a, b, c (Å)11.0563 (2), 11.1562 (2), 14.2127 (3)10.8604 (2), 11.0724 (3), 13.9909 (2)
α, β, γ (°)68.3494 (11), 70.0959 (12), 66.0299 (12)67.5857 (10), 70.5870 (8), 65.5666 (9)
V3)1450.92 (5)1385.20 (5)
Z22
Radiation typeMo KαMo Kα
µ (mm1)2.703.03
Crystal size (mm)0.16 × 0.15 × 0.040.60 × 0.54 × 0.42
Data collection
DiffractometerBruker–Nonius KappaCCD
diffractometer
Bruker–Nonius KappaCCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2003)
Multi-scan
(SADABS; Sheldrick, 2003)
Tmin, Tmax0.672, 0.8990.187, 0.280
No. of measured, independent and
observed [I > 2σ(I)] reflections
34884, 6646, 6382 27907, 6348, 6022
Rint0.0380.033
(sin θ/λ)max1)0.6500.651
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.040, 0.108, 1.04 0.020, 0.047, 1.09
No. of reflections66466348
No. of parameters334334
No. of restraints88
H-atom treatmentH-atom parameters constrainedH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0507P)2 + 9.2124P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0144P)2 + 1.6153P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)3.60, 1.631.00, 0.91

Computer programs: COLLECT (Hooft, 1999), DENZO (Otwinowski & Minor, 1997) and COLLECT, DENZO and COLLECT, OSCAIL (McArdle, 2003) and SHELXS97 (Sheldrick, 1997), OSCAIL and SHELXL97 (Sheldrick, 1997), PLATON (Spek, 2003), SHELXL97 and PRPKAPPA (Ferguson, 1999).

Hydrogen-bond geometry (Å, º) for (I) top
D—H···AD—HH···AD···AD—H···A
O19—H19A···O21i0.811.912.700 (2)163
O19—H19B···N110.812.142.917 (2)161
O20—H20A···O21ii0.821.962.768 (2)168
O20—H20B···N12iii0.821.922.739 (2)171
O21—H21A···N13ii0.821.942.757 (2)173
O21—H21B···N110.822.072.888 (2)175
Symmetry codes: (i) x, y+1, z; (ii) x, y+1, z+1/2; (iii) x, y, z+1/2.
Hydrogen-bond geometry (Å, º) for (II) top
D—H···AD—HH···AD···AD—H···A
O19—H19A···O21i0.811.922.697 (2)161
O19—H19B···N110.842.092.904 (2)161
O20—H20A···O21ii0.831.962.773 (2)166
O20—H20B···N12iii0.841.902.734 (2)169
O21—H21A···N13ii0.831.932.753 (2)173
O21—H21B···N110.802.102.893 (2)175
Symmetry codes: (i) x, y+1, z; (ii) x, y+1, z+1/2; (iii) x, y, z+1/2.
Ln—O distances (Å) in (I) and (II) top
Distance(I)(II)
Ln1—O12.5784 (13)2.5515 (12)
Ln1—O42.6811 (14)2.6620 (13)
Ln1—O72.5619 (13)2.5312 (12)
Ln1—O192.5389 (14)2.5062 (12)
Ln1—O202.4962 (14)2.4615 (12)
Ln—O distances (Å) in (III)–(VII) top
Distance(III)(IV)(V)(VI)(VII)
Ln1—O12.602 (2)2.590 (5)2.581 (3)2.5790 (17)2.5769 (14)
Ln1—O42.505 (2)2.502 (6)2.489 (4)2.4882 (19)2.4863 (16)
Ln1—O72.563 (2)2.553 (5)2.548 (3)2.5476 (17)2.5437 (15)
Ln1—O102.529 (2)2.511 (5)2.504 (3)2.5007 (17)2.4989 (15)
Ln1—O132.552 (2)2.550 (5)2.543 (3)2.5361 (17)2.5347 (15)
Ln1—O162.481 (2)2.467 (6)2.476 (3)2.4608 (17)2.4573 (15)
Ln1—O192.327 (2)2.318 (6)2.307 (3)2.3088 (17)2.3042 (15)
Ln1—O202.409 (2)2.405 (5)2.381 (3)2.3884 (17)2.3887 (15)
Ln1—O212.408 (2)2.392 (5)2.377 (3)2.3881 (17)2.3883 (15)
Data for compound (VI) are taken from Koner et al. (2005).
 

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