Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270107040449/gg3119sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270107040449/gg3119Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270107040449/gg3119IIsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270107040449/gg3119IIIsup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270107040449/gg3119IVsup5.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270107040449/gg3119Vsup6.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270107040449/gg3119VIIsup7.hkl |
CCDC references: 602734; 602735; 602736; 602737; 602738; 602739; 602740
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.
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.
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).
[Ce(C12H24O6)(H2O)4][Fe(CN)6]·2H2O | F(000) = 1464 |
Mr = 724.50 | Dx = 1.627 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 3385 reflections |
a = 19.8534 (6) Å | θ = 3.4–27.5° |
b = 11.5705 (2) Å | µ = 2.07 mm−1 |
c = 14.0258 (4) Å | T = 120 K |
β = 113.3930 (13)° | Block, yellow |
V = 2957.09 (13) Å3 | 0.20 × 0.10 × 0.10 mm |
Z = 4 |
Bruker–Nonius KappaCCD diffractometer | 3385 independent reflections |
Radiation source: Bruker-Nonius FR591 rotating anode | 3079 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.036 |
Detector resolution: 9.091 pixels mm-1 | θmax = 27.5°, θmin = 3.4° |
ϕ & ω scans | h = −25→25 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | k = −14→15 |
Tmin = 0.682, Tmax = 0.820 | l = −18→18 |
15557 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.023 | H-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 reflections | Δρmax = 0.81 e Å−3 |
176 parameters | Δρmin = −0.87 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00166 (8) |
[Ce(C12H24O6)(H2O)4][Fe(CN)6]·2H2O | V = 2957.09 (13) Å3 |
Mr = 724.50 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 19.8534 (6) Å | µ = 2.07 mm−1 |
b = 11.5705 (2) Å | T = 120 K |
c = 14.0258 (4) Å | 0.20 × 0.10 × 0.10 mm |
β = 113.3930 (13)° |
Bruker–Nonius KappaCCD diffractometer | 3385 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | 3079 reflections with I > 2σ(I) |
Tmin = 0.682, Tmax = 0.820 | Rint = 0.036 |
15557 measured reflections |
R[F2 > 2σ(F2)] = 0.023 | 0 restraints |
wR(F2) = 0.049 | H-atom parameters constrained |
S = 1.09 | Δρmax = 0.81 e Å−3 |
3385 reflections | Δρmin = −0.87 e Å−3 |
176 parameters |
x | y | z | Uiso*/Ueq | ||
Ce1 | 0.0000 | 0.234944 (13) | 0.2500 | 0.01137 (7) | |
O1 | 0.07320 (7) | 0.42168 (11) | 0.32310 (10) | 0.0161 (3) | |
C2 | 0.14240 (11) | 0.44021 (17) | 0.31446 (16) | 0.0179 (4) | |
C3 | 0.18455 (11) | 0.32906 (17) | 0.33975 (17) | 0.0224 (5) | |
O4 | 0.14017 (8) | 0.24169 (11) | 0.27090 (11) | 0.0175 (3) | |
C5 | 0.17858 (12) | 0.13413 (18) | 0.28102 (19) | 0.0253 (5) | |
C6 | 0.12504 (12) | 0.04820 (18) | 0.21163 (19) | 0.0254 (5) | |
O7 | 0.06382 (7) | 0.04500 (11) | 0.24187 (11) | 0.0174 (3) | |
C8 | 0.02244 (12) | −0.06091 (18) | 0.21778 (19) | 0.0269 (5) | |
C18 | 0.02867 (12) | 0.52538 (16) | 0.30468 (16) | 0.0197 (5) | |
O19 | 0.02820 (7) | 0.31805 (13) | 0.10237 (10) | 0.0221 (3) | |
O20 | 0.08468 (8) | 0.17105 (12) | 0.42718 (11) | 0.0229 (3) | |
Fe1 | 0.2500 | 0.2500 | 0.0000 | 0.00981 (9) | |
N11 | 0.14808 (10) | 0.41328 (15) | 0.05656 (14) | 0.0220 (4) | |
C11 | 0.18455 (11) | 0.35034 (16) | 0.03461 (15) | 0.0146 (4) | |
N12 | 0.16334 (10) | 0.02792 (15) | −0.00100 (14) | 0.0222 (4) | |
C12 | 0.19468 (11) | 0.11178 (17) | 0.00123 (15) | 0.0147 (4) | |
N13 | 0.15844 (10) | 0.27245 (14) | −0.23566 (13) | 0.0192 (4) | |
C13 | 0.19222 (11) | 0.26503 (15) | −0.14782 (16) | 0.0135 (4) | |
O21 | 0.09957 (8) | 0.64744 (12) | 0.06265 (10) | 0.0232 (3) | |
H2A | 0.1705 | 0.5015 | 0.3633 | 0.022* | |
H2B | 0.1339 | 0.4650 | 0.2430 | 0.022* | |
H3A | 0.2313 | 0.3380 | 0.3307 | 0.027* | |
H3B | 0.1961 | 0.3071 | 0.4128 | 0.027* | |
H5A | 0.1978 | 0.1072 | 0.3540 | 0.030* | |
H5B | 0.2204 | 0.1439 | 0.2602 | 0.030* | |
H6A | 0.1086 | 0.0720 | 0.1380 | 0.030* | |
H6B | 0.1481 | −0.0291 | 0.2199 | 0.030* | |
H8A | 0.0558 | −0.1284 | 0.2353 | 0.032* | |
H8B | −0.0098 | −0.0642 | 0.1429 | 0.032* | |
H18A | 0.0603 | 0.5945 | 0.3158 | 0.024* | |
H18B | 0.0046 | 0.5286 | 0.3544 | 0.024* | |
H19A | −0.0049 | 0.3304 | 0.0462 | 0.046* | |
H19B | 0.0677 | 0.3340 | 0.1011 | 0.046* | |
H20A | 0.0949 | 0.2198 | 0.4730 | 0.046* | |
H20B | 0.1100 | 0.1146 | 0.4552 | 0.046* | |
H21A | 0.1157 | 0.6666 | 0.1242 | 0.046* | |
H21B | 0.1138 | 0.5823 | 0.0580 | 0.046* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ce1 | 0.01244 (10) | 0.01085 (10) | 0.01076 (10) | 0.000 | 0.00456 (7) | 0.000 |
O1 | 0.0137 (7) | 0.0141 (7) | 0.0188 (8) | −0.0003 (6) | 0.0047 (6) | −0.0003 (5) |
C2 | 0.0154 (11) | 0.0160 (10) | 0.0222 (12) | −0.0064 (8) | 0.0073 (9) | −0.0014 (8) |
C3 | 0.0155 (11) | 0.0228 (12) | 0.0260 (12) | −0.0046 (9) | 0.0050 (10) | −0.0006 (9) |
O4 | 0.0146 (7) | 0.0150 (7) | 0.0230 (8) | 0.0003 (6) | 0.0076 (6) | 0.0003 (5) |
C5 | 0.0206 (12) | 0.0197 (11) | 0.0421 (15) | 0.0069 (9) | 0.0193 (11) | 0.0071 (10) |
C6 | 0.0296 (13) | 0.0191 (11) | 0.0386 (14) | 0.0032 (10) | 0.0254 (11) | −0.0014 (10) |
O7 | 0.0185 (8) | 0.0127 (7) | 0.0242 (8) | 0.0000 (6) | 0.0119 (7) | −0.0022 (6) |
C8 | 0.0212 (12) | 0.0113 (10) | 0.0460 (15) | 0.0011 (9) | 0.0110 (11) | −0.0079 (9) |
C18 | 0.0204 (11) | 0.0123 (10) | 0.0253 (12) | 0.0003 (9) | 0.0079 (9) | −0.0029 (8) |
O19 | 0.0150 (8) | 0.0337 (9) | 0.0155 (8) | −0.0047 (7) | 0.0038 (6) | 0.0040 (6) |
O20 | 0.0315 (9) | 0.0178 (8) | 0.0150 (8) | 0.0099 (7) | 0.0046 (7) | 0.0004 (6) |
Fe1 | 0.0104 (2) | 0.0101 (2) | 0.0091 (2) | −0.00070 (14) | 0.00391 (16) | −0.00008 (13) |
N11 | 0.0239 (10) | 0.0220 (10) | 0.0216 (10) | 0.0036 (8) | 0.0105 (8) | 0.0014 (7) |
C11 | 0.0169 (11) | 0.0129 (10) | 0.0125 (10) | −0.0019 (8) | 0.0042 (9) | 0.0030 (7) |
N12 | 0.0289 (11) | 0.0193 (10) | 0.0201 (10) | −0.0089 (8) | 0.0115 (8) | −0.0037 (7) |
C12 | 0.0164 (10) | 0.0160 (10) | 0.0115 (10) | 0.0016 (9) | 0.0054 (8) | −0.0008 (8) |
N13 | 0.0222 (10) | 0.0176 (9) | 0.0151 (10) | −0.0036 (8) | 0.0045 (8) | 0.0009 (7) |
C13 | 0.0155 (10) | 0.0097 (9) | 0.0173 (11) | −0.0017 (8) | 0.0087 (9) | 0.0005 (7) |
O21 | 0.0330 (9) | 0.0183 (8) | 0.0126 (8) | 0.0039 (7) | 0.0030 (7) | −0.0009 (6) |
Ce1—O20i | 2.4962 (14) | C6—H6B | 0.99 |
Ce1—O20 | 2.4962 (14) | O7—C8 | 1.439 (2) |
Ce1—O19i | 2.5389 (14) | C8—C8i | 1.500 (5) |
Ce1—O19 | 2.5389 (14) | C8—H8A | 0.99 |
Ce1—O7i | 2.5619 (13) | C8—H8B | 0.99 |
Ce1—O7 | 2.5619 (13) | C18—C18i | 1.504 (4) |
Ce1—O1 | 2.5784 (13) | C18—H18A | 0.99 |
Ce1—O1i | 2.5784 (13) | C18—H18B | 0.99 |
Ce1—O4i | 2.6811 (14) | O19—H19A | 0.81 |
Ce1—O4 | 2.6811 (14) | O19—H19B | 0.81 |
O1—C2 | 1.442 (2) | O20—H20A | 0.82 |
O1—C18 | 1.451 (2) | O20—H20B | 0.82 |
C2—C3 | 1.498 (3) | Fe1—C13ii | 1.938 (2) |
C2—H2A | 0.99 | Fe1—C13 | 1.938 (2) |
C2—H2B | 0.99 | Fe1—C11ii | 1.942 (2) |
C3—O4 | 1.434 (2) | Fe1—C11 | 1.942 (2) |
C3—H3A | 0.99 | Fe1—C12ii | 1.944 (2) |
C3—H3B | 0.99 | Fe1—C12 | 1.944 (2) |
O4—C5 | 1.437 (2) | N11—C11 | 1.152 (3) |
C5—C6 | 1.498 (3) | N12—C12 | 1.146 (2) |
C5—H5A | 0.99 | N13—C13 | 1.148 (3) |
C5—H5B | 0.99 | O21—H21A | 0.82 |
C6—O7 | 1.438 (2) | O21—H21B | 0.82 |
C6—H6A | 0.99 | ||
O20i—Ce1—O20 | 145.54 (6) | C2—C3—H3B | 110.1 |
O20i—Ce1—O19i | 130.14 (5) | H3A—C3—H3B | 108.4 |
O20—Ce1—O19i | 65.14 (4) | C3—O4—C5 | 112.58 (16) |
O20i—Ce1—O19 | 65.14 (4) | C3—O4—Ce1 | 115.33 (11) |
O20—Ce1—O19 | 130.14 (5) | C5—O4—Ce1 | 118.21 (11) |
O19i—Ce1—O19 | 135.49 (7) | O4—C5—C6 | 107.39 (17) |
O20i—Ce1—O7i | 68.95 (4) | O4—C5—H5A | 110.2 |
O20—Ce1—O7i | 81.44 (5) | C6—C5—H5A | 110.2 |
O19i—Ce1—O7i | 90.89 (5) | O4—C5—H5B | 110.2 |
O19—Ce1—O7i | 129.37 (5) | C6—C5—H5B | 110.2 |
O20i—Ce1—O7 | 81.44 (5) | H5A—C5—H5B | 108.5 |
O20—Ce1—O7 | 68.95 (4) | O7—C6—C5 | 106.88 (17) |
O19i—Ce1—O7 | 129.37 (5) | O7—C6—H6A | 110.3 |
O19—Ce1—O7 | 90.89 (5) | C5—C6—H6A | 110.3 |
O7i—Ce1—O7 | 61.85 (6) | O7—C6—H6B | 110.3 |
O20i—Ce1—O1 | 133.99 (4) | C5—C6—H6B | 110.3 |
O20—Ce1—O1 | 78.57 (4) | H6A—C6—H6B | 108.6 |
O19i—Ce1—O1 | 68.30 (5) | C6—O7—C8 | 115.05 (15) |
O19—Ce1—O1 | 74.63 (4) | C6—O7—Ce1 | 118.81 (11) |
O7i—Ce1—O1 | 155.75 (4) | C8—O7—Ce1 | 119.65 (11) |
O7—Ce1—O1 | 121.73 (4) | O7—C8—C8i | 106.20 (15) |
O20i—Ce1—O1i | 78.57 (4) | O7—C8—H8A | 110.5 |
O20—Ce1—O1i | 133.99 (4) | C8i—C8—H8A | 110.5 |
O19i—Ce1—O1i | 74.63 (4) | O7—C8—H8B | 110.5 |
O19—Ce1—O1i | 68.30 (5) | C8i—C8—H8B | 110.5 |
O7i—Ce1—O1i | 121.73 (4) | H8A—C8—H8B | 108.7 |
O7—Ce1—O1i | 155.75 (4) | O1—C18—C18i | 110.03 (14) |
O1—Ce1—O1i | 66.15 (6) | O1—C18—H18A | 109.7 |
O20i—Ce1—O4i | 68.92 (5) | C18i—C18—H18A | 109.7 |
O20—Ce1—O4i | 112.15 (5) | O1—C18—H18B | 109.7 |
O19i—Ce1—O4i | 61.50 (4) | C18i—C18—H18B | 109.7 |
O19—Ce1—O4i | 117.08 (4) | H18A—C18—H18B | 108.2 |
O7i—Ce1—O4i | 61.29 (4) | Ce1—O19—H19A | 120.1 |
O7—Ce1—O4i | 122.03 (4) | Ce1—O19—H19B | 129.1 |
O1—Ce1—O4i | 114.57 (4) | H19A—O19—H19B | 110.8 |
O1i—Ce1—O4i | 62.32 (4) | Ce1—O20—H20A | 115.9 |
O20i—Ce1—O4 | 112.15 (5) | Ce1—O20—H20B | 138.9 |
O20—Ce1—O4 | 68.92 (5) | H20A—O20—H20B | 105.0 |
O19i—Ce1—O4 | 117.08 (4) | C13ii—Fe1—C13 | 180.00 (10) |
O19—Ce1—O4 | 61.50 (4) | C13ii—Fe1—C11ii | 92.48 (8) |
O7i—Ce1—O4 | 122.03 (4) | C13—Fe1—C11ii | 87.52 (8) |
O7—Ce1—O4 | 61.29 (4) | C13ii—Fe1—C11 | 87.52 (8) |
O1—Ce1—O4 | 62.32 (4) | C13—Fe1—C11 | 92.48 (8) |
O1i—Ce1—O4 | 114.57 (4) | C11ii—Fe1—C11 | 180.00 (11) |
O4i—Ce1—O4 | 176.66 (5) | C13ii—Fe1—C12ii | 89.24 (8) |
C2—O1—C18 | 113.28 (15) | C13—Fe1—C12ii | 90.76 (8) |
C2—O1—Ce1 | 119.76 (11) | C11ii—Fe1—C12ii | 93.04 (8) |
C18—O1—Ce1 | 114.50 (11) | C11—Fe1—C12ii | 86.96 (8) |
O1—C2—C3 | 108.28 (16) | C13ii—Fe1—C12 | 90.76 (8) |
O1—C2—H2A | 110.0 | C13—Fe1—C12 | 89.24 (8) |
C3—C2—H2A | 110.0 | C11ii—Fe1—C12 | 86.96 (8) |
O1—C2—H2B | 110.0 | C11—Fe1—C12 | 93.04 (8) |
C3—C2—H2B | 110.0 | C12ii—Fe1—C12 | 180.00 (12) |
H2A—C2—H2B | 108.4 | N11—C11—Fe1 | 177.10 (18) |
O4—C3—C2 | 108.04 (16) | N12—C12—Fe1 | 176.85 (18) |
O4—C3—H3A | 110.1 | N13—C13—Fe1 | 178.99 (19) |
C2—C3—H3A | 110.1 | H21A—O21—H21B | 109.3 |
O4—C3—H3B | 110.1 | ||
O20i—Ce1—O1—C2 | −81.07 (14) | O19i—Ce1—O4—C5 | 113.47 (14) |
O20—Ce1—O1—C2 | 85.86 (13) | O19—Ce1—O4—C5 | −117.20 (15) |
O19i—Ce1—O1—C2 | 153.46 (13) | O7i—Ce1—O4—C5 | 3.57 (15) |
O19—Ce1—O1—C2 | −51.68 (13) | O7—Ce1—O4—C5 | −8.69 (13) |
O7i—Ce1—O1—C2 | 120.90 (14) | O1—Ce1—O4—C5 | 155.99 (15) |
O7—Ce1—O1—C2 | 29.64 (14) | O1i—Ce1—O4—C5 | −161.90 (13) |
O1i—Ce1—O1—C2 | −124.35 (15) | C3—O4—C5—C6 | 175.74 (17) |
O4i—Ce1—O1—C2 | −164.84 (12) | Ce1—O4—C5—C6 | 37.2 (2) |
O4—Ce1—O1—C2 | 13.82 (12) | O4—C5—C6—O7 | −55.8 (2) |
O20i—Ce1—O1—C18 | 58.48 (14) | C5—C6—O7—C8 | −155.13 (18) |
O20—Ce1—O1—C18 | −134.59 (13) | C5—C6—O7—Ce1 | 53.2 (2) |
O19i—Ce1—O1—C18 | −66.99 (12) | O20i—Ce1—O7—C6 | 96.62 (14) |
O19—Ce1—O1—C18 | 87.88 (13) | O20—Ce1—O7—C6 | −101.31 (14) |
O7i—Ce1—O1—C18 | −99.55 (15) | O19i—Ce1—O7—C6 | −127.35 (14) |
O7—Ce1—O1—C18 | 169.19 (12) | O19—Ce1—O7—C6 | 31.92 (14) |
O1i—Ce1—O1—C18 | 15.20 (10) | O7i—Ce1—O7—C6 | 167.26 (17) |
O4i—Ce1—O1—C18 | −25.29 (13) | O1—Ce1—O7—C6 | −40.50 (15) |
O4—Ce1—O1—C18 | 153.37 (14) | O1i—Ce1—O7—C6 | 61.93 (18) |
C18—O1—C2—C3 | 177.45 (16) | O4i—Ce1—O7—C6 | 155.06 (13) |
Ce1—O1—C2—C3 | −42.55 (19) | O4—Ce1—O7—C6 | −24.53 (13) |
O1—C2—C3—O4 | 56.6 (2) | O20i—Ce1—O7—C8 | −53.73 (15) |
C2—C3—O4—C5 | 173.73 (17) | O20—Ce1—O7—C8 | 108.34 (15) |
C2—C3—O4—Ce1 | −46.52 (19) | O19i—Ce1—O7—C8 | 82.30 (15) |
O20i—Ce1—O4—C3 | 147.88 (12) | O19—Ce1—O7—C8 | −118.43 (15) |
O20—Ce1—O4—C3 | −69.25 (13) | O7i—Ce1—O7—C8 | 16.91 (12) |
O19i—Ce1—O4—C3 | −23.93 (14) | O1—Ce1—O7—C8 | 169.16 (14) |
O19—Ce1—O4—C3 | 105.40 (13) | O1i—Ce1—O7—C8 | −88.42 (17) |
O7i—Ce1—O4—C3 | −133.82 (12) | O4i—Ce1—O7—C8 | 4.71 (16) |
O7—Ce1—O4—C3 | −146.08 (14) | O4—Ce1—O7—C8 | −174.87 (16) |
O1—Ce1—O4—C3 | 18.59 (12) | C6—O7—C8—C8i | 163.3 (2) |
O1i—Ce1—O4—C3 | 60.70 (13) | Ce1—O7—C8—C8i | −45.3 (3) |
O20i—Ce1—O4—C5 | −74.72 (14) | C2—O1—C18—C18i | 99.3 (2) |
O20—Ce1—O4—C5 | 68.14 (14) | Ce1—O1—C18—C18i | −42.9 (2) |
Symmetry codes: (i) −x, y, −z+1/2; (ii) −x+1/2, −y+1/2, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O19—H19A···O21iii | 0.81 | 1.91 | 2.700 (2) | 163 |
O19—H19B···N11 | 0.81 | 2.14 | 2.917 (2) | 161 |
O20—H20A···O21iv | 0.82 | 1.96 | 2.768 (2) | 168 |
O20—H20B···N12v | 0.82 | 1.92 | 2.739 (2) | 171 |
O21—H21A···N13iv | 0.82 | 1.94 | 2.757 (2) | 173 |
O21—H21B···N11 | 0.82 | 2.07 | 2.888 (2) | 175 |
Symmetry codes: (iii) −x, −y+1, −z; (iv) x, −y+1, z+1/2; (v) x, −y, z+1/2. |
[Nd(C12H24O6)(H2O)4][Fe(CN)6]·2H2O | F(000) = 1472 |
Mr = 728.62 | Dx = 1.644 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 3360 reflections |
a = 19.9552 (6) Å | θ = 3.4–27.5° |
b = 11.5063 (2) Å | µ = 2.30 mm−1 |
c = 13.9706 (3) Å | T = 120 K |
β = 113.4189 (11)° | Block, yellow |
V = 2943.55 (12) Å3 | 0.34 × 0.34 × 0.25 mm |
Z = 4 |
Bruker–Nonius KappaCCD diffractometer | 3360 independent reflections |
Radiation source: Bruker-Nonius FR591 rotating anode | 3168 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
Detector resolution: 9.091 pixels mm-1 | θmax = 27.5°, θmin = 3.4° |
ϕ & ω scans | h = −25→25 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | k = −14→14 |
Tmin = 0.478, Tmax = 0.561 | l = −17→18 |
21701 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.018 | H-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 reflections | Δρmax = 0.83 e Å−3 |
176 parameters | Δρmin = −1.07 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00110 (7) |
[Nd(C12H24O6)(H2O)4][Fe(CN)6]·2H2O | V = 2943.55 (12) Å3 |
Mr = 728.62 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 19.9552 (6) Å | µ = 2.30 mm−1 |
b = 11.5063 (2) Å | T = 120 K |
c = 13.9706 (3) Å | 0.34 × 0.34 × 0.25 mm |
β = 113.4189 (11)° |
Bruker–Nonius KappaCCD diffractometer | 3360 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | 3168 reflections with I > 2σ(I) |
Tmin = 0.478, Tmax = 0.561 | Rint = 0.031 |
21701 measured reflections |
R[F2 > 2σ(F2)] = 0.018 | 0 restraints |
wR(F2) = 0.043 | H-atom parameters constrained |
S = 1.06 | Δρmax = 0.83 e Å−3 |
3360 reflections | Δρmin = −1.07 e Å−3 |
176 parameters |
x | y | z | Uiso*/Ueq | ||
Nd1 | 0.0000 | 0.235995 (11) | 0.2500 | 0.01047 (6) | |
O1 | 0.07244 (6) | 0.42143 (10) | 0.32299 (9) | 0.0147 (3) | |
C2 | 0.14156 (10) | 0.44074 (16) | 0.31489 (15) | 0.0184 (4) | |
C3 | 0.18301 (10) | 0.32854 (16) | 0.33869 (15) | 0.0210 (4) | |
O4 | 0.13804 (7) | 0.24246 (10) | 0.26887 (10) | 0.0171 (3) | |
C5 | 0.17568 (10) | 0.13461 (16) | 0.27458 (17) | 0.0235 (4) | |
C6 | 0.12105 (11) | 0.05085 (17) | 0.20432 (17) | 0.0252 (4) | |
O7 | 0.06155 (7) | 0.04755 (11) | 0.23773 (10) | 0.0174 (3) | |
C8 | 0.02092 (11) | −0.05890 (16) | 0.21581 (18) | 0.0265 (5) | |
C18 | 0.02852 (10) | 0.52602 (15) | 0.30506 (15) | 0.0190 (4) | |
O19 | 0.02701 (7) | 0.31846 (12) | 0.10311 (10) | 0.0208 (3) | |
O20 | 0.08381 (7) | 0.17143 (11) | 0.42465 (10) | 0.0208 (3) | |
Fe1 | 0.2500 | 0.2500 | 0.0000 | 0.00844 (8) | |
N11 | 0.14676 (9) | 0.40933 (14) | 0.05722 (13) | 0.0209 (3) | |
C11 | 0.18383 (9) | 0.34807 (15) | 0.03506 (13) | 0.0140 (3) | |
N12 | 0.16593 (9) | 0.02424 (14) | −0.00129 (12) | 0.0214 (3) | |
C12 | 0.19654 (9) | 0.10940 (15) | 0.00127 (13) | 0.0135 (3) | |
N13 | 0.15783 (9) | 0.27066 (14) | −0.23642 (12) | 0.0194 (3) | |
C13 | 0.19176 (9) | 0.26363 (14) | −0.14838 (14) | 0.0126 (3) | |
O21 | 0.10008 (7) | 0.64648 (11) | 0.06217 (10) | 0.0225 (3) | |
H2A | 0.1697 | 0.5014 | 0.3650 | 0.022* | |
H2B | 0.1333 | 0.4671 | 0.2436 | 0.022* | |
H3A | 0.2293 | 0.3373 | 0.3291 | 0.025* | |
H3B | 0.1948 | 0.3054 | 0.4118 | 0.025* | |
H5A | 0.1961 | 0.1051 | 0.3471 | 0.028* | |
H5B | 0.2162 | 0.1457 | 0.2516 | 0.028* | |
H6A | 0.1036 | 0.0770 | 0.1309 | 0.030* | |
H6B | 0.1431 | −0.0273 | 0.2099 | 0.030* | |
H8A | 0.0543 | −0.1265 | 0.2318 | 0.032* | |
H8B | −0.0128 | −0.0625 | 0.1414 | 0.032* | |
H18A | 0.0601 | 0.5954 | 0.3164 | 0.023* | |
H18B | 0.0045 | 0.5293 | 0.3549 | 0.023* | |
H19A | −0.0049 | 0.3304 | 0.0462 | 0.046* | |
H19B | 0.0677 | 0.3340 | 0.1011 | 0.046* | |
H20A | 0.0949 | 0.2198 | 0.4730 | 0.046* | |
H20B | 0.1100 | 0.1146 | 0.4552 | 0.046* | |
H21A | 0.1157 | 0.6666 | 0.1242 | 0.046* | |
H21B | 0.1138 | 0.5823 | 0.0580 | 0.046* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nd1 | 0.01103 (8) | 0.01016 (8) | 0.00979 (8) | 0.000 | 0.00369 (5) | 0.000 |
O1 | 0.0128 (6) | 0.0130 (6) | 0.0169 (6) | −0.0010 (4) | 0.0044 (5) | 0.0001 (5) |
C2 | 0.0153 (9) | 0.0184 (9) | 0.0210 (10) | −0.0055 (7) | 0.0068 (8) | −0.0009 (7) |
C3 | 0.0125 (9) | 0.0228 (10) | 0.0246 (10) | −0.0037 (7) | 0.0040 (8) | −0.0003 (8) |
O4 | 0.0134 (6) | 0.0160 (7) | 0.0216 (7) | 0.0010 (4) | 0.0065 (5) | 0.0011 (5) |
C5 | 0.0186 (9) | 0.0200 (10) | 0.0381 (12) | 0.0047 (7) | 0.0179 (9) | 0.0050 (8) |
C6 | 0.0289 (11) | 0.0215 (10) | 0.0357 (12) | 0.0039 (8) | 0.0238 (10) | −0.0008 (8) |
O7 | 0.0180 (6) | 0.0128 (6) | 0.0240 (7) | −0.0001 (5) | 0.0112 (6) | −0.0029 (5) |
C8 | 0.0202 (10) | 0.0123 (9) | 0.0453 (13) | 0.0006 (7) | 0.0111 (9) | −0.0070 (8) |
C18 | 0.0188 (9) | 0.0114 (9) | 0.0235 (10) | 0.0004 (7) | 0.0050 (8) | −0.0021 (7) |
O19 | 0.0158 (6) | 0.0315 (8) | 0.0137 (6) | −0.0044 (5) | 0.0043 (5) | 0.0044 (5) |
O20 | 0.0299 (7) | 0.0156 (7) | 0.0126 (6) | 0.0098 (5) | 0.0039 (6) | 0.0009 (5) |
Fe1 | 0.00896 (16) | 0.00895 (17) | 0.00733 (16) | −0.00085 (11) | 0.00316 (13) | −0.00016 (11) |
N11 | 0.0225 (8) | 0.0214 (8) | 0.0215 (8) | 0.0037 (6) | 0.0118 (7) | 0.0008 (7) |
C11 | 0.0157 (8) | 0.0141 (8) | 0.0113 (8) | −0.0015 (6) | 0.0045 (7) | 0.0023 (6) |
N12 | 0.0270 (9) | 0.0198 (8) | 0.0194 (8) | −0.0086 (7) | 0.0114 (7) | −0.0032 (6) |
C12 | 0.0151 (8) | 0.0160 (9) | 0.0090 (8) | 0.0001 (7) | 0.0044 (7) | −0.0017 (6) |
N13 | 0.0232 (8) | 0.0185 (8) | 0.0133 (8) | −0.0043 (6) | 0.0039 (7) | 0.0012 (6) |
C13 | 0.0143 (8) | 0.0097 (8) | 0.0148 (9) | −0.0013 (6) | 0.0067 (7) | 0.0005 (6) |
O21 | 0.0320 (8) | 0.0181 (7) | 0.0110 (6) | 0.0047 (5) | 0.0019 (6) | −0.0009 (5) |
Nd1—O20i | 2.4615 (12) | C6—H6B | 0.99 |
Nd1—O20 | 2.4615 (12) | O7—C8 | 1.433 (2) |
Nd1—O19i | 2.5062 (12) | C8—C8i | 1.498 (4) |
Nd1—O19 | 2.5062 (12) | C8—H8A | 0.99 |
Nd1—O7i | 2.5312 (12) | C8—H8B | 0.99 |
Nd1—O7 | 2.5312 (12) | C18—C18i | 1.507 (4) |
Nd1—O1 | 2.5515 (12) | C18—H18A | 0.99 |
Nd1—O1i | 2.5515 (12) | C18—H18B | 0.99 |
Nd1—O4i | 2.6620 (13) | O19—H19A | 0.81 |
Nd1—O4 | 2.6620 (13) | O19—H19B | 0.84 |
O1—C2 | 1.445 (2) | O20—H20A | 0.83 |
O1—C18 | 1.451 (2) | O20—H20B | 0.84 |
C2—C3 | 1.498 (3) | Fe1—C13 | 1.9384 (18) |
C2—H2A | 0.99 | Fe1—C13ii | 1.9384 (18) |
C2—H2B | 0.99 | Fe1—C12 | 1.9418 (17) |
C3—O4 | 1.429 (2) | Fe1—C12ii | 1.9418 (17) |
C3—H3A | 0.99 | Fe1—C11ii | 1.9419 (18) |
C3—H3B | 0.99 | Fe1—C11 | 1.9419 (18) |
O4—C5 | 1.436 (2) | N11—C11 | 1.150 (2) |
C5—C6 | 1.493 (3) | N12—C12 | 1.148 (2) |
C5—H5A | 0.99 | N13—C13 | 1.147 (2) |
C5—H5B | 0.99 | O21—H21A | 0.83 |
C6—O7 | 1.439 (2) | O21—H21B | 0.80 |
C6—H6A | 0.99 | ||
O20i—Nd1—O20 | 144.86 (6) | C2—C3—H3B | 110.2 |
O20i—Nd1—O19i | 130.05 (4) | H3A—C3—H3B | 108.5 |
O20—Nd1—O19i | 65.49 (4) | C3—O4—C5 | 112.85 (14) |
O20i—Nd1—O19 | 65.49 (4) | C3—O4—Nd1 | 115.55 (10) |
O20—Nd1—O19 | 130.05 (4) | C5—O4—Nd1 | 118.62 (10) |
O19i—Nd1—O19 | 135.51 (6) | O4—C5—C6 | 106.99 (15) |
O20i—Nd1—O7i | 69.62 (4) | O4—C5—H5A | 110.3 |
O20—Nd1—O7i | 80.28 (4) | C6—C5—H5A | 110.3 |
O19i—Nd1—O7i | 90.05 (4) | O4—C5—H5B | 110.3 |
O19—Nd1—O7i | 130.38 (4) | C6—C5—H5B | 110.3 |
O20i—Nd1—O7 | 80.28 (4) | H5A—C5—H5B | 108.6 |
O20—Nd1—O7 | 69.62 (4) | O7—C6—C5 | 106.54 (15) |
O19i—Nd1—O7 | 130.38 (4) | O7—C6—H6A | 110.4 |
O19—Nd1—O7 | 90.05 (4) | C5—C6—H6A | 110.4 |
O7i—Nd1—O7 | 62.11 (6) | O7—C6—H6B | 110.4 |
O20i—Nd1—O1 | 134.62 (4) | C5—C6—H6B | 110.4 |
O20—Nd1—O1 | 78.60 (4) | H6A—C6—H6B | 108.6 |
O19i—Nd1—O1 | 68.18 (4) | C8—O7—C6 | 115.02 (14) |
O19—Nd1—O1 | 74.85 (4) | C8—O7—Nd1 | 119.88 (10) |
O7i—Nd1—O1 | 154.47 (4) | C6—O7—Nd1 | 118.99 (10) |
O7—Nd1—O1 | 122.03 (4) | O7—C8—C8i | 105.96 (14) |
O20i—Nd1—O1i | 78.60 (4) | O7—C8—H8A | 110.5 |
O20—Nd1—O1i | 134.62 (4) | C8i—C8—H8A | 110.5 |
O19i—Nd1—O1i | 74.85 (4) | O7—C8—H8B | 110.5 |
O19—Nd1—O1i | 68.18 (4) | C8i—C8—H8B | 110.5 |
O7i—Nd1—O1i | 122.03 (4) | H8A—C8—H8B | 108.7 |
O7—Nd1—O1i | 154.47 (4) | O1—C18—C18i | 109.61 (12) |
O1—Nd1—O1i | 66.51 (5) | O1—C18—H18A | 109.7 |
O20i—Nd1—O4i | 69.00 (4) | C18i—C18—H18A | 109.7 |
O20—Nd1—O4i | 112.04 (4) | O1—C18—H18B | 109.7 |
O19i—Nd1—O4i | 61.29 (4) | C18i—C18—H18B | 109.7 |
O19—Nd1—O4i | 117.33 (4) | H18A—C18—H18B | 108.2 |
O7i—Nd1—O4i | 61.30 (4) | Nd1—O19—H19A | 121.8 |
O7—Nd1—O4i | 121.88 (4) | Nd1—O19—H19B | 129.1 |
O1—Nd1—O4i | 114.57 (4) | H19A—O19—H19B | 109.0 |
O1i—Nd1—O4i | 62.45 (4) | Nd1—O20—H20A | 117.3 |
O20i—Nd1—O4 | 112.04 (4) | Nd1—O20—H20B | 141.2 |
O20—Nd1—O4 | 69.00 (4) | H20A—O20—H20B | 101.4 |
O19i—Nd1—O4 | 117.33 (4) | C13—Fe1—C13ii | 180.00 (11) |
O19—Nd1—O4 | 61.29 (4) | C13—Fe1—C12 | 88.80 (7) |
O7i—Nd1—O4 | 121.88 (4) | C13ii—Fe1—C12 | 91.20 (7) |
O7—Nd1—O4 | 61.30 (4) | C13—Fe1—C12ii | 91.20 (7) |
O1—Nd1—O4 | 62.45 (4) | C13ii—Fe1—C12ii | 88.80 (7) |
O1i—Nd1—O4 | 114.57 (4) | C12—Fe1—C12ii | 180.00 (11) |
O4i—Nd1—O4 | 176.80 (5) | C13—Fe1—C11ii | 87.48 (7) |
C2—O1—C18 | 112.88 (13) | C13ii—Fe1—C11ii | 92.52 (7) |
C2—O1—Nd1 | 120.27 (10) | C12—Fe1—C11ii | 87.09 (7) |
C18—O1—Nd1 | 114.66 (9) | C12ii—Fe1—C11ii | 92.91 (7) |
O1—C2—C3 | 108.07 (14) | C13—Fe1—C11 | 92.52 (7) |
O1—C2—H2A | 110.1 | C13ii—Fe1—C11 | 87.48 (7) |
C3—C2—H2A | 110.1 | C12—Fe1—C11 | 92.91 (7) |
O1—C2—H2B | 110.1 | C12ii—Fe1—C11 | 87.09 (7) |
C3—C2—H2B | 110.1 | C11ii—Fe1—C11 | 180.00 (9) |
H2A—C2—H2B | 108.4 | N11—C11—Fe1 | 177.35 (16) |
O4—C3—C2 | 107.72 (14) | N12—C12—Fe1 | 176.93 (16) |
O4—C3—H3A | 110.2 | N13—C13—Fe1 | 179.14 (17) |
C2—C3—H3A | 110.2 | H21A—O21—H21B | 109.7 |
O4—C3—H3B | 110.2 | ||
O20i—Nd1—O1—C2 | −81.42 (13) | O19i—Nd1—O4—C5 | 115.81 (13) |
O20—Nd1—O1—C2 | 85.26 (12) | O19—Nd1—O4—C5 | −114.95 (14) |
O19i—Nd1—O1—C2 | 153.22 (12) | O7i—Nd1—O4—C5 | 7.00 (14) |
O19—Nd1—O1—C2 | −52.01 (11) | O7—Nd1—O4—C5 | −7.44 (12) |
O7i—Nd1—O1—C2 | 119.99 (13) | O1—Nd1—O4—C5 | 157.94 (14) |
O7—Nd1—O1—C2 | 28.29 (13) | O1i—Nd1—O4—C5 | −159.19 (12) |
O1i—Nd1—O1—C2 | −124.42 (13) | C3—O4—C5—C6 | 175.73 (15) |
O4i—Nd1—O1—C2 | −165.54 (11) | Nd1—O4—C5—C6 | 35.97 (19) |
O4—Nd1—O1—C2 | 13.15 (11) | O4—C5—C6—O7 | −55.2 (2) |
O20i—Nd1—O1—C18 | 58.33 (13) | C5—C6—O7—C8 | −153.11 (16) |
O20—Nd1—O1—C18 | −134.98 (12) | C5—C6—O7—Nd1 | 54.39 (18) |
O19i—Nd1—O1—C18 | −67.02 (11) | O20i—Nd1—O7—C8 | −55.06 (14) |
O19—Nd1—O1—C18 | 87.74 (11) | O20—Nd1—O7—C8 | 106.52 (14) |
O7i—Nd1—O1—C18 | −100.25 (13) | O19i—Nd1—O7—C8 | 80.28 (14) |
O7—Nd1—O1—C18 | 168.05 (10) | O19—Nd1—O7—C8 | −120.16 (14) |
O1i—Nd1—O1—C18 | 15.34 (9) | O7i—Nd1—O7—C8 | 16.94 (11) |
O4i—Nd1—O1—C18 | −25.79 (12) | O1—Nd1—O7—C8 | 167.77 (13) |
O4—Nd1—O1—C18 | 152.91 (12) | O1i—Nd1—O7—C8 | −89.58 (16) |
C18—O1—C2—C3 | 177.91 (14) | O4i—Nd1—O7—C8 | 2.61 (15) |
Nd1—O1—C2—C3 | −41.69 (17) | O4—Nd1—O7—C8 | −176.92 (15) |
O1—C2—C3—O4 | 55.92 (19) | O20i—Nd1—O7—C6 | 96.09 (13) |
C2—C3—O4—C5 | 172.09 (15) | O20—Nd1—O7—C6 | −102.33 (13) |
C2—C3—O4—Nd1 | −46.86 (17) | O19i—Nd1—O7—C6 | −128.58 (12) |
O20i—Nd1—O4—C3 | 149.28 (11) | O19—Nd1—O7—C6 | 30.99 (13) |
O20—Nd1—O4—C3 | −68.57 (12) | O7i—Nd1—O7—C6 | 168.08 (16) |
O19i—Nd1—O4—C3 | −22.89 (13) | O1—Nd1—O7—C6 | −41.08 (14) |
O19—Nd1—O4—C3 | 106.34 (12) | O1i—Nd1—O7—C6 | 61.57 (16) |
O7i—Nd1—O4—C3 | −131.71 (11) | O4i—Nd1—O7—C6 | 153.76 (12) |
O7—Nd1—O4—C3 | −146.15 (13) | O4—Nd1—O7—C6 | −25.78 (12) |
O1—Nd1—O4—C3 | 19.23 (11) | C6—O7—C8—C8i | 162.68 (18) |
O1i—Nd1—O4—C3 | 62.10 (12) | Nd1—O7—C8—C8i | −45.1 (2) |
O20i—Nd1—O4—C5 | −72.01 (13) | C2—O1—C18—C18i | 99.72 (19) |
O20—Nd1—O4—C5 | 70.14 (13) | Nd1—O1—C18—C18i | −43.0 (2) |
Symmetry codes: (i) −x, y, −z+1/2; (ii) −x+1/2, −y+1/2, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O19—H19A···O21iii | 0.81 | 1.92 | 2.697 (2) | 161 |
O19—H19B···N11 | 0.84 | 2.09 | 2.904 (2) | 161 |
O20—H20A···O21iv | 0.83 | 1.96 | 2.773 (2) | 166 |
O20—H20B···N12v | 0.84 | 1.90 | 2.734 (2) | 169 |
O21—H21A···N13iv | 0.83 | 1.93 | 2.753 (2) | 173 |
O21—H21B···N11 | 0.80 | 2.10 | 2.893 (2) | 175 |
Symmetry codes: (iii) −x, −y+1, −z; (iv) x, −y+1, z+1/2; (v) x, −y, z+1/2. |
[Sm(C12H24O6)(H2O)3][Fe(CN)6]·2H2O | Z = 2 |
Mr = 716.71 | F(000) = 720 |
Triclinic, P1 | Dx = 1.694 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.9324 (2) Å | Cell parameters from 6393 reflections |
b = 11.0996 (2) Å | θ = 2.9–27.5° |
c = 14.0119 (4) Å | µ = 2.65 mm−1 |
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 |
Bruker–Nonius KappaCCD diffractometer | 6453 independent reflections |
Radiation source: Bruker–Nonius FR591 rotating anode | 5624 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.050 |
Detector resolution: 9.091 pixels mm-1 | θmax = 27.5°, θmin = 3.4° |
ϕ & ω scans | h = −14→14 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | k = −14→14 |
Tmin = 0.836, Tmax = 0.900 | l = −18→18 |
28348 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.030 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.067 | H-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 parameters | Δρmax = 0.95 e Å−3 |
8 restraints | Δρmin = −0.91 e Å−3 |
[Sm(C12H24O6)(H2O)3][Fe(CN)6]·2H2O | γ = 65.7231 (14)° |
Mr = 716.71 | V = 1404.77 (6) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.9324 (2) Å | Mo Kα radiation |
b = 11.0996 (2) Å | µ = 2.65 mm−1 |
c = 14.0119 (4) Å | T = 120 K |
α = 67.9012 (13)° | 0.10 × 0.06 × 0.04 mm |
β = 70.7291 (13)° |
Bruker–Nonius KappaCCD diffractometer | 6453 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | 5624 reflections with I > 2σ(I) |
Tmin = 0.836, Tmax = 0.900 | Rint = 0.050 |
28348 measured reflections |
R[F2 > 2σ(F2)] = 0.030 | 8 restraints |
wR(F2) = 0.067 | H-atom parameters constrained |
S = 1.01 | Δρmax = 0.95 e Å−3 |
6453 reflections | Δρmin = −0.91 e Å−3 |
334 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Sm1 | 0.205433 (16) | 0.728591 (16) | 0.277416 (13) | 0.01394 (6) | |
O1 | 0.0588 (2) | 0.5655 (2) | 0.36656 (17) | 0.0189 (5) | |
C2 | 0.0921 (4) | 0.4542 (4) | 0.3228 (4) | 0.0279 (12)* | 0.815 (7) |
C2A | 0.1295 (12) | 0.4229 (6) | 0.3844 (7) | 0.010 (4)* | 0.185 (7) |
C3 | 0.2417 (3) | 0.3963 (3) | 0.2901 (3) | 0.0275 (8) | |
O4 | 0.2921 (2) | 0.5070 (2) | 0.2303 (2) | 0.0275 (6) | |
C5 | 0.4238 (3) | 0.4739 (4) | 0.1590 (3) | 0.0254 (8) | |
C6 | 0.5228 (3) | 0.4977 (3) | 0.1954 (3) | 0.0246 (8) | |
O7 | 0.4633 (2) | 0.6364 (2) | 0.20323 (17) | 0.0181 (5) | |
C8 | 0.5484 (3) | 0.6729 (3) | 0.2401 (3) | 0.0233 (7) | |
C9 | 0.4956 (3) | 0.8257 (3) | 0.2162 (3) | 0.0248 (8) | |
O10 | 0.3491 (2) | 0.8688 (2) | 0.25898 (18) | 0.0200 (5) | |
C11 | 0.2963 (4) | 1.0173 (3) | 0.2268 (3) | 0.0280 (8) | |
C12 | 0.1440 (3) | 1.0625 (3) | 0.2628 (3) | 0.0246 (8) | |
O13 | 0.0962 (2) | 0.9900 (2) | 0.22425 (17) | 0.0186 (5) | |
C14 | −0.0485 (3) | 1.0509 (3) | 0.2243 (3) | 0.0219 (7) | |
C15 | −0.0818 (3) | 0.9621 (3) | 0.1857 (3) | 0.0219 (7) | |
O16 | −0.0338 (2) | 0.8226 (2) | 0.25158 (18) | 0.0205 (5) | |
C17 | −0.1292 (3) | 0.7491 (3) | 0.2942 (3) | 0.0273 (8) | |
C18 | −0.0848 (3) | 0.6330 (4) | 0.3879 (3) | 0.0270 (12)* | 0.815 (7) |
C18A | −0.0590 (12) | 0.5983 (6) | 0.3272 (14) | 0.018 (4)* | 0.185 (7) |
O19 | 0.2297 (2) | 0.7930 (2) | 0.09554 (17) | 0.0196 (5) | |
O20 | 0.3158 (2) | 0.5735 (2) | 0.42200 (17) | 0.0195 (5) | |
O21 | 0.0801 (2) | 0.8005 (2) | 0.43465 (17) | 0.0189 (5) | |
Fe2 | 0.0000 | 0.5000 | 0.0000 | 0.01376 (13) | |
N21 | 0.0581 (3) | 0.7292 (3) | 0.0340 (2) | 0.0285 (7) | |
N22 | 0.1331 (3) | 0.5978 (3) | −0.2337 (2) | 0.0230 (6) | |
N23 | 0.2919 (3) | 0.3143 (3) | 0.0375 (3) | 0.0321 (7) | |
C21 | 0.0333 (3) | 0.6454 (3) | 0.0226 (2) | 0.0188 (7) | |
C22 | 0.0823 (3) | 0.5611 (3) | −0.1474 (3) | 0.0174 (7) | |
C23 | 0.1822 (3) | 0.3810 (3) | 0.0247 (3) | 0.0209 (7) | |
Fe3 | 0.5000 | 0.0000 | 0.5000 | 0.01334 (13) | |
N31 | 0.4328 (3) | −0.1013 (3) | 0.7432 (2) | 0.0250 (6) | |
N32 | 0.1950 (3) | 0.0809 (3) | 0.4967 (2) | 0.0255 (7) | |
N33 | 0.4472 (3) | 0.2968 (3) | 0.4966 (2) | 0.0261 (7) | |
C31 | 0.4565 (3) | −0.0631 (3) | 0.6529 (3) | 0.0177 (7) | |
C32 | 0.3086 (3) | 0.0499 (3) | 0.4966 (3) | 0.0177 (7) | |
C33 | 0.4666 (3) | 0.1848 (3) | 0.5010 (3) | 0.0183 (7) | |
O41 | 0.2522 (2) | 0.7061 (2) | 0.56604 (18) | 0.0237 (5) | |
O42 | 0.4350 (2) | 0.8550 (3) | −0.04449 (19) | 0.0297 (6) | |
H2A | 0.0490 | 0.4887 | 0.2613 | 0.033* | 0.815 (7) |
H2B | 0.0556 | 0.3816 | 0.3761 | 0.033* | 0.815 (7) |
H2C | 0.0648 | 0.3742 | 0.3973 | 0.012* | 0.185 (7) |
H2D | 0.1694 | 0.3874 | 0.4476 | 0.012* | 0.185 (7) |
H3A | 0.2836 | 0.3435 | 0.3527 | 0.033* | 0.815 (7) |
H3B | 0.2648 | 0.3336 | 0.2472 | 0.033* | 0.815 (7) |
H3C | 0.3188 | 0.3143 | 0.3143 | 0.033* | 0.185 (7) |
H3D | 0.2066 | 0.3747 | 0.2439 | 0.033* | 0.185 (7) |
H5A | 0.4162 | 0.5329 | 0.0865 | 0.030* | |
H5B | 0.4553 | 0.3765 | 0.1591 | 0.030* | |
H6A | 0.5384 | 0.4319 | 0.2648 | 0.029* | |
H6B | 0.6118 | 0.4856 | 0.1445 | 0.029* | |
H8A | 0.6454 | 0.6413 | 0.2036 | 0.028* | |
H8B | 0.5425 | 0.6299 | 0.3168 | 0.028* | |
H9A | 0.5424 | 0.8560 | 0.2481 | 0.030* | |
H9B | 0.5138 | 0.8678 | 0.1391 | 0.030* | |
H11A | 0.3210 | 1.0519 | 0.1492 | 0.034* | |
H11B | 0.3367 | 1.0549 | 0.2582 | 0.034* | |
H12A | 0.1184 | 1.0391 | 0.3407 | 0.030* | |
H12B | 0.1038 | 1.1632 | 0.2339 | 0.030* | |
H14A | −0.0693 | 1.1461 | 0.1772 | 0.026* | |
H14B | −0.1025 | 1.0534 | 0.2962 | 0.026* | |
H15A | −0.1819 | 0.9921 | 0.1912 | 0.026* | |
H15B | −0.0353 | 0.9677 | 0.1112 | 0.026* | |
H17A | −0.1314 | 0.7125 | 0.2406 | 0.033* | 0.815 (7) |
H17B | −0.2224 | 0.8113 | 0.3156 | 0.033* | 0.815 (7) |
H17C | −0.1815 | 0.7711 | 0.2406 | 0.033* | 0.185 (7) |
H17D | −0.1952 | 0.7790 | 0.3556 | 0.033* | 0.185 (7) |
H18A | −0.1104 | 0.6695 | 0.4488 | 0.032* | 0.815 (7) |
H18B | −0.1329 | 0.5662 | 0.4065 | 0.032* | 0.815 (7) |
H18C | −0.1236 | 0.5539 | 0.3825 | 0.021* | 0.185 (7) |
H18D | −0.0309 | 0.5612 | 0.2662 | 0.021* | 0.185 (7) |
H19A | 0.1785 | 0.7762 | 0.0688 | 0.044 (4)* | |
H19B | 0.2949 | 0.8061 | 0.0467 | 0.044 (4)* | |
H20A | 0.3082 | 0.6023 | 0.4749 | 0.044 (4)* | |
H20B | 0.3674 | 0.4866 | 0.4372 | 0.044 (4)* | |
H21A | 0.1168 | 0.7892 | 0.4850 | 0.044 (4)* | |
H21B | −0.0057 | 0.8469 | 0.4544 | 0.044 (4)* | |
H41A | 0.2206 | 0.6776 | 0.6291 | 0.044 (4)* | |
H41B | 0.3102 | 0.7349 | 0.5636 | 0.044 (4)* | |
H42A | 0.4296 | 0.8676 | −0.1060 | 0.044 (4)* | |
H42B | 0.5093 | 0.7951 | −0.0421 | 0.044 (4)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sm1 | 0.01185 (9) | 0.01500 (9) | 0.01319 (9) | −0.00443 (6) | −0.00128 (6) | −0.00318 (6) |
O1 | 0.0195 (12) | 0.0219 (12) | 0.0169 (12) | −0.0102 (9) | −0.0028 (9) | −0.0042 (9) |
C3 | 0.039 (2) | 0.0166 (17) | 0.027 (2) | −0.0138 (16) | −0.0002 (17) | −0.0061 (15) |
O4 | 0.0218 (13) | 0.0224 (12) | 0.0390 (16) | −0.0116 (10) | 0.0066 (11) | −0.0155 (11) |
C5 | 0.0240 (18) | 0.0256 (18) | 0.026 (2) | −0.0066 (15) | 0.0030 (15) | −0.0156 (15) |
C6 | 0.0166 (17) | 0.0216 (17) | 0.030 (2) | −0.0016 (14) | −0.0007 (15) | −0.0099 (15) |
O7 | 0.0126 (11) | 0.0182 (11) | 0.0222 (12) | −0.0035 (9) | −0.0014 (9) | −0.0079 (10) |
C8 | 0.0125 (16) | 0.0306 (19) | 0.029 (2) | −0.0067 (14) | −0.0031 (14) | −0.0127 (16) |
C9 | 0.0116 (16) | 0.0295 (19) | 0.032 (2) | −0.0086 (14) | 0.0015 (14) | −0.0109 (16) |
O10 | 0.0123 (11) | 0.0157 (11) | 0.0305 (14) | −0.0039 (9) | −0.0032 (10) | −0.0066 (10) |
C11 | 0.0242 (19) | 0.0158 (16) | 0.043 (2) | −0.0084 (14) | −0.0071 (17) | −0.0054 (16) |
C12 | 0.0260 (19) | 0.0148 (16) | 0.034 (2) | −0.0053 (14) | −0.0100 (16) | −0.0064 (15) |
O13 | 0.0157 (11) | 0.0165 (11) | 0.0222 (13) | −0.0037 (9) | −0.0056 (10) | −0.0045 (9) |
C14 | 0.0149 (16) | 0.0196 (16) | 0.0232 (19) | −0.0004 (13) | −0.0050 (14) | −0.0025 (14) |
C15 | 0.0186 (17) | 0.0208 (17) | 0.0194 (18) | −0.0010 (14) | −0.0073 (14) | −0.0014 (14) |
O16 | 0.0136 (11) | 0.0183 (11) | 0.0279 (13) | −0.0050 (9) | −0.0070 (10) | −0.0026 (10) |
C17 | 0.0170 (17) | 0.037 (2) | 0.025 (2) | −0.0140 (15) | −0.0020 (15) | −0.0019 (16) |
O19 | 0.0154 (11) | 0.0297 (13) | 0.0144 (12) | −0.0105 (10) | −0.0003 (9) | −0.0058 (10) |
O20 | 0.0219 (12) | 0.0166 (11) | 0.0165 (12) | −0.0009 (9) | −0.0076 (10) | −0.0038 (9) |
O21 | 0.0106 (11) | 0.0264 (12) | 0.0155 (12) | 0.0006 (9) | −0.0027 (9) | −0.0087 (10) |
Fe2 | 0.0117 (3) | 0.0164 (3) | 0.0127 (3) | −0.0058 (2) | −0.0023 (2) | −0.0024 (2) |
N21 | 0.0381 (18) | 0.0305 (17) | 0.0238 (17) | −0.0184 (14) | −0.0072 (14) | −0.0063 (13) |
N22 | 0.0219 (15) | 0.0260 (15) | 0.0203 (16) | −0.0094 (12) | −0.0024 (13) | −0.0056 (13) |
N23 | 0.0206 (17) | 0.0287 (16) | 0.0364 (19) | −0.0058 (13) | −0.0087 (14) | 0.0019 (14) |
C21 | 0.0186 (17) | 0.0221 (17) | 0.0129 (16) | −0.0070 (14) | −0.0023 (13) | −0.0024 (13) |
C22 | 0.0149 (16) | 0.0186 (16) | 0.0180 (18) | −0.0058 (13) | −0.0038 (14) | −0.0038 (13) |
C23 | 0.0210 (18) | 0.0202 (16) | 0.0182 (17) | −0.0099 (14) | −0.0018 (14) | −0.0004 (14) |
Fe3 | 0.0096 (3) | 0.0130 (3) | 0.0141 (3) | −0.0025 (2) | −0.0010 (2) | −0.0029 (2) |
N31 | 0.0193 (15) | 0.0305 (16) | 0.0184 (16) | −0.0052 (13) | −0.0026 (12) | −0.0040 (13) |
N32 | 0.0169 (15) | 0.0305 (16) | 0.0245 (17) | −0.0054 (12) | −0.0019 (12) | −0.0075 (13) |
N33 | 0.0284 (17) | 0.0187 (15) | 0.0309 (18) | −0.0059 (13) | −0.0095 (14) | −0.0057 (13) |
C31 | 0.0100 (15) | 0.0161 (15) | 0.0225 (19) | −0.0015 (12) | −0.0026 (13) | −0.0044 (14) |
C32 | 0.0153 (17) | 0.0183 (16) | 0.0161 (17) | −0.0051 (13) | 0.0002 (13) | −0.0046 (13) |
C33 | 0.0104 (15) | 0.0235 (18) | 0.0167 (17) | −0.0048 (13) | −0.0022 (13) | −0.0025 (14) |
O41 | 0.0240 (13) | 0.0361 (14) | 0.0150 (12) | −0.0184 (11) | −0.0015 (10) | −0.0040 (10) |
O42 | 0.0149 (12) | 0.0450 (15) | 0.0194 (13) | −0.0065 (11) | −0.0021 (10) | −0.0038 (11) |
Sm1—O19 | 2.327 (2) | C14—C15 | 1.491 (5) |
Sm1—O21 | 2.408 (2) | C14—H14A | 0.99 |
Sm1—O20 | 2.409 (2) | C14—H14B | 0.99 |
Sm1—O16 | 2.481 (2) | C15—O16 | 1.450 (4) |
Sm1—O4 | 2.505 (2) | C15—H15A | 0.99 |
Sm1—O10 | 2.529 (2) | C15—H15B | 0.99 |
Sm1—O13 | 2.552 (2) | O16—C17 | 1.425 (4) |
Sm1—O7 | 2.563 (2) | C17—C18A | 1.484 (5) |
Sm1—O1 | 2.602 (2) | C17—C18 | 1.501 (4) |
O1—C2A | 1.410 (5) | C17—H17A | 0.99 |
O1—C18 | 1.416 (3) | C17—H17B | 0.99 |
O1—C18A | 1.424 (5) | C17—H17C | 0.99 |
O1—C2 | 1.445 (3) | C17—H17D | 0.99 |
C2—C3 | 1.471 (4) | C18—H18A | 0.99 |
C2—H2A | 0.99 | C18—H18B | 0.99 |
C2—H2B | 0.99 | C18A—H18C | 0.99 |
C2A—C3 | 1.505 (5) | C18A—H18D | 0.99 |
C2A—H2C | 0.99 | O19—H19A | 0.87 |
C2A—H2D | 0.99 | O19—H19B | 0.83 |
C3—O4 | 1.411 (4) | O20—H20A | 0.88 |
C3—H3A | 0.99 | O20—H20B | 0.88 |
C3—H3B | 0.99 | O21—H21A | 0.87 |
C3—H3C | 0.99 | O21—H21B | 0.87 |
C3—H3D | 0.99 | Fe2—C22 | 1.939 (3) |
O4—C5 | 1.449 (4) | Fe2—C22i | 1.939 (3) |
C5—C6 | 1.484 (5) | Fe2—C23i | 1.945 (3) |
C5—H5A | 0.99 | Fe2—C23 | 1.945 (3) |
C5—H5B | 0.99 | Fe2—C21 | 1.945 (3) |
C6—O7 | 1.436 (4) | Fe2—C21i | 1.945 (3) |
C6—H6A | 0.99 | N21—C21 | 1.146 (4) |
C6—H6B | 0.99 | N22—C22 | 1.143 (4) |
O7—C8 | 1.442 (4) | N23—C23 | 1.153 (4) |
C8—C9 | 1.489 (5) | Fe3—C33 | 1.934 (3) |
C8—H8A | 0.99 | Fe3—C33ii | 1.934 (3) |
C8—H8B | 0.99 | Fe3—C32 | 1.944 (3) |
C9—O10 | 1.451 (4) | Fe3—C32ii | 1.944 (3) |
C9—H9A | 0.99 | Fe3—C31 | 1.944 (3) |
C9—H9B | 0.99 | Fe3—C31ii | 1.944 (3) |
O10—C11 | 1.443 (4) | N31—C31 | 1.147 (4) |
C11—C12 | 1.492 (5) | N32—C32 | 1.144 (4) |
C11—H11A | 0.99 | N33—C33 | 1.153 (4) |
C11—H11B | 0.99 | O41—H41A | 0.82 |
C12—O13 | 1.440 (4) | O41—H41B | 0.80 |
C12—H12A | 0.99 | O42—H42A | 0.84 |
C12—H12B | 0.99 | O42—H42B | 0.81 |
O13—C14 | 1.442 (4) | ||
O19—Sm1—O21 | 144.30 (7) | O10—C11—H11A | 109.9 |
O19—Sm1—O20 | 144.23 (7) | C12—C11—H11A | 109.9 |
O21—Sm1—O20 | 70.41 (7) | O10—C11—H11B | 109.9 |
O19—Sm1—O16 | 76.07 (8) | C12—C11—H11B | 109.9 |
O21—Sm1—O16 | 78.51 (7) | H11A—C11—H11B | 108.3 |
O20—Sm1—O16 | 134.35 (7) | O13—C12—C11 | 106.0 (3) |
O19—Sm1—O4 | 74.97 (8) | O13—C12—H12A | 110.5 |
O21—Sm1—O4 | 135.03 (8) | C11—C12—H12A | 110.5 |
O20—Sm1—O4 | 79.77 (8) | O13—C12—H12B | 110.5 |
O16—Sm1—O4 | 101.33 (8) | C11—C12—H12B | 110.5 |
O19—Sm1—O10 | 90.85 (8) | H12A—C12—H12B | 108.7 |
O21—Sm1—O10 | 84.05 (7) | C12—O13—C14 | 112.8 (2) |
O20—Sm1—O10 | 83.84 (7) | C12—O13—Sm1 | 115.11 (17) |
O16—Sm1—O10 | 125.77 (7) | C14—O13—Sm1 | 119.85 (18) |
O4—Sm1—O10 | 125.99 (7) | O13—C14—C15 | 106.0 (2) |
O19—Sm1—O13 | 74.59 (7) | O13—C14—H14A | 110.5 |
O21—Sm1—O13 | 71.66 (7) | C15—C14—H14A | 110.5 |
O20—Sm1—O13 | 131.34 (7) | O13—C14—H14B | 110.5 |
O16—Sm1—O13 | 62.89 (7) | C15—C14—H14B | 110.5 |
O4—Sm1—O13 | 148.36 (8) | H14A—C14—H14B | 108.7 |
O10—Sm1—O13 | 62.89 (7) | O16—C15—C14 | 106.8 (3) |
O19—Sm1—O7 | 74.23 (7) | O16—C15—H15A | 110.4 |
O21—Sm1—O7 | 131.71 (7) | C14—C15—H15A | 110.4 |
O20—Sm1—O7 | 71.91 (7) | O16—C15—H15B | 110.4 |
O16—Sm1—O7 | 149.21 (7) | C14—C15—H15B | 110.4 |
O4—Sm1—O7 | 63.15 (7) | H15A—C15—H15B | 108.6 |
O10—Sm1—O7 | 62.83 (7) | C17—O16—C15 | 116.1 (2) |
O13—Sm1—O7 | 115.60 (7) | C17—O16—Sm1 | 125.34 (17) |
O19—Sm1—O1 | 109.70 (7) | C15—O16—Sm1 | 118.51 (18) |
O21—Sm1—O1 | 79.51 (7) | O16—C17—C18A | 111.5 (5) |
O20—Sm1—O1 | 79.10 (7) | O16—C17—C18 | 108.2 (3) |
O16—Sm1—O1 | 62.70 (7) | O16—C17—H17A | 110.1 |
O4—Sm1—O1 | 62.01 (7) | C18—C17—H17A | 110.1 |
O10—Sm1—O1 | 159.45 (7) | O16—C17—H17B | 110.1 |
O13—Sm1—O1 | 122.01 (7) | C18—C17—H17B | 110.1 |
O7—Sm1—O1 | 121.17 (6) | H17A—C17—H17B | 108.4 |
C2A—O1—C18A | 108.6 (7) | O16—C17—H17C | 109.3 |
C18—O1—C2 | 110.9 (3) | C18A—C17—H17C | 109.3 |
C2A—O1—Sm1 | 117.2 (5) | O16—C17—H17D | 109.3 |
C18—O1—Sm1 | 114.9 (2) | C18A—C17—H17D | 109.3 |
C18A—O1—Sm1 | 118.1 (5) | H17C—C17—H17D | 108.0 |
C2—O1—Sm1 | 117.6 (2) | O1—C18—C17 | 111.0 (3) |
O1—C2—C3 | 109.7 (3) | O1—C18—H18A | 109.4 |
O1—C2—H2A | 109.7 | C17—C18—H18A | 109.4 |
C3—C2—H2A | 109.7 | O1—C18—H18B | 109.4 |
O1—C2—H2B | 109.7 | C17—C18—H18B | 109.4 |
C3—C2—H2B | 109.7 | H18A—C18—H18B | 108.0 |
H2A—C2—H2B | 108.2 | O1—C18A—C17 | 111.6 (5) |
O1—C2A—C3 | 109.7 (4) | O1—C18A—H18C | 109.3 |
O1—C2A—H2C | 109.7 | C17—C18A—H18C | 109.3 |
C3—C2A—H2C | 109.7 | O1—C18A—H18D | 109.3 |
O1—C2A—H2D | 109.7 | C17—C18A—H18D | 109.3 |
C3—C2A—H2D | 109.7 | H18C—C18A—H18D | 108.0 |
H2C—C2A—H2D | 108.2 | Sm1—O19—H19A | 119.5 |
O4—C3—C2 | 107.7 (3) | Sm1—O19—H19B | 131.6 |
O4—C3—C2A | 114.3 (4) | H19A—O19—H19B | 105.3 |
O4—C3—H3A | 110.2 | Sm1—O20—H20A | 120.4 |
C2—C3—H3A | 110.2 | Sm1—O20—H20B | 134.6 |
O4—C3—H3B | 110.2 | H20A—O20—H20B | 105.0 |
C2—C3—H3B | 110.2 | Sm1—O21—H21A | 124.6 |
H3A—C3—H3B | 108.5 | Sm1—O21—H21B | 132.2 |
O4—C3—H3C | 108.7 | H21A—O21—H21B | 103.0 |
C2A—C3—H3C | 108.7 | C22—Fe2—C22i | 180.0 (2) |
O4—C3—H3D | 108.7 | C22—Fe2—C23i | 91.64 (13) |
C2A—C3—H3D | 108.7 | C22i—Fe2—C23i | 88.36 (13) |
H3C—C3—H3D | 107.6 | C22—Fe2—C23 | 88.36 (13) |
C3—O4—C5 | 116.0 (2) | C22i—Fe2—C23 | 91.64 (13) |
C3—O4—Sm1 | 123.26 (19) | C23i—Fe2—C23 | 180.0 (2) |
C5—O4—Sm1 | 118.28 (18) | C22—Fe2—C21 | 87.90 (13) |
O4—C5—C6 | 107.9 (3) | C22i—Fe2—C21 | 92.10 (13) |
O4—C5—H5A | 110.1 | C23i—Fe2—C21 | 91.97 (13) |
C6—C5—H5A | 110.1 | C23—Fe2—C21 | 88.03 (13) |
O4—C5—H5B | 110.1 | C22—Fe2—C21i | 92.10 (13) |
C6—C5—H5B | 110.1 | C22i—Fe2—C21i | 87.90 (13) |
H5A—C5—H5B | 108.4 | C23i—Fe2—C21i | 88.03 (13) |
O7—C6—C5 | 106.6 (3) | C23—Fe2—C21i | 91.97 (13) |
O7—C6—H6A | 110.4 | C21—Fe2—C21i | 180.00 (17) |
C5—C6—H6A | 110.4 | N21—C21—Fe2 | 177.3 (3) |
O7—C6—H6B | 110.4 | N22—C22—Fe2 | 178.3 (3) |
C5—C6—H6B | 110.4 | N23—C23—Fe2 | 177.6 (3) |
H6A—C6—H6B | 108.6 | C33—Fe3—C33ii | 180.0 (2) |
C6—O7—C8 | 112.5 (2) | C33—Fe3—C32 | 89.79 (13) |
C6—O7—Sm1 | 118.97 (18) | C33ii—Fe3—C32 | 90.21 (13) |
C8—O7—Sm1 | 114.86 (17) | C33—Fe3—C32ii | 90.21 (13) |
O7—C8—C9 | 106.4 (3) | C33ii—Fe3—C32ii | 89.79 (13) |
O7—C8—H8A | 110.5 | C32—Fe3—C32ii | 180.0 (2) |
C9—C8—H8A | 110.5 | C33—Fe3—C31 | 92.14 (13) |
O7—C8—H8B | 110.5 | C33ii—Fe3—C31 | 87.86 (13) |
C9—C8—H8B | 110.5 | C32—Fe3—C31 | 90.21 (13) |
H8A—C8—H8B | 108.6 | C32ii—Fe3—C31 | 89.79 (13) |
O10—C9—C8 | 108.7 (3) | C33—Fe3—C31ii | 87.86 (13) |
O10—C9—H9A | 110.0 | C33ii—Fe3—C31ii | 92.14 (13) |
C8—C9—H9A | 110.0 | C32—Fe3—C31ii | 89.79 (13) |
O10—C9—H9B | 110.0 | C32ii—Fe3—C31ii | 90.21 (13) |
C8—C9—H9B | 110.0 | C31—Fe3—C31ii | 180.000 (1) |
H9A—C9—H9B | 108.3 | N31—C31—Fe3 | 179.1 (3) |
C11—O10—C9 | 108.4 (2) | N32—C32—Fe3 | 178.2 (3) |
C11—O10—Sm1 | 120.66 (18) | N33—C33—Fe3 | 176.8 (3) |
C9—O10—Sm1 | 120.97 (18) | H41A—O41—H41B | 105.7 |
O10—C11—C12 | 108.8 (3) | H42A—O42—H42B | 100.3 |
O19—Sm1—O1—C2A | 91.0 (6) | O10—Sm1—O7—C8 | 29.4 (2) |
O21—Sm1—O1—C2A | −124.8 (6) | O13—Sm1—O7—C8 | 64.9 (2) |
O20—Sm1—O1—C2A | −53.0 (6) | O1—Sm1—O7—C8 | −127.5 (2) |
O16—Sm1—O1—C2A | 152.8 (6) | C6—O7—C8—C9 | 164.6 (3) |
O4—Sm1—O1—C2A | 31.1 (6) | Sm1—O7—C8—C9 | −55.0 (3) |
O10—Sm1—O1—C2A | −87.4 (6) | O7—C8—C9—O10 | 52.3 (4) |
O13—Sm1—O1—C2A | 174.7 (6) | C8—C9—O10—C11 | −174.5 (3) |
O7—Sm1—O1—C2A | 7.9 (6) | C8—C9—O10—Sm1 | −28.8 (4) |
O19—Sm1—O1—C18 | −86.9 (2) | O19—Sm1—O10—C11 | 70.7 (2) |
O21—Sm1—O1—C18 | 57.3 (2) | O21—Sm1—O10—C11 | −73.9 (2) |
O20—Sm1—O1—C18 | 129.2 (2) | O20—Sm1—O10—C11 | −144.7 (2) |
O16—Sm1—O1—C18 | −25.1 (2) | O16—Sm1—O10—C11 | −2.7 (3) |
O4—Sm1—O1—C18 | −146.7 (3) | O4—Sm1—O10—C11 | 142.7 (2) |
O10—Sm1—O1—C18 | 94.7 (3) | O13—Sm1—O10—C11 | −1.5 (2) |
O13—Sm1—O1—C18 | −3.1 (3) | O7—Sm1—O10—C11 | 142.5 (3) |
O7—Sm1—O1—C18 | −169.9 (2) | O1—Sm1—O10—C11 | −110.8 (3) |
O19—Sm1—O1—C18A | −41.9 (8) | O19—Sm1—O10—C9 | −70.8 (2) |
O21—Sm1—O1—C18A | 102.3 (7) | O21—Sm1—O10—C9 | 144.6 (2) |
O20—Sm1—O1—C18A | 174.1 (7) | O20—Sm1—O10—C9 | 73.7 (2) |
O16—Sm1—O1—C18A | 19.9 (7) | O16—Sm1—O10—C9 | −144.2 (2) |
O4—Sm1—O1—C18A | −101.7 (8) | O4—Sm1—O10—C9 | 1.2 (3) |
O10—Sm1—O1—C18A | 139.7 (8) | O13—Sm1—O10—C9 | −143.0 (2) |
O13—Sm1—O1—C18A | 41.9 (8) | O7—Sm1—O10—C9 | 0.9 (2) |
O7—Sm1—O1—C18A | −124.9 (7) | O1—Sm1—O10—C9 | 107.7 (3) |
O19—Sm1—O1—C2 | 46.4 (2) | C9—O10—C11—C12 | 175.4 (3) |
O21—Sm1—O1—C2 | −169.4 (2) | Sm1—O10—C11—C12 | 29.6 (4) |
O20—Sm1—O1—C2 | −97.5 (2) | O10—C11—C12—O13 | −52.7 (4) |
O16—Sm1—O1—C2 | 108.2 (2) | C11—C12—O13—C14 | −162.5 (3) |
O4—Sm1—O1—C2 | −13.4 (2) | C11—C12—O13—Sm1 | 55.0 (3) |
O10—Sm1—O1—C2 | −132.0 (3) | O19—Sm1—O13—C12 | −128.5 (2) |
O13—Sm1—O1—C2 | 130.2 (2) | O21—Sm1—O13—C12 | 63.3 (2) |
O7—Sm1—O1—C2 | −36.6 (3) | O20—Sm1—O13—C12 | 23.0 (2) |
C2A—O1—C2—C3 | −61.7 (6) | O16—Sm1—O13—C12 | 149.6 (2) |
C18—O1—C2—C3 | 173.5 (3) | O4—Sm1—O13—C12 | −144.7 (2) |
C18A—O1—C2—C3 | 153.1 (8) | O10—Sm1—O13—C12 | −29.4 (2) |
Sm1—O1—C2—C3 | 38.5 (4) | O7—Sm1—O13—C12 | −64.9 (2) |
C18—O1—C2A—C3 | 135.7 (7) | O1—Sm1—O13—C12 | 127.6 (2) |
C18A—O1—C2A—C3 | 95.1 (13) | O19—Sm1—O13—C14 | 91.8 (2) |
C2—O1—C2A—C3 | 59.3 (6) | O21—Sm1—O13—C14 | −76.4 (2) |
Sm1—O1—C2A—C3 | −41.9 (12) | O20—Sm1—O13—C14 | −116.7 (2) |
O1—C2—C3—O4 | −48.3 (4) | O16—Sm1—O13—C14 | 9.9 (2) |
O1—C2—C3—C2A | 58.8 (6) | O4—Sm1—O13—C14 | 75.6 (3) |
O1—C2A—C3—O4 | 26.5 (13) | O10—Sm1—O13—C14 | −169.0 (2) |
O1—C2A—C3—C2 | −61.2 (7) | O7—Sm1—O13—C14 | 155.4 (2) |
C2—C3—O4—C5 | −157.6 (3) | O1—Sm1—O13—C14 | −12.0 (2) |
C2A—C3—O4—C5 | 162.5 (7) | C12—O13—C14—C15 | −178.3 (3) |
C2—C3—O4—Sm1 | 40.7 (4) | Sm1—O13—C14—C15 | −37.8 (3) |
C2A—C3—O4—Sm1 | 0.8 (7) | O13—C14—C15—O16 | 53.8 (3) |
O19—Sm1—O4—C3 | −138.3 (3) | C14—C15—O16—C17 | 130.8 (3) |
O21—Sm1—O4—C3 | 18.7 (3) | C14—C15—O16—Sm1 | −50.8 (3) |
O20—Sm1—O4—C3 | 67.2 (3) | O19—Sm1—O16—C17 | 121.3 (3) |
O16—Sm1—O4—C3 | −66.3 (3) | O21—Sm1—O16—C17 | −83.9 (2) |
O10—Sm1—O4—C3 | 141.8 (2) | O20—Sm1—O16—C17 | −36.6 (3) |
O13—Sm1—O4—C3 | −122.2 (3) | O4—Sm1—O16—C17 | 50.1 (3) |
O7—Sm1—O4—C3 | 142.0 (3) | O10—Sm1—O16—C17 | −157.9 (2) |
O1—Sm1—O4—C3 | −15.8 (2) | O13—Sm1—O16—C17 | −159.1 (3) |
O19—Sm1—O4—C5 | 60.3 (2) | O7—Sm1—O16—C17 | 105.8 (3) |
O21—Sm1—O4—C5 | −142.6 (2) | O1—Sm1—O16—C17 | 0.1 (2) |
O20—Sm1—O4—C5 | −94.1 (2) | O19—Sm1—O16—C15 | −56.8 (2) |
O16—Sm1—O4—C5 | 132.4 (2) | O21—Sm1—O16—C15 | 97.9 (2) |
O10—Sm1—O4—C5 | −19.5 (3) | O20—Sm1—O16—C15 | 145.26 (19) |
O13—Sm1—O4—C5 | 76.5 (3) | O4—Sm1—O16—C15 | −128.0 (2) |
O7—Sm1—O4—C5 | −19.3 (2) | O10—Sm1—O16—C15 | 24.0 (2) |
O1—Sm1—O4—C5 | −177.1 (3) | O13—Sm1—O16—C15 | 22.8 (2) |
C3—O4—C5—C6 | −115.2 (3) | O7—Sm1—O16—C15 | −72.3 (2) |
Sm1—O4—C5—C6 | 47.4 (3) | O1—Sm1—O16—C15 | −178.1 (2) |
O4—C5—C6—O7 | −54.1 (4) | C15—O16—C17—C18A | 160.0 (7) |
C5—C6—O7—C8 | 178.9 (3) | Sm1—O16—C17—C18A | −18.2 (8) |
C5—C6—O7—Sm1 | 40.3 (3) | C15—O16—C17—C18 | −159.5 (3) |
O19—Sm1—O7—C6 | −93.6 (2) | Sm1—O16—C17—C18 | 22.3 (4) |
O21—Sm1—O7—C6 | 114.9 (2) | C2A—O1—C18—C17 | −131.0 (7) |
O20—Sm1—O7—C6 | 74.7 (2) | C18A—O1—C18—C17 | −58.2 (7) |
O16—Sm1—O7—C6 | −77.9 (3) | C2—O1—C18—C17 | −89.8 (4) |
O4—Sm1—O7—C6 | −12.7 (2) | Sm1—O1—C18—C17 | 46.6 (4) |
O10—Sm1—O7—C6 | 167.1 (2) | O16—C17—C18—O1 | −43.5 (4) |
O13—Sm1—O7—C6 | −157.4 (2) | C18A—C17—C18—O1 | 58.4 (7) |
O1—Sm1—O7—C6 | 10.2 (2) | C2A—O1—C18A—C17 | −173.0 (9) |
O19—Sm1—O7—C8 | 128.7 (2) | C18—O1—C18A—C17 | 59.7 (7) |
O21—Sm1—O7—C8 | −22.7 (2) | C2—O1—C18A—C17 | −150.6 (13) |
O20—Sm1—O7—C8 | −62.9 (2) | Sm1—O1—C18A—C17 | −36.5 (15) |
O16—Sm1—O7—C8 | 144.4 (2) | O16—C17—C18A—O1 | 34.1 (14) |
O4—Sm1—O7—C8 | −150.4 (2) | C18—C17—C18A—O1 | −58.3 (7) |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O19—H19A···N21 | 0.87 | 1.85 | 2.717 (4) | 171 |
O19—H19B···O42 | 0.83 | 1.77 | 2.590 (3) | 169 |
O20—H20A···O41 | 0.88 | 1.83 | 2.682 (3) | 163 |
O20—H20B···N33 | 0.88 | 1.88 | 2.745 (3) | 167 |
O21—H21A···O41 | 0.87 | 1.88 | 2.691 (3) | 155 |
O21—H21B···N32iii | 0.87 | 1.87 | 2.737 (3) | 171 |
O41—H41A···N22iv | 0.82 | 1.90 | 2.712 (4) | 170 |
O41—H41B···N33v | 0.80 | 2.42 | 3.099 (4) | 143 |
O42—H42A···N31vi | 0.84 | 2.00 | 2.836 (4) | 175 |
O42—H42B···N23vii | 0.81 | 2.02 | 2.810 (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, z−1; (vii) −x+1, −y+1, −z. |
[Eu(C12H24O6)(H2O)3][Fe(CN)6]·2H2O | Z = 2 |
Mr = 718.32 | F(000) = 722 |
Triclinic, P1 | Dx = 1.703 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.9125 (3) Å | Cell parameters from 6139 reflections |
b = 11.0947 (4) Å | θ = 2.9–27.5° |
c = 14.0119 (3) Å | µ = 2.80 mm−1 |
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 |
Bruker–Nonius KappaCCD diffractometer | 6420 independent reflections |
Radiation source: Bruker–Nonius FR591 rotating anode | 5973 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.060 |
Detector resolution: 9.091 pixels mm-1 | θmax = 27.6°, θmin = 3.2° |
ϕ & ω scans | h = −14→14 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | k = −14→14 |
Tmin = 0.509, Tmax = 0.568 | l = −18→18 |
27604 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.077 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.212 | H-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 parameters | Δρmax = 11.43 e Å−3 |
8 restraints | Δρmin = −3.03 e Å−3 |
[Eu(C12H24O6)(H2O)3][Fe(CN)6]·2H2O | γ = 65.743 (2)° |
Mr = 718.32 | V = 1400.57 (8) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.9125 (3) Å | Mo Kα radiation |
b = 11.0947 (4) Å | µ = 2.80 mm−1 |
c = 14.0119 (3) Å | T = 120 K |
α = 67.8201 (18)° | 0.25 × 0.20 × 0.20 mm |
β = 70.635 (2)° |
Bruker–Nonius KappaCCD diffractometer | 6420 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | 5973 reflections with I > 2σ(I) |
Tmin = 0.509, Tmax = 0.568 | Rint = 0.060 |
27604 measured reflections |
R[F2 > 2σ(F2)] = 0.077 | 8 restraints |
wR(F2) = 0.212 | H-atom parameters constrained |
S = 1.10 | w = 1/[σ2(Fo2) + (0.1382P)2 + 13.515P] where P = (Fo2 + 2Fc2)/3 |
6420 reflections | Δρmax = 11.43 e Å−3 |
334 parameters | Δρmin = −3.03 e Å−3 |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Eu1 | 0.20539 (3) | 0.72823 (3) | 0.27729 (3) | 0.01553 (16) | |
O1 | 0.0592 (5) | 0.5655 (5) | 0.3664 (4) | 0.0218 (11) | |
C2 | 0.0893 (8) | 0.4559 (9) | 0.3237 (9) | 0.0259 (16)* | 0.762 (14) |
C2A | 0.127 (2) | 0.4216 (8) | 0.3832 (15) | 0.0259 (16)* | 0.238 (14) |
C3 | 0.2416 (8) | 0.3962 (9) | 0.2902 (7) | 0.0300 (18) | |
O4 | 0.2905 (6) | 0.5068 (6) | 0.2306 (6) | 0.0311 (14) | |
C5 | 0.4213 (9) | 0.4752 (9) | 0.1589 (7) | 0.0282 (18) | |
C6 | 0.5221 (8) | 0.4978 (8) | 0.1952 (7) | 0.0275 (17) | |
O7 | 0.4628 (5) | 0.6361 (6) | 0.2037 (5) | 0.0211 (11) | |
C8 | 0.5477 (8) | 0.6701 (9) | 0.2423 (8) | 0.0290 (18) | |
C9 | 0.4951 (8) | 0.8258 (9) | 0.2178 (8) | 0.0288 (18) | |
O10 | 0.3486 (6) | 0.8667 (6) | 0.2602 (5) | 0.0228 (11) | |
C11 | 0.2960 (10) | 1.0171 (9) | 0.2273 (8) | 0.0310 (19) | |
C12 | 0.1435 (10) | 1.0622 (9) | 0.2626 (8) | 0.0296 (18) | |
O13 | 0.0968 (6) | 0.9897 (5) | 0.2235 (5) | 0.0226 (11) | |
C14 | −0.0479 (8) | 1.0508 (8) | 0.2224 (7) | 0.0253 (16) | |
C15 | −0.0800 (8) | 0.9618 (8) | 0.1843 (8) | 0.0282 (17) | |
O16 | −0.0321 (6) | 0.8222 (6) | 0.2500 (5) | 0.0241 (12) | |
C17 | −0.1290 (9) | 0.7506 (9) | 0.2938 (7) | 0.0313 (19) | |
C18 | −0.0847 (7) | 0.6349 (9) | 0.3882 (7) | 0.0259 (16)* | 0.762 (14) |
C18A | −0.059 (2) | 0.5983 (11) | 0.327 (3) | 0.0259 (16)* | 0.238 (14) |
O19 | 0.2303 (6) | 0.7931 (6) | 0.0959 (4) | 0.0227 (11) | |
O20 | 0.3152 (6) | 0.5729 (6) | 0.4218 (4) | 0.0219 (11) | |
O21 | 0.0804 (5) | 0.8001 (6) | 0.4333 (4) | 0.0205 (11) | |
Fe2 | 0.0000 | 0.5000 | 0.0000 | 0.0155 (3) | |
N21 | 0.0612 (9) | 0.7267 (8) | 0.0339 (6) | 0.0339 (17) | |
N22 | 0.1326 (8) | 0.5989 (8) | −0.2346 (6) | 0.0277 (15) | |
N23 | 0.2921 (9) | 0.3135 (9) | 0.0374 (8) | 0.044 (2) | |
C21 | 0.0342 (8) | 0.6443 (8) | 0.0230 (6) | 0.0225 (15) | |
C22 | 0.0817 (8) | 0.5612 (8) | −0.1470 (6) | 0.0196 (14) | |
C23 | 0.1811 (8) | 0.3802 (9) | 0.0255 (7) | 0.0253 (16) | |
Fe3 | 0.5000 | 0.0000 | 0.5000 | 0.0152 (3) | |
N31 | 0.4322 (8) | −0.1000 (8) | 0.7428 (6) | 0.0284 (15) | |
N32 | 0.1927 (7) | 0.0800 (8) | 0.4979 (6) | 0.0290 (16) | |
N33 | 0.4469 (8) | 0.2961 (7) | 0.4965 (6) | 0.0295 (16) | |
C31 | 0.4560 (7) | −0.0630 (8) | 0.6526 (6) | 0.0206 (15) | |
C32 | 0.3083 (8) | 0.0495 (8) | 0.4980 (6) | 0.0205 (14) | |
C33 | 0.4673 (8) | 0.1848 (8) | 0.5000 (6) | 0.0209 (15) | |
O41 | 0.2521 (6) | 0.7052 (6) | 0.5656 (4) | 0.0255 (12) | |
O42 | 0.4345 (6) | 0.8559 (7) | −0.0449 (5) | 0.0327 (14) | |
H2A | 0.0458 | 0.4910 | 0.2624 | 0.031* | 0.762 (14) |
H2B | 0.0521 | 0.3838 | 0.3774 | 0.031* | 0.762 (14) |
H2C | 0.0606 | 0.3762 | 0.3922 | 0.031* | 0.238 (14) |
H2D | 0.1638 | 0.3824 | 0.4481 | 0.031* | 0.238 (14) |
H3A | 0.2839 | 0.3435 | 0.3527 | 0.036* | 0.762 (14) |
H3B | 0.2643 | 0.3335 | 0.2474 | 0.036* | 0.762 (14) |
H3C | 0.3190 | 0.3156 | 0.3158 | 0.036* | 0.238 (14) |
H3D | 0.2096 | 0.3722 | 0.2436 | 0.036* | 0.238 (14) |
H5A | 0.4130 | 0.5355 | 0.0867 | 0.034* | |
H5B | 0.4527 | 0.3782 | 0.1579 | 0.034* | |
H6A | 0.5380 | 0.4313 | 0.2643 | 0.033* | |
H6B | 0.6109 | 0.4861 | 0.1438 | 0.033* | |
H8A | 0.6452 | 0.6376 | 0.2067 | 0.035* | |
H8B | 0.5399 | 0.6270 | 0.3192 | 0.035* | |
H9A | 0.5411 | 0.8559 | 0.2505 | 0.035* | |
H9B | 0.5140 | 0.8683 | 0.1406 | 0.035* | |
H11A | 0.3217 | 1.0517 | 0.1497 | 0.037* | |
H11B | 0.3360 | 1.0545 | 0.2592 | 0.037* | |
H12A | 0.1169 | 1.0388 | 0.3405 | 0.035* | |
H12B | 0.1033 | 1.1630 | 0.2335 | 0.035* | |
H14A | −0.0681 | 1.1457 | 0.1747 | 0.030* | |
H14B | −0.1030 | 1.0540 | 0.2941 | 0.030* | |
H15A | −0.1803 | 0.9915 | 0.1895 | 0.034* | |
H15B | −0.0331 | 0.9676 | 0.1097 | 0.034* | |
H17A | −0.1324 | 0.7134 | 0.2410 | 0.038* | 0.762 (14) |
H17B | −0.2217 | 0.8138 | 0.3151 | 0.038* | 0.762 (14) |
H17C | −0.1822 | 0.7727 | 0.2408 | 0.038* | 0.238 (14) |
H17D | −0.1940 | 0.7812 | 0.3553 | 0.038* | 0.238 (14) |
H18A | −0.1088 | 0.6722 | 0.4484 | 0.031* | 0.762 (14) |
H18B | −0.1342 | 0.5687 | 0.4082 | 0.031* | 0.762 (14) |
H18C | −0.1238 | 0.5543 | 0.3831 | 0.031* | 0.238 (14) |
H18D | −0.0310 | 0.5609 | 0.2667 | 0.031* | 0.238 (14) |
H19A | 0.1791 | 0.7763 | 0.0692 | 0.045 (11)* | |
H19B | 0.2954 | 0.8062 | 0.0470 | 0.045 (11)* | |
H20A | 0.3077 | 0.6016 | 0.4747 | 0.045 (11)* | |
H20B | 0.3668 | 0.4860 | 0.4370 | 0.045 (11)* | |
H21A | 0.1171 | 0.7889 | 0.4836 | 0.045 (11)* | |
H21B | −0.0054 | 0.8465 | 0.4530 | 0.045 (11)* | |
H41A | 0.2205 | 0.6766 | 0.6286 | 0.045 (11)* | |
H41B | 0.3101 | 0.7339 | 0.5632 | 0.045 (11)* | |
H42A | 0.4291 | 0.8685 | −0.1065 | 0.045 (11)* | |
H42B | 0.5088 | 0.7960 | −0.0425 | 0.045 (11)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Eu1 | 0.0163 (2) | 0.0170 (2) | 0.0140 (2) | −0.00982 (16) | −0.00108 (14) | −0.00214 (14) |
O1 | 0.025 (3) | 0.025 (3) | 0.020 (3) | −0.018 (2) | 0.000 (2) | −0.003 (2) |
C3 | 0.042 (5) | 0.023 (4) | 0.028 (4) | −0.019 (4) | −0.001 (4) | −0.006 (3) |
O4 | 0.026 (3) | 0.026 (3) | 0.046 (4) | −0.015 (2) | 0.006 (3) | −0.019 (3) |
C5 | 0.028 (4) | 0.028 (4) | 0.033 (4) | −0.015 (3) | 0.006 (3) | −0.017 (4) |
C6 | 0.019 (4) | 0.022 (4) | 0.037 (5) | −0.003 (3) | 0.001 (3) | −0.012 (3) |
O7 | 0.017 (2) | 0.022 (3) | 0.026 (3) | −0.009 (2) | −0.002 (2) | −0.008 (2) |
C8 | 0.016 (3) | 0.033 (4) | 0.042 (5) | −0.008 (3) | −0.005 (3) | −0.016 (4) |
C9 | 0.019 (4) | 0.033 (4) | 0.041 (5) | −0.018 (3) | 0.000 (3) | −0.014 (4) |
O10 | 0.019 (3) | 0.019 (3) | 0.034 (3) | −0.014 (2) | −0.002 (2) | −0.007 (2) |
C11 | 0.034 (5) | 0.022 (4) | 0.042 (5) | −0.018 (4) | −0.008 (4) | −0.004 (4) |
C12 | 0.032 (4) | 0.021 (4) | 0.038 (5) | −0.008 (3) | −0.009 (4) | −0.010 (3) |
O13 | 0.022 (3) | 0.017 (2) | 0.029 (3) | −0.007 (2) | −0.007 (2) | −0.005 (2) |
C14 | 0.020 (4) | 0.015 (3) | 0.033 (4) | −0.002 (3) | −0.008 (3) | −0.001 (3) |
C15 | 0.020 (4) | 0.022 (4) | 0.036 (5) | −0.002 (3) | −0.011 (3) | −0.002 (3) |
O16 | 0.018 (3) | 0.019 (3) | 0.035 (3) | −0.010 (2) | −0.009 (2) | 0.001 (2) |
C17 | 0.021 (4) | 0.044 (5) | 0.028 (4) | −0.018 (4) | −0.003 (3) | −0.002 (4) |
O19 | 0.021 (3) | 0.034 (3) | 0.015 (2) | −0.015 (2) | 0.000 (2) | −0.006 (2) |
O20 | 0.029 (3) | 0.020 (2) | 0.014 (2) | −0.009 (2) | −0.007 (2) | −0.001 (2) |
O21 | 0.017 (2) | 0.026 (3) | 0.018 (3) | −0.007 (2) | −0.003 (2) | −0.007 (2) |
Fe2 | 0.0163 (7) | 0.0181 (7) | 0.0139 (7) | −0.0113 (6) | −0.0022 (5) | −0.0008 (5) |
N21 | 0.049 (5) | 0.033 (4) | 0.028 (4) | −0.022 (4) | −0.010 (3) | −0.006 (3) |
N22 | 0.030 (4) | 0.033 (4) | 0.020 (3) | −0.016 (3) | −0.001 (3) | −0.005 (3) |
N23 | 0.027 (4) | 0.036 (4) | 0.053 (6) | −0.004 (3) | −0.014 (4) | 0.001 (4) |
C21 | 0.027 (4) | 0.027 (4) | 0.015 (3) | −0.015 (3) | −0.002 (3) | −0.002 (3) |
C22 | 0.021 (3) | 0.022 (3) | 0.020 (4) | −0.013 (3) | −0.004 (3) | −0.003 (3) |
C23 | 0.020 (4) | 0.027 (4) | 0.029 (4) | −0.010 (3) | −0.003 (3) | −0.006 (3) |
Fe3 | 0.0134 (6) | 0.0155 (6) | 0.0154 (7) | −0.0077 (5) | −0.0008 (5) | −0.0016 (5) |
N31 | 0.027 (3) | 0.035 (4) | 0.017 (3) | −0.009 (3) | −0.004 (3) | −0.003 (3) |
N32 | 0.019 (3) | 0.036 (4) | 0.029 (4) | −0.008 (3) | −0.005 (3) | −0.008 (3) |
N33 | 0.034 (4) | 0.022 (3) | 0.029 (4) | −0.009 (3) | −0.006 (3) | −0.005 (3) |
C31 | 0.014 (3) | 0.019 (3) | 0.026 (4) | −0.008 (3) | −0.002 (3) | −0.003 (3) |
C32 | 0.021 (4) | 0.023 (3) | 0.017 (3) | −0.014 (3) | 0.001 (3) | −0.002 (3) |
C33 | 0.018 (3) | 0.023 (4) | 0.018 (3) | −0.007 (3) | −0.002 (3) | −0.003 (3) |
O41 | 0.028 (3) | 0.037 (3) | 0.017 (3) | −0.022 (3) | 0.000 (2) | −0.004 (2) |
O42 | 0.023 (3) | 0.050 (4) | 0.018 (3) | −0.014 (3) | −0.003 (2) | −0.001 (3) |
Eu1—O19 | 2.318 (5) | C14—C15 | 1.479 (12) |
Eu1—O21 | 2.392 (5) | C14—H14A | 0.99 |
Eu1—O20 | 2.405 (5) | C14—H14B | 0.99 |
Eu1—O16 | 2.467 (5) | C15—O16 | 1.448 (10) |
Eu1—O4 | 2.502 (6) | C15—H15A | 0.99 |
Eu1—O10 | 2.511 (5) | C15—H15B | 0.99 |
Eu1—O13 | 2.550 (5) | O16—C17 | 1.421 (10) |
Eu1—O7 | 2.553 (5) | C17—C18A | 1.496 (5) |
Eu1—O1 | 2.590 (5) | C17—C18 | 1.505 (5) |
O1—C2A | 1.418 (5) | C17—H17A | 0.99 |
O1—C18A | 1.420 (5) | C17—H17B | 0.99 |
O1—C18 | 1.420 (5) | C17—H17C | 0.99 |
O1—C2 | 1.427 (5) | C17—H17D | 0.99 |
C2—C3 | 1.495 (5) | C18—H18A | 0.99 |
C2—H2A | 0.99 | C18—H18B | 0.99 |
C2—H2B | 0.99 | C18A—H18C | 0.99 |
C2A—C3 | 1.501 (5) | C18A—H18D | 0.99 |
C2A—H2C | 0.99 | O19—H19A | 0.87 |
C2A—H2D | 0.99 | O19—H19B | 0.82 |
C3—O4 | 1.399 (10) | O20—H20A | 0.88 |
C3—H3A | 0.99 | O20—H20B | 0.88 |
C3—H3B | 0.99 | O21—H21A | 0.87 |
C3—H3C | 0.99 | O21—H21B | 0.87 |
C3—H3D | 0.99 | Fe2—C22 | 1.929 (8) |
O4—C5 | 1.440 (10) | Fe2—C22i | 1.929 (8) |
C5—C6 | 1.491 (12) | Fe2—C23 | 1.936 (8) |
C5—H5A | 0.99 | Fe2—C23i | 1.936 (8) |
C5—H5B | 0.99 | Fe2—C21 | 1.941 (8) |
C6—O7 | 1.435 (9) | Fe2—C21i | 1.941 (8) |
C6—H6A | 0.99 | N21—C21 | 1.141 (11) |
C6—H6B | 0.99 | N22—C22 | 1.159 (11) |
O7—C8 | 1.437 (10) | N23—C23 | 1.161 (12) |
C8—C9 | 1.516 (12) | Fe3—C33 | 1.932 (8) |
C8—H8A | 0.99 | Fe3—C33ii | 1.932 (8) |
C8—H8B | 0.99 | Fe3—C31ii | 1.939 (8) |
C9—O10 | 1.446 (10) | Fe3—C31 | 1.939 (8) |
C9—H9A | 0.99 | Fe3—C32ii | 1.940 (8) |
C9—H9B | 0.99 | Fe3—C32 | 1.940 (8) |
O10—C11 | 1.461 (10) | N31—C31 | 1.144 (11) |
C11—C12 | 1.490 (13) | N32—C32 | 1.164 (11) |
C11—H11A | 0.99 | N33—C33 | 1.145 (11) |
C11—H11B | 0.99 | O41—H41A | 0.82 |
C12—O13 | 1.437 (10) | O41—H41B | 0.80 |
C12—H12A | 0.99 | O42—H42A | 0.84 |
C12—H12B | 0.99 | O42—H42B | 0.81 |
O13—C14 | 1.443 (9) | ||
O19—Eu1—O21 | 144.10 (19) | O10—C11—H11A | 110.0 |
O19—Eu1—O20 | 144.23 (19) | C12—C11—H11A | 110.0 |
O21—Eu1—O20 | 70.55 (18) | O10—C11—H11B | 110.0 |
O19—Eu1—O16 | 75.7 (2) | C12—C11—H11B | 110.0 |
O21—Eu1—O16 | 78.9 (2) | H11A—C11—H11B | 108.4 |
O20—Eu1—O16 | 134.7 (2) | O13—C12—C11 | 105.8 (7) |
O19—Eu1—O4 | 75.2 (2) | O13—C12—H12A | 110.6 |
O21—Eu1—O4 | 135.0 (2) | C11—C12—H12A | 110.6 |
O20—Eu1—O4 | 79.8 (2) | O13—C12—H12B | 110.6 |
O16—Eu1—O4 | 100.8 (2) | C11—C12—H12B | 110.6 |
O19—Eu1—O10 | 91.0 (2) | H12A—C12—H12B | 108.7 |
O21—Eu1—O10 | 83.71 (19) | C12—O13—C14 | 112.8 (6) |
O20—Eu1—O10 | 83.59 (19) | C12—O13—Eu1 | 115.2 (5) |
O16—Eu1—O10 | 125.90 (18) | C14—O13—Eu1 | 119.8 (4) |
O4—Eu1—O10 | 126.37 (19) | O13—C14—C15 | 105.9 (6) |
O19—Eu1—O13 | 74.3 (2) | O13—C14—H14A | 110.6 |
O21—Eu1—O13 | 71.67 (19) | C15—C14—H14A | 110.6 |
O20—Eu1—O13 | 131.53 (19) | O13—C14—H14B | 110.6 |
O16—Eu1—O13 | 62.85 (18) | C15—C14—H14B | 110.6 |
O4—Eu1—O13 | 148.2 (2) | H14A—C14—H14B | 108.7 |
O10—Eu1—O13 | 63.05 (18) | O16—C15—C14 | 107.2 (7) |
O19—Eu1—O7 | 74.26 (19) | O16—C15—H15A | 110.3 |
O21—Eu1—O7 | 131.67 (18) | C14—C15—H15A | 110.3 |
O20—Eu1—O7 | 71.84 (19) | O16—C15—H15B | 110.3 |
O16—Eu1—O7 | 148.8 (2) | C14—C15—H15B | 110.3 |
O4—Eu1—O7 | 63.50 (19) | H15A—C15—H15B | 108.5 |
O10—Eu1—O7 | 62.88 (18) | C17—O16—C15 | 115.8 (6) |
O13—Eu1—O7 | 115.53 (18) | C17—O16—Eu1 | 125.5 (4) |
O19—Eu1—O1 | 109.97 (19) | C15—O16—Eu1 | 118.8 (5) |
O21—Eu1—O1 | 79.60 (18) | O16—C17—C18A | 111.0 (11) |
O20—Eu1—O1 | 78.89 (18) | O16—C17—C18 | 108.0 (7) |
O16—Eu1—O1 | 63.06 (17) | O16—C17—H17A | 110.1 |
O4—Eu1—O1 | 61.65 (18) | C18—C17—H17A | 110.1 |
O10—Eu1—O1 | 158.99 (19) | O16—C17—H17B | 110.1 |
O13—Eu1—O1 | 122.21 (17) | C18—C17—H17B | 110.1 |
O7—Eu1—O1 | 121.04 (17) | H17A—C17—H17B | 108.4 |
C2A—O1—C18A | 106.6 (16) | O16—C17—H17C | 109.4 |
C18—O1—C2 | 110.7 (7) | C18A—C17—H17C | 109.4 |
C2A—O1—Eu1 | 118.8 (10) | O16—C17—H17D | 109.4 |
C18A—O1—Eu1 | 118.0 (10) | C18A—C17—H17D | 109.4 |
C18—O1—Eu1 | 114.0 (5) | H17C—C17—H17D | 108.0 |
C2—O1—Eu1 | 118.5 (5) | O1—C18—C17 | 111.0 (7) |
O1—C2—C3 | 109.0 (6) | O1—C18—H18A | 109.4 |
O1—C2—H2A | 109.9 | C17—C18—H18A | 109.4 |
C3—C2—H2A | 109.9 | O1—C18—H18B | 109.4 |
O1—C2—H2B | 109.9 | C17—C18—H18B | 109.4 |
C3—C2—H2B | 109.9 | H18A—C18—H18B | 108.0 |
H2A—C2—H2B | 108.3 | O1—C18A—C17 | 111.5 (8) |
O1—C2A—C3 | 109.2 (7) | O1—C18A—H18C | 109.3 |
O1—C2A—H2C | 109.8 | C17—C18A—H18C | 109.3 |
C3—C2A—H2C | 109.8 | O1—C18A—H18D | 109.3 |
O1—C2A—H2D | 109.8 | C17—C18A—H18D | 109.3 |
C3—C2A—H2D | 109.8 | H18C—C18A—H18D | 108.0 |
H2C—C2A—H2D | 108.3 | Eu1—O19—H19A | 119.4 |
O4—C3—C2 | 106.9 (7) | Eu1—O19—H19B | 131.9 |
O4—C3—C2A | 115.1 (9) | H19A—O19—H19B | 105.2 |
O4—C3—H3A | 110.3 | Eu1—O20—H20A | 120.3 |
C2—C3—H3A | 110.3 | Eu1—O20—H20B | 134.6 |
O4—C3—H3B | 110.3 | H20A—O20—H20B | 105.1 |
C2—C3—H3B | 110.3 | Eu1—O21—H21A | 124.6 |
H3A—C3—H3B | 108.6 | Eu1—O21—H21B | 132.3 |
O4—C3—H3C | 108.5 | H21A—O21—H21B | 103.0 |
C2A—C3—H3C | 108.5 | C22—Fe2—C22i | 180.0 (5) |
O4—C3—H3D | 108.5 | C22—Fe2—C23 | 88.9 (3) |
C2A—C3—H3D | 108.5 | C22i—Fe2—C23 | 91.1 (3) |
H3C—C3—H3D | 107.5 | C22—Fe2—C23i | 91.1 (3) |
C3—O4—C5 | 116.1 (6) | C22i—Fe2—C23i | 88.9 (3) |
C3—O4—Eu1 | 123.7 (5) | C23—Fe2—C23i | 180.0 (6) |
C5—O4—Eu1 | 117.6 (5) | C22—Fe2—C21 | 88.1 (3) |
O4—C5—C6 | 108.2 (7) | C22i—Fe2—C21 | 91.9 (3) |
O4—C5—H5A | 110.1 | C23—Fe2—C21 | 88.0 (4) |
C6—C5—H5A | 110.1 | C23i—Fe2—C21 | 92.0 (4) |
O4—C5—H5B | 110.1 | C22—Fe2—C21i | 91.9 (3) |
C6—C5—H5B | 110.1 | C22i—Fe2—C21i | 88.1 (3) |
H5A—C5—H5B | 108.4 | C23—Fe2—C21i | 92.0 (4) |
O7—C6—C5 | 106.3 (7) | C23i—Fe2—C21i | 88.0 (4) |
O7—C6—H6A | 110.5 | C21—Fe2—C21i | 180.0 (4) |
C5—C6—H6A | 110.5 | N21—C21—Fe2 | 176.4 (8) |
O7—C6—H6B | 110.5 | N22—C22—Fe2 | 178.5 (7) |
C5—C6—H6B | 110.5 | N23—C23—Fe2 | 176.7 (8) |
H6A—C6—H6B | 108.7 | C33—Fe3—C33ii | 180.0 (5) |
C6—O7—C8 | 112.2 (6) | C33—Fe3—C31ii | 87.5 (3) |
C6—O7—Eu1 | 119.0 (5) | C33ii—Fe3—C31ii | 92.5 (3) |
C8—O7—Eu1 | 114.7 (5) | C33—Fe3—C31 | 92.5 (3) |
O7—C8—C9 | 105.9 (7) | C33ii—Fe3—C31 | 87.5 (3) |
O7—C8—H8A | 110.6 | C31ii—Fe3—C31 | 180.000 (1) |
C9—C8—H8A | 110.6 | C33—Fe3—C32ii | 90.2 (3) |
O7—C8—H8B | 110.6 | C33ii—Fe3—C32ii | 89.8 (3) |
C9—C8—H8B | 110.6 | C31ii—Fe3—C32ii | 89.6 (3) |
H8A—C8—H8B | 108.7 | C31—Fe3—C32ii | 90.4 (3) |
O10—C9—C8 | 107.3 (6) | C33—Fe3—C32 | 89.8 (3) |
O10—C9—H9A | 110.3 | C33ii—Fe3—C32 | 90.2 (3) |
C8—C9—H9A | 110.3 | C31ii—Fe3—C32 | 90.4 (3) |
O10—C9—H9B | 110.3 | C31—Fe3—C32 | 89.6 (3) |
C8—C9—H9B | 110.2 | C32ii—Fe3—C32 | 180.0 (5) |
H9A—C9—H9B | 108.5 | N31—C31—Fe3 | 178.8 (7) |
C9—O10—C11 | 107.2 (6) | N32—C32—Fe3 | 179.1 (8) |
C9—O10—Eu1 | 122.0 (5) | N33—C33—Fe3 | 177.6 (7) |
C11—O10—Eu1 | 120.7 (5) | H41A—O41—H41B | 105.5 |
O10—C11—C12 | 108.5 (7) | H42A—O42—H42B | 100.3 |
O19—Eu1—O1—C2A | 89.4 (14) | O10—Eu1—O7—C8 | 30.2 (5) |
O21—Eu1—O1—C2A | −126.6 (14) | O13—Eu1—O7—C8 | 66.2 (6) |
O20—Eu1—O1—C2A | −54.5 (14) | O1—Eu1—O7—C8 | −126.1 (5) |
O16—Eu1—O1—C2A | 150.7 (14) | C6—O7—C8—C9 | 164.2 (7) |
O4—Eu1—O1—C2A | 29.8 (14) | Eu1—O7—C8—C9 | −55.9 (8) |
O10—Eu1—O1—C2A | −88.6 (15) | O7—C8—C9—O10 | 52.6 (9) |
O13—Eu1—O1—C2A | 173.0 (14) | C8—C9—O10—C11 | −174.4 (7) |
O7—Eu1—O1—C2A | 6.2 (14) | C8—C9—O10—Eu1 | −29.0 (9) |
O19—Eu1—O1—C18A | −42.1 (14) | O19—Eu1—O10—C9 | −70.6 (6) |
O21—Eu1—O1—C18A | 102.0 (14) | O21—Eu1—O10—C9 | 145.0 (6) |
O20—Eu1—O1—C18A | 174.0 (14) | O20—Eu1—O10—C9 | 74.0 (6) |
O16—Eu1—O1—C18A | 19.2 (14) | O16—Eu1—O10—C9 | −143.6 (6) |
O4—Eu1—O1—C18A | −101.7 (14) | O4—Eu1—O10—C9 | 1.7 (7) |
O10—Eu1—O1—C18A | 139.9 (14) | O13—Eu1—O10—C9 | −142.4 (7) |
O13—Eu1—O1—C18A | 41.5 (14) | O7—Eu1—O10—C9 | 1.1 (6) |
O7—Eu1—O1—C18A | −125.3 (14) | O1—Eu1—O10—C9 | 107.5 (7) |
O19—Eu1—O1—C18 | −87.4 (5) | O19—Eu1—O10—C11 | 70.4 (6) |
O21—Eu1—O1—C18 | 56.6 (5) | O21—Eu1—O10—C11 | −74.0 (6) |
O20—Eu1—O1—C18 | 128.6 (5) | O20—Eu1—O10—C11 | −145.1 (6) |
O16—Eu1—O1—C18 | −26.1 (5) | O16—Eu1—O10—C11 | −2.6 (7) |
O4—Eu1—O1—C18 | −147.1 (6) | O4—Eu1—O10—C11 | 142.6 (6) |
O10—Eu1—O1—C18 | 94.6 (7) | O13—Eu1—O10—C11 | −1.4 (6) |
O13—Eu1—O1—C18 | −3.8 (6) | O7—Eu1—O10—C11 | 142.1 (7) |
O7—Eu1—O1—C18 | −170.7 (5) | O1—Eu1—O10—C11 | −111.6 (7) |
O19—Eu1—O1—C2 | 45.6 (6) | C9—O10—C11—C12 | 175.6 (8) |
O21—Eu1—O1—C2 | −170.3 (6) | Eu1—O10—C11—C12 | 29.6 (10) |
O20—Eu1—O1—C2 | −98.3 (6) | O10—C11—C12—O13 | −52.6 (10) |
O16—Eu1—O1—C2 | 106.9 (6) | C11—C12—O13—C14 | −162.3 (7) |
O4—Eu1—O1—C2 | −14.0 (6) | C11—C12—O13—Eu1 | 55.2 (8) |
O10—Eu1—O1—C2 | −132.3 (6) | O19—Eu1—O13—C12 | −128.9 (6) |
O13—Eu1—O1—C2 | 129.3 (6) | O21—Eu1—O13—C12 | 62.7 (6) |
O7—Eu1—O1—C2 | −37.6 (6) | O20—Eu1—O13—C12 | 22.4 (6) |
C2A—O1—C2—C3 | −62.3 (12) | O16—Eu1—O13—C12 | 149.4 (6) |
C18A—O1—C2—C3 | 153.2 (16) | O4—Eu1—O13—C12 | −145.8 (6) |
C18—O1—C2—C3 | 173.5 (7) | O10—Eu1—O13—C12 | −29.5 (5) |
Eu1—O1—C2—C3 | 38.9 (10) | O7—Eu1—O13—C12 | −65.4 (6) |
C18A—O1—C2A—C3 | 98 (3) | O1—Eu1—O13—C12 | 127.1 (5) |
C18—O1—C2A—C3 | 137.8 (14) | O19—Eu1—O13—C14 | 91.4 (6) |
C2—O1—C2A—C3 | 61.9 (12) | O21—Eu1—O13—C14 | −77.0 (6) |
Eu1—O1—C2A—C3 | −39 (3) | O20—Eu1—O13—C14 | −117.3 (6) |
O1—C2—C3—O4 | −48.5 (10) | O16—Eu1—O13—C14 | 9.7 (5) |
O1—C2—C3—C2A | 61.1 (12) | O4—Eu1—O13—C14 | 74.6 (7) |
O1—C2A—C3—O4 | 23 (3) | O10—Eu1—O13—C14 | −169.2 (6) |
O1—C2A—C3—C2 | −61.9 (13) | O7—Eu1—O13—C14 | 154.9 (5) |
C2—C3—O4—C5 | −157.6 (8) | O1—Eu1—O13—C14 | −12.6 (6) |
C2A—C3—O4—C5 | 164.5 (16) | C12—O13—C14—C15 | −178.0 (7) |
C2—C3—O4—Eu1 | 41.1 (9) | Eu1—O13—C14—C15 | −37.4 (8) |
C2A—C3—O4—Eu1 | 3.2 (17) | O13—C14—C15—O16 | 53.2 (8) |
O19—Eu1—O4—C3 | −139.4 (7) | C14—C15—O16—C17 | 129.4 (8) |
O21—Eu1—O4—C3 | 17.6 (8) | C14—C15—O16—Eu1 | −50.6 (8) |
O20—Eu1—O4—C3 | 66.4 (7) | O19—Eu1—O16—C17 | 123.1 (7) |
O16—Eu1—O4—C3 | −67.5 (7) | O21—Eu1—O16—C17 | −82.5 (7) |
O10—Eu1—O4—C3 | 140.5 (6) | O20—Eu1—O16—C17 | −34.7 (8) |
O13—Eu1—O4—C3 | −122.6 (7) | O4—Eu1—O16—C17 | 51.6 (7) |
O7—Eu1—O4—C3 | 141.1 (7) | O10—Eu1—O16—C17 | −156.3 (6) |
O1—Eu1—O4—C3 | −16.4 (6) | O13—Eu1—O16—C17 | −157.5 (7) |
O19—Eu1—O4—C5 | 59.6 (6) | O7—Eu1—O16—C17 | 107.5 (7) |
O21—Eu1—O4—C5 | −143.4 (6) | O1—Eu1—O16—C17 | 1.4 (6) |
O20—Eu1—O4—C5 | −94.6 (7) | O19—Eu1—O16—C15 | −57.0 (6) |
O16—Eu1—O4—C5 | 131.5 (6) | O21—Eu1—O16—C15 | 97.4 (6) |
O10—Eu1—O4—C5 | −20.4 (7) | O20—Eu1—O16—C15 | 145.2 (6) |
O13—Eu1—O4—C5 | 76.4 (7) | O4—Eu1—O16—C15 | −128.5 (6) |
O7—Eu1—O4—C5 | −19.9 (6) | O10—Eu1—O16—C15 | 23.6 (7) |
O1—Eu1—O4—C5 | −177.4 (7) | O13—Eu1—O16—C15 | 22.4 (6) |
C3—O4—C5—C6 | −114.3 (8) | O7—Eu1—O16—C15 | −72.6 (7) |
Eu1—O4—C5—C6 | 48.1 (9) | O1—Eu1—O16—C15 | −178.7 (6) |
O4—C5—C6—O7 | −54.4 (9) | C15—O16—C17—C18A | 160.5 (14) |
C5—C6—O7—C8 | 177.7 (7) | Eu1—O16—C17—C18A | −19.6 (16) |
C5—C6—O7—Eu1 | 39.7 (8) | C15—O16—C17—C18 | −158.8 (8) |
O19—Eu1—O7—C6 | −93.3 (6) | Eu1—O16—C17—C18 | 21.1 (10) |
O21—Eu1—O7—C6 | 115.6 (6) | C2A—O1—C18—C17 | −129.0 (16) |
O20—Eu1—O7—C6 | 75.1 (6) | C18A—O1—C18—C17 | −58.2 (13) |
O16—Eu1—O7—C6 | −77.6 (7) | C2—O1—C18—C17 | −89.1 (10) |
O4—Eu1—O7—C6 | −12.3 (6) | Eu1—O1—C18—C17 | 47.6 (9) |
O10—Eu1—O7—C6 | 167.2 (6) | O16—C17—C18—O1 | −43.6 (11) |
O13—Eu1—O7—C6 | −156.8 (5) | C18A—C17—C18—O1 | 57.8 (13) |
O1—Eu1—O7—C6 | 10.9 (6) | C2A—O1—C18A—C17 | −172.8 (18) |
O19—Eu1—O7—C8 | 129.7 (6) | C18—O1—C18A—C17 | 59.0 (13) |
O21—Eu1—O7—C8 | −21.4 (6) | C2—O1—C18A—C17 | −151 (3) |
O20—Eu1—O7—C8 | −61.8 (5) | Eu1—O1—C18A—C17 | −36 (3) |
O16—Eu1—O7—C8 | 145.4 (5) | O16—C17—C18A—O1 | 35 (3) |
O4—Eu1—O7—C8 | −149.3 (6) | C18—C17—C18A—O1 | −58.1 (13) |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O19—H19A···N21 | 0.87 | 1.85 | 2.713 (10) | 171 |
O19—H19B···O42 | 0.83 | 1.77 | 2.582 (8) | 169 |
O20—H20A···O41 | 0.88 | 1.82 | 2.677 (8) | 163 |
O20—H20B···N33 | 0.88 | 1.88 | 2.745 (9) | 167 |
O21—H21A···O41 | 0.87 | 1.88 | 2.695 (8) | 155 |
O21—H21B···N32iii | 0.87 | 1.85 | 2.718 (9) | 171 |
O41—H41A···N22iv | 0.82 | 1.88 | 2.698 (9) | 170 |
O41—H41B···N33v | 0.80 | 2.42 | 3.102 (10) | 143 |
O42—H42A···N31vi | 0.84 | 2.00 | 2.834 (10) | 175 |
O42—H42B···N23vii | 0.81 | 2.02 | 2.810 (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, z−1; (vii) −x+1, −y+1, −z. |
[Gd(C12H24O6)(H2O)3][Cr(CN)6]·2H2O | Z = 2 |
Mr = 719.76 | F(000) = 720 |
Triclinic, P1 | Dx = 1.647 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.0563 (2) Å | Cell parameters from 6595 reflections |
b = 11.1562 (2) Å | θ = 2.9–27.5° |
c = 14.2127 (3) Å | µ = 2.70 mm−1 |
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 |
Bruker–Nonius KappaCCD diffractometer | 6646 independent reflections |
Radiation source: Bruker–Nonius FR591 rotating anode | 6382 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.038 |
Detector resolution: 9.091 pixels mm-1 | θmax = 27.5°, θmin = 3.4° |
ϕ & ω scans | h = −14→14 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | k = −14→14 |
Tmin = 0.672, Tmax = 0.899 | l = −18→18 |
34884 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.108 | H-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 parameters | Δρmax = 3.60 e Å−3 |
8 restraints | Δρmin = −1.63 e Å−3 |
[Gd(C12H24O6)(H2O)3][Cr(CN)6]·2H2O | γ = 66.0299 (12)° |
Mr = 719.76 | V = 1450.92 (5) Å3 |
Triclinic, P1 | Z = 2 |
a = 11.0563 (2) Å | Mo Kα radiation |
b = 11.1562 (2) Å | µ = 2.70 mm−1 |
c = 14.2127 (3) Å | T = 120 K |
α = 68.3494 (11)° | 0.16 × 0.15 × 0.04 mm |
β = 70.0959 (12)° |
Bruker–Nonius KappaCCD diffractometer | 6646 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | 6382 reflections with I > 2σ(I) |
Tmin = 0.672, Tmax = 0.899 | Rint = 0.038 |
34884 measured reflections |
R[F2 > 2σ(F2)] = 0.040 | 8 restraints |
wR(F2) = 0.108 | H-atom parameters constrained |
S = 1.04 | Δρmax = 3.60 e Å−3 |
6646 reflections | Δρmin = −1.63 e Å−3 |
334 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Gd1 | 0.21115 (2) | 0.72456 (2) | 0.279303 (15) | 0.01806 (8) | |
O1 | 0.0618 (3) | 0.5681 (3) | 0.3682 (2) | 0.0249 (7) | |
C2 | 0.0899 (7) | 0.4598 (8) | 0.3253 (8) | 0.0297 (10)* | 0.458 (7) |
C2A | 0.1330 (8) | 0.4262 (5) | 0.3896 (5) | 0.0297 (10)* | 0.542 (7) |
C3 | 0.2388 (5) | 0.3941 (5) | 0.2941 (4) | 0.0353 (12) | |
O4 | 0.2990 (4) | 0.4985 (4) | 0.2432 (4) | 0.0461 (11) | |
C5 | 0.4264 (6) | 0.4663 (6) | 0.1679 (5) | 0.0403 (13) | |
C6 | 0.5252 (5) | 0.4964 (5) | 0.1965 (4) | 0.0322 (11) | |
O7 | 0.4652 (3) | 0.6338 (3) | 0.2047 (3) | 0.0242 (7) | |
C8 | 0.5504 (5) | 0.6713 (6) | 0.2388 (5) | 0.0338 (11) | |
C9 | 0.4962 (5) | 0.8220 (6) | 0.2185 (5) | 0.0339 (11) | |
O10 | 0.3519 (3) | 0.8611 (3) | 0.2652 (3) | 0.0305 (8) | |
C11 | 0.2994 (8) | 1.0077 (7) | 0.2354 (8) | 0.065 (2) | |
C12 | 0.1618 (9) | 1.0583 (7) | 0.2497 (10) | 0.090 (4) | |
O13 | 0.1098 (4) | 0.9822 (4) | 0.2203 (3) | 0.0293 (7) | |
C14 | −0.0342 (7) | 1.0460 (7) | 0.2218 (6) | 0.0511 (16) | |
C15 | −0.0738 (6) | 0.9580 (5) | 0.1922 (5) | 0.0359 (12) | |
O16 | −0.0223 (3) | 0.8180 (3) | 0.2506 (3) | 0.0261 (7) | |
C17 | −0.1214 (5) | 0.7500 (5) | 0.2998 (4) | 0.0320 (11) | |
C18 | −0.0795 (6) | 0.6364 (9) | 0.3917 (6) | 0.0297 (10)* | 0.458 (7) |
C18A | −0.0495 (7) | 0.6003 (6) | 0.3241 (7) | 0.0297 (10)* | 0.542 (7) |
O19 | 0.2388 (4) | 0.7767 (5) | 0.1020 (3) | 0.0364 (9) | |
O20 | 0.3150 (3) | 0.5812 (3) | 0.4216 (3) | 0.0264 (7) | |
O21 | 0.0845 (3) | 0.8050 (3) | 0.4289 (2) | 0.0241 (7) | |
Cr2 | 0.0000 | 0.5000 | 0.0000 | 0.01807 (19) | |
N21 | 0.0580 (7) | 0.7365 (6) | 0.0374 (4) | 0.0495 (13) | |
N22 | 0.1309 (5) | 0.6085 (5) | −0.2423 (3) | 0.0334 (10) | |
N23 | 0.3003 (5) | 0.3136 (6) | 0.0358 (4) | 0.0466 (13) | |
C21 | 0.0315 (6) | 0.6548 (6) | 0.0254 (4) | 0.0311 (10) | |
C22 | 0.0827 (5) | 0.5693 (5) | −0.1566 (4) | 0.0240 (9) | |
C23 | 0.1922 (5) | 0.3776 (5) | 0.0238 (4) | 0.0305 (10) | |
Cr3 | 0.5000 | 0.0000 | 0.5000 | 0.01763 (19) | |
N31 | 0.4262 (4) | −0.0966 (5) | 0.7500 (3) | 0.0322 (9) | |
N32 | 0.1859 (4) | 0.0726 (5) | 0.5029 (4) | 0.0348 (10) | |
N33 | 0.4356 (5) | 0.3094 (4) | 0.4976 (4) | 0.0346 (10) | |
C31 | 0.4518 (4) | −0.0627 (5) | 0.6612 (4) | 0.0235 (9) | |
C32 | 0.2989 (5) | 0.0460 (5) | 0.4989 (4) | 0.0245 (9) | |
C33 | 0.4588 (5) | 0.1976 (5) | 0.5018 (4) | 0.0240 (9) | |
O41 | 0.2465 (4) | 0.7199 (4) | 0.5609 (3) | 0.0310 (8) | |
O42 | 0.4314 (4) | 0.8577 (5) | −0.0406 (3) | 0.0414 (10) | |
H2A | 0.0496 | 0.4960 | 0.2640 | 0.036* | 0.458 (7) |
H2B | 0.0482 | 0.3914 | 0.3774 | 0.036* | 0.458 (7) |
H2C | 0.0686 | 0.3752 | 0.4104 | 0.036* | 0.542 (7) |
H2D | 0.1773 | 0.3980 | 0.4477 | 0.036* | 0.542 (7) |
H3A | 0.2757 | 0.3337 | 0.3561 | 0.042* | 0.458 (7) |
H3B | 0.2586 | 0.3386 | 0.2468 | 0.042* | 0.458 (7) |
H3C | 0.3093 | 0.3058 | 0.3142 | 0.042* | 0.542 (7) |
H3D | 0.1960 | 0.3867 | 0.2464 | 0.042* | 0.542 (7) |
H5A | 0.4147 | 0.5222 | 0.0970 | 0.048* | |
H5B | 0.4583 | 0.3690 | 0.1695 | 0.048* | |
H6A | 0.5454 | 0.4327 | 0.2636 | 0.039* | |
H6B | 0.6110 | 0.4866 | 0.1427 | 0.039* | |
H8A | 0.6457 | 0.6425 | 0.1998 | 0.041* | |
H8B | 0.5471 | 0.6275 | 0.3138 | 0.041* | |
H9A | 0.5434 | 0.8527 | 0.2486 | 0.041* | |
H9B | 0.5115 | 0.8652 | 0.1427 | 0.041* | |
H11A | 0.3276 | 1.0429 | 0.2762 | 0.078* | |
H11B | 0.3403 | 1.0414 | 0.1611 | 0.078* | |
H12A | 0.1354 | 1.1545 | 0.2081 | 0.108* | |
H12B | 0.1208 | 1.0563 | 0.3238 | 0.108* | |
H14A | −0.0513 | 1.1376 | 0.1722 | 0.061* | |
H14B | −0.0866 | 1.0554 | 0.2922 | 0.061* | |
H15A | −0.1741 | 0.9867 | 0.2060 | 0.043* | |
H15B | −0.0373 | 0.9660 | 0.1170 | 0.043* | |
H17A | −0.1307 | 0.7132 | 0.2500 | 0.038* | 0.458 (7) |
H17B | −0.2105 | 0.8153 | 0.3226 | 0.038* | 0.458 (7) |
H17C | −0.1822 | 0.7757 | 0.2532 | 0.038* | 0.542 (7) |
H17D | −0.1771 | 0.7765 | 0.3646 | 0.038* | 0.542 (7) |
H18A | −0.1028 | 0.6734 | 0.4514 | 0.036* | 0.458 (7) |
H18B | −0.1293 | 0.5713 | 0.4115 | 0.036* | 0.458 (7) |
H18C | −0.1133 | 0.5516 | 0.3736 | 0.036* | 0.542 (7) |
H18D | −0.0157 | 0.5703 | 0.2597 | 0.036* | 0.542 (7) |
H19A | 0.1876 | 0.7599 | 0.0753 | 0.055 (7)* | |
H19B | 0.3040 | 0.7898 | 0.0531 | 0.055 (7)* | |
H20A | 0.3075 | 0.6100 | 0.4745 | 0.055 (7)* | |
H20B | 0.3666 | 0.4943 | 0.4369 | 0.055 (7)* | |
H21A | 0.1211 | 0.7938 | 0.4792 | 0.055 (7)* | |
H21B | −0.0014 | 0.8514 | 0.4487 | 0.055 (7)* | |
H41A | 0.2149 | 0.6913 | 0.6240 | 0.055 (7)* | |
H41B | 0.3045 | 0.7486 | 0.5585 | 0.055 (7)* | |
H42A | 0.4260 | 0.8704 | −0.1021 | 0.055 (7)* | |
H42B | 0.5057 | 0.7978 | −0.0381 | 0.055 (7)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Gd1 | 0.01794 (12) | 0.02037 (12) | 0.01745 (12) | −0.00866 (8) | −0.00270 (8) | −0.00512 (8) |
O1 | 0.0286 (17) | 0.0291 (17) | 0.0229 (15) | −0.0176 (14) | −0.0049 (13) | −0.0048 (13) |
C3 | 0.046 (3) | 0.025 (2) | 0.039 (3) | −0.016 (2) | −0.004 (2) | −0.011 (2) |
O4 | 0.035 (2) | 0.041 (2) | 0.072 (3) | −0.0248 (18) | 0.018 (2) | −0.039 (2) |
C5 | 0.036 (3) | 0.039 (3) | 0.049 (3) | −0.013 (2) | 0.006 (2) | −0.029 (3) |
C6 | 0.028 (2) | 0.025 (2) | 0.038 (3) | −0.0043 (19) | −0.001 (2) | −0.013 (2) |
O7 | 0.0202 (15) | 0.0237 (16) | 0.0299 (17) | −0.0069 (13) | −0.0048 (13) | −0.0095 (13) |
C8 | 0.019 (2) | 0.039 (3) | 0.047 (3) | −0.009 (2) | −0.006 (2) | −0.019 (2) |
C9 | 0.026 (2) | 0.036 (3) | 0.046 (3) | −0.015 (2) | −0.003 (2) | −0.016 (2) |
O10 | 0.0209 (16) | 0.0234 (17) | 0.052 (2) | −0.0061 (13) | −0.0084 (15) | −0.0165 (16) |
C11 | 0.052 (4) | 0.029 (3) | 0.137 (8) | −0.003 (3) | −0.047 (5) | −0.033 (4) |
C12 | 0.077 (6) | 0.024 (3) | 0.193 (12) | −0.018 (3) | −0.088 (7) | 0.001 (5) |
O13 | 0.0304 (18) | 0.0252 (17) | 0.0312 (18) | −0.0129 (14) | −0.0113 (14) | 0.0019 (14) |
C14 | 0.047 (4) | 0.034 (3) | 0.064 (4) | −0.009 (3) | −0.020 (3) | −0.001 (3) |
C15 | 0.029 (3) | 0.026 (2) | 0.048 (3) | −0.001 (2) | −0.021 (2) | −0.003 (2) |
O16 | 0.0185 (15) | 0.0235 (16) | 0.0333 (18) | −0.0080 (13) | −0.0078 (13) | −0.0011 (13) |
C17 | 0.020 (2) | 0.040 (3) | 0.035 (3) | −0.016 (2) | −0.0051 (19) | −0.003 (2) |
O19 | 0.0254 (17) | 0.064 (3) | 0.0199 (16) | −0.0144 (17) | −0.0040 (13) | −0.0128 (17) |
O20 | 0.0306 (17) | 0.0216 (16) | 0.0218 (16) | −0.0027 (13) | −0.0092 (13) | −0.0038 (12) |
O21 | 0.0194 (15) | 0.0303 (17) | 0.0214 (15) | −0.0039 (13) | −0.0046 (12) | −0.0100 (13) |
Cr2 | 0.0183 (4) | 0.0221 (5) | 0.0163 (4) | −0.0111 (4) | −0.0034 (3) | −0.0031 (4) |
N21 | 0.071 (4) | 0.054 (3) | 0.043 (3) | −0.038 (3) | −0.012 (3) | −0.015 (2) |
N22 | 0.040 (2) | 0.040 (2) | 0.024 (2) | −0.023 (2) | −0.0050 (18) | −0.0031 (18) |
N23 | 0.028 (2) | 0.049 (3) | 0.051 (3) | −0.013 (2) | −0.013 (2) | 0.003 (2) |
C21 | 0.038 (3) | 0.036 (3) | 0.026 (2) | −0.019 (2) | −0.007 (2) | −0.008 (2) |
C22 | 0.026 (2) | 0.027 (2) | 0.023 (2) | −0.0125 (18) | −0.0064 (17) | −0.0067 (18) |
C23 | 0.024 (2) | 0.032 (3) | 0.030 (2) | −0.010 (2) | −0.0068 (19) | −0.001 (2) |
Cr3 | 0.0155 (4) | 0.0174 (4) | 0.0186 (4) | −0.0067 (3) | −0.0033 (3) | −0.0022 (3) |
N31 | 0.028 (2) | 0.040 (2) | 0.025 (2) | −0.0118 (19) | −0.0052 (16) | −0.0050 (18) |
N32 | 0.022 (2) | 0.047 (3) | 0.037 (2) | −0.0090 (19) | −0.0059 (17) | −0.017 (2) |
N33 | 0.037 (2) | 0.021 (2) | 0.045 (3) | −0.0082 (18) | −0.015 (2) | −0.0052 (18) |
C31 | 0.0164 (19) | 0.023 (2) | 0.027 (2) | −0.0046 (16) | −0.0048 (17) | −0.0050 (17) |
C32 | 0.022 (2) | 0.027 (2) | 0.024 (2) | −0.0083 (18) | −0.0033 (17) | −0.0077 (18) |
C33 | 0.021 (2) | 0.024 (2) | 0.026 (2) | −0.0085 (17) | −0.0059 (17) | −0.0032 (17) |
O41 | 0.040 (2) | 0.045 (2) | 0.0179 (15) | −0.0294 (17) | −0.0045 (14) | −0.0031 (14) |
O42 | 0.0292 (19) | 0.060 (3) | 0.0216 (17) | −0.0061 (18) | −0.0053 (14) | −0.0065 (17) |
Gd1—O19 | 2.307 (3) | C14—C15 | 1.453 (9) |
Gd1—O21 | 2.377 (3) | C14—H14A | 0.99 |
Gd1—O20 | 2.381 (3) | C14—H14B | 0.99 |
Gd1—O16 | 2.476 (3) | C15—O16 | 1.448 (6) |
Gd1—O4 | 2.489 (4) | C15—H15A | 0.99 |
Gd1—O10 | 2.504 (3) | C15—H15B | 0.99 |
Gd1—O13 | 2.543 (3) | O16—C17 | 1.423 (6) |
Gd1—O7 | 2.548 (3) | C17—C18A | 1.491 (5) |
Gd1—O1 | 2.581 (3) | C17—C18 | 1.497 (5) |
O1—C18 | 1.413 (5) | C17—H17A | 0.99 |
O1—C2A | 1.419 (5) | C17—H17B | 0.99 |
O1—C18A | 1.426 (5) | C17—H17C | 0.99 |
O1—C2 | 1.427 (5) | C17—H17D | 0.99 |
C2—C3 | 1.485 (5) | C18—H18A | 0.99 |
C2—H2A | 0.99 | C18—H18B | 0.99 |
C2—H2B | 0.99 | C18A—H18C | 0.99 |
C2A—C3 | 1.509 (5) | C18A—H18D | 0.99 |
C2A—H2C | 0.99 | O19—H19A | 0.89 |
C2A—H2D | 0.99 | O19—H19B | 0.83 |
C3—O4 | 1.415 (6) | O20—H20A | 0.89 |
C3—H3A | 0.99 | O20—H20B | 0.89 |
C3—H3B | 0.99 | O21—H21A | 0.88 |
C3—H3C | 0.99 | O21—H21B | 0.88 |
C3—H3D | 0.99 | Cr2—C21 | 2.066 (5) |
O4—C5 | 1.450 (6) | Cr2—C21i | 2.066 (5) |
C5—C6 | 1.473 (8) | Cr2—C23 | 2.070 (5) |
C5—H5A | 0.99 | Cr2—C23i | 2.070 (5) |
C5—H5B | 0.99 | Cr2—C22i | 2.075 (5) |
C6—O7 | 1.435 (6) | Cr2—C22 | 2.075 (5) |
C6—H6A | 0.99 | N21—C21 | 1.145 (7) |
C6—H6B | 0.99 | N22—C22 | 1.146 (6) |
O7—C8 | 1.441 (6) | N23—C23 | 1.150 (7) |
C8—C9 | 1.486 (8) | Cr3—C33 | 2.071 (5) |
C8—H8A | 0.99 | Cr3—C33ii | 2.071 (5) |
C8—H8B | 0.99 | Cr3—C32ii | 2.074 (5) |
C9—O10 | 1.450 (6) | Cr3—C32 | 2.074 (5) |
C9—H9A | 0.99 | Cr3—C31ii | 2.076 (5) |
C9—H9B | 0.99 | Cr3—C31 | 2.076 (5) |
O10—C11 | 1.441 (7) | N31—C31 | 1.143 (6) |
C11—C12 | 1.360 (11) | N32—C32 | 1.147 (6) |
C11—H11A | 0.99 | N33—C33 | 1.149 (7) |
C11—H11B | 0.99 | O41—H41A | 0.83 |
C12—O13 | 1.432 (8) | O41—H41B | 0.81 |
C12—H12A | 0.99 | O42—H42A | 0.85 |
C12—H12B | 0.99 | O42—H42B | 0.82 |
O13—C14 | 1.453 (7) | ||
O19—Gd1—O21 | 144.08 (13) | C12—C11—H11A | 108.8 |
O19—Gd1—O20 | 144.24 (13) | O10—C11—H11A | 108.8 |
O21—Gd1—O20 | 70.73 (11) | C12—C11—H11B | 108.8 |
O19—Gd1—O16 | 75.00 (12) | O10—C11—H11B | 108.8 |
O21—Gd1—O16 | 78.66 (11) | H11A—C11—H11B | 107.7 |
O20—Gd1—O16 | 135.57 (12) | C11—C12—O13 | 111.9 (8) |
O19—Gd1—O4 | 76.01 (16) | C11—C12—H12A | 109.2 |
O21—Gd1—O4 | 134.26 (14) | O13—C12—H12A | 109.2 |
O20—Gd1—O4 | 78.39 (15) | C11—C12—H12B | 109.2 |
O16—Gd1—O4 | 102.87 (13) | O13—C12—H12B | 109.2 |
O19—Gd1—O10 | 93.87 (14) | H12A—C12—H12B | 107.9 |
O21—Gd1—O10 | 82.15 (12) | C12—O13—C14 | 112.4 (5) |
O20—Gd1—O10 | 81.39 (12) | C12—O13—Gd1 | 115.8 (3) |
O16—Gd1—O10 | 125.86 (11) | C14—O13—Gd1 | 120.5 (3) |
O4—Gd1—O10 | 125.97 (12) | O13—C14—C15 | 106.7 (5) |
O19—Gd1—O13 | 74.60 (14) | O13—C14—H14A | 110.4 |
O21—Gd1—O13 | 71.80 (12) | C15—C14—H14A | 110.4 |
O20—Gd1—O13 | 130.99 (12) | O13—C14—H14B | 110.4 |
O16—Gd1—O13 | 62.80 (11) | C15—C14—H14B | 110.4 |
O4—Gd1—O13 | 149.82 (15) | H14A—C14—H14B | 108.6 |
O10—Gd1—O13 | 63.16 (11) | O16—C15—C14 | 110.1 (5) |
O19—Gd1—O7 | 73.45 (12) | O16—C15—H15A | 109.6 |
O21—Gd1—O7 | 132.65 (11) | C14—C15—H15A | 109.6 |
O20—Gd1—O7 | 72.82 (11) | O16—C15—H15B | 109.6 |
O16—Gd1—O7 | 147.74 (11) | C14—C15—H15B | 109.6 |
O4—Gd1—O7 | 62.94 (11) | H15A—C15—H15B | 108.2 |
O10—Gd1—O7 | 63.30 (11) | C17—O16—C15 | 114.4 (4) |
O13—Gd1—O7 | 113.99 (11) | C17—O16—Gd1 | 124.6 (3) |
O19—Gd1—O1 | 108.29 (13) | C15—O16—Gd1 | 120.4 (3) |
O21—Gd1—O1 | 79.92 (11) | O16—C17—C18A | 108.4 (5) |
O20—Gd1—O1 | 80.48 (11) | O16—C17—C18 | 109.7 (5) |
O16—Gd1—O1 | 62.74 (10) | O16—C17—H17A | 109.7 |
O4—Gd1—O1 | 62.02 (11) | C18—C17—H17A | 109.7 |
O10—Gd1—O1 | 157.84 (12) | O16—C17—H17B | 109.7 |
O13—Gd1—O1 | 122.13 (11) | C18—C17—H17B | 109.7 |
O7—Gd1—O1 | 122.25 (10) | H17A—C17—H17B | 108.2 |
C2A—O1—C18A | 110.6 (5) | O16—C17—H17C | 110.0 |
C18—O1—C2 | 110.6 (6) | C18A—C17—H17C | 110.0 |
C18A—O1—C2 | 72.8 (4) | O16—C17—H17D | 110.0 |
C18—O1—Gd1 | 115.1 (4) | C18A—C17—H17D | 110.0 |
C2A—O1—Gd1 | 115.6 (4) | H17C—C17—H17D | 108.4 |
C18A—O1—Gd1 | 116.4 (4) | O1—C18—C17 | 110.3 (5) |
C2—O1—Gd1 | 117.8 (4) | O1—C18—H18A | 109.6 |
O1—C2—C3 | 110.5 (5) | C17—C18—H18A | 109.6 |
O1—C2—H2A | 109.5 | O1—C18—H18B | 109.6 |
C3—C2—H2A | 109.5 | C17—C18—H18B | 109.6 |
O1—C2—H2B | 109.5 | H18A—C18—H18B | 108.1 |
C3—C2—H2B | 109.5 | O1—C18A—C17 | 109.9 (5) |
H2A—C2—H2B | 108.1 | O1—C18A—H18C | 109.7 |
O1—C2A—C3 | 109.6 (5) | C17—C18A—H18C | 109.7 |
O1—C2A—H2C | 109.8 | O1—C18A—H18D | 109.7 |
C3—C2A—H2C | 109.8 | C17—C18A—H18D | 109.7 |
O1—C2A—H2D | 109.8 | H18C—C18A—H18D | 108.2 |
C3—C2A—H2D | 109.8 | Gd1—O19—H19A | 121.1 |
H2C—C2A—H2D | 108.2 | Gd1—O19—H19B | 131.4 |
O4—C3—C2 | 107.8 (5) | H19A—O19—H19B | 105.1 |
O4—C3—C2A | 109.6 (5) | Gd1—O20—H20A | 122.9 |
O4—C3—H3A | 110.1 | Gd1—O20—H20B | 133.1 |
C2—C3—H3A | 110.1 | H20A—O20—H20B | 104.1 |
O4—C3—H3B | 110.1 | Gd1—O21—H21A | 123.2 |
C2—C3—H3B | 110.1 | Gd1—O21—H21B | 133.1 |
H3A—C3—H3B | 108.5 | H21A—O21—H21B | 103.7 |
O4—C3—H3C | 109.7 | C21—Cr2—C21i | 180.0 (3) |
C2A—C3—H3C | 109.7 | C21—Cr2—C23 | 88.2 (2) |
O4—C3—H3D | 109.7 | C21i—Cr2—C23 | 91.8 (2) |
C2A—C3—H3D | 109.7 | C21—Cr2—C23i | 91.8 (2) |
H3C—C3—H3D | 108.2 | C21i—Cr2—C23i | 88.2 (2) |
C3—O4—C5 | 116.3 (4) | C23—Cr2—C23i | 180.00 (18) |
C3—O4—Gd1 | 125.5 (3) | C21—Cr2—C22i | 91.82 (19) |
C5—O4—Gd1 | 118.1 (3) | C21i—Cr2—C22i | 88.18 (19) |
O4—C5—C6 | 107.1 (4) | C23—Cr2—C22i | 90.10 (19) |
O4—C5—H5A | 110.3 | C23i—Cr2—C22i | 89.90 (19) |
C6—C5—H5A | 110.3 | C21—Cr2—C22 | 88.18 (19) |
O4—C5—H5B | 110.3 | C21i—Cr2—C22 | 91.82 (19) |
C6—C5—H5B | 110.3 | C23—Cr2—C22 | 89.90 (19) |
H5A—C5—H5B | 108.6 | C23i—Cr2—C22 | 90.10 (19) |
O7—C6—C5 | 107.2 (4) | C22i—Cr2—C22 | 180.0 (4) |
O7—C6—H6A | 110.3 | N21—C21—Cr2 | 175.5 (6) |
C5—C6—H6A | 110.3 | N22—C22—Cr2 | 178.1 (4) |
O7—C6—H6B | 110.3 | N23—C23—Cr2 | 177.6 (5) |
C5—C6—H6B | 110.3 | C33—Cr3—C33ii | 180.0 |
H6A—C6—H6B | 108.5 | C33—Cr3—C32ii | 90.41 (18) |
C6—O7—C8 | 111.8 (4) | C33ii—Cr3—C32ii | 89.59 (18) |
C6—O7—Gd1 | 119.6 (3) | C33—Cr3—C32 | 89.59 (18) |
C8—O7—Gd1 | 115.4 (3) | C33ii—Cr3—C32 | 90.41 (18) |
O7—C8—C9 | 106.4 (4) | C32ii—Cr3—C32 | 180.000 (1) |
O7—C8—H8A | 110.5 | C33—Cr3—C31ii | 88.76 (18) |
C9—C8—H8A | 110.5 | C33ii—Cr3—C31ii | 91.24 (18) |
O7—C8—H8B | 110.5 | C32ii—Cr3—C31ii | 89.76 (18) |
C9—C8—H8B | 110.5 | C32—Cr3—C31ii | 90.24 (18) |
H8A—C8—H8B | 108.6 | C33—Cr3—C31 | 91.24 (18) |
O10—C9—C8 | 108.6 (4) | C33ii—Cr3—C31 | 88.76 (18) |
O10—C9—H9A | 110.0 | C32ii—Cr3—C31 | 90.24 (18) |
C8—C9—H9A | 110.0 | C32—Cr3—C31 | 89.76 (18) |
O10—C9—H9B | 110.0 | C31ii—Cr3—C31 | 180.0 |
C8—C9—H9B | 110.0 | N31—C31—Cr3 | 179.2 (4) |
H9A—C9—H9B | 108.3 | N32—C32—Cr3 | 176.7 (4) |
C11—O10—C9 | 107.5 (5) | N33—C33—Cr3 | 176.5 (4) |
C11—O10—Gd1 | 120.0 (3) | H41A—O41—H41B | 105.1 |
C9—O10—Gd1 | 120.8 (3) | H42A—O42—H42B | 101.4 |
C12—C11—O10 | 113.8 (6) | ||
O19—Gd1—O1—C18 | −89.6 (5) | O10—Gd1—O7—C8 | 27.2 (3) |
O21—Gd1—O1—C18 | 54.2 (4) | O13—Gd1—O7—C8 | 66.2 (3) |
O20—Gd1—O1—C18 | 126.2 (5) | O1—Gd1—O7—C8 | −128.1 (3) |
O16—Gd1—O1—C18 | −28.1 (4) | C6—O7—C8—C9 | 165.9 (4) |
O4—Gd1—O1—C18 | −152.0 (5) | Gd1—O7—C8—C9 | −52.8 (5) |
O10—Gd1—O1—C18 | 90.7 (5) | O7—C8—C9—O10 | 52.4 (6) |
O13—Gd1—O1—C18 | −6.7 (5) | C8—C9—O10—C11 | −174.2 (5) |
O7—Gd1—O1—C18 | −171.2 (4) | C8—C9—O10—Gd1 | −31.3 (6) |
O19—Gd1—O1—C2A | 92.5 (4) | O19—Gd1—O10—C11 | 72.5 (6) |
O21—Gd1—O1—C2A | −123.7 (4) | O21—Gd1—O10—C11 | −71.6 (6) |
O20—Gd1—O1—C2A | −51.7 (4) | O20—Gd1—O10—C11 | −143.1 (6) |
O16—Gd1—O1—C2A | 154.0 (4) | O16—Gd1—O10—C11 | −1.7 (6) |
O4—Gd1—O1—C2A | 30.1 (4) | O4—Gd1—O10—C11 | 148.0 (5) |
O10—Gd1—O1—C2A | −87.2 (5) | O13—Gd1—O10—C11 | 2.0 (5) |
O13—Gd1—O1—C2A | 175.4 (4) | O7—Gd1—O10—C11 | 141.8 (6) |
O7—Gd1—O1—C2A | 10.9 (4) | O1—Gd1—O10—C11 | −107.8 (6) |
O19—Gd1—O1—C18A | −39.9 (4) | O19—Gd1—O10—C9 | −65.9 (4) |
O21—Gd1—O1—C18A | 104.0 (4) | O21—Gd1—O10—C9 | 150.1 (4) |
O20—Gd1—O1—C18A | 175.9 (4) | O20—Gd1—O10—C9 | 78.5 (4) |
O16—Gd1—O1—C18A | 21.6 (4) | O16—Gd1—O10—C9 | −140.1 (4) |
O4—Gd1—O1—C18A | −102.2 (4) | O4—Gd1—O10—C9 | 9.7 (4) |
O10—Gd1—O1—C18A | 140.4 (4) | O13—Gd1—O10—C9 | −136.4 (4) |
O13—Gd1—O1—C18A | 43.1 (4) | O7—Gd1—O10—C9 | 3.4 (4) |
O7—Gd1—O1—C18A | −121.5 (4) | O1—Gd1—O10—C9 | 113.8 (4) |
O19—Gd1—O1—C2 | 43.8 (5) | C9—O10—C11—C12 | 163.5 (9) |
O21—Gd1—O1—C2 | −172.4 (5) | Gd1—O10—C11—C12 | 20.2 (11) |
O20—Gd1—O1—C2 | −100.4 (5) | O10—C11—C12—O13 | −40.9 (13) |
O16—Gd1—O1—C2 | 105.3 (5) | C11—C12—O13—C14 | −172.2 (8) |
O4—Gd1—O1—C2 | −18.6 (5) | C11—C12—O13—Gd1 | 43.8 (11) |
O10—Gd1—O1—C2 | −135.9 (5) | O19—Gd1—O13—C12 | −125.8 (6) |
O13—Gd1—O1—C2 | 126.7 (5) | O21—Gd1—O13—C12 | 67.1 (6) |
O7—Gd1—O1—C2 | −37.8 (5) | O20—Gd1—O13—C12 | 25.3 (7) |
C18—O1—C2—C3 | 176.2 (6) | O16—Gd1—O13—C12 | 153.4 (7) |
C2A—O1—C2—C3 | −57.9 (6) | O4—Gd1—O13—C12 | −139.3 (6) |
C18A—O1—C2—C3 | 152.2 (9) | O10—Gd1—O13—C12 | −23.2 (6) |
Gd1—O1—C2—C3 | 40.9 (9) | O7—Gd1—O13—C12 | −62.3 (6) |
C18—O1—C2A—C3 | 134.2 (7) | O1—Gd1—O13—C12 | 132.0 (6) |
C18A—O1—C2A—C3 | 86.7 (7) | O19—Gd1—O13—C14 | 93.2 (4) |
C2—O1—C2A—C3 | 56.0 (6) | O21—Gd1—O13—C14 | −73.9 (4) |
Gd1—O1—C2A—C3 | −48.3 (7) | O20—Gd1—O13—C14 | −115.6 (4) |
O1—C2—C3—O4 | −43.4 (9) | O16—Gd1—O13—C14 | 12.5 (4) |
O1—C2—C3—C2A | 56.3 (6) | O4—Gd1—O13—C14 | 79.8 (5) |
O1—C2A—C3—O4 | 38.6 (8) | O10—Gd1—O13—C14 | −164.2 (5) |
O1—C2A—C3—C2 | −56.3 (6) | O7—Gd1—O13—C14 | 156.7 (4) |
C2—C3—O4—C5 | −153.2 (6) | O1—Gd1—O13—C14 | −9.0 (5) |
C2A—C3—O4—C5 | 163.5 (6) | C12—O13—C14—C15 | −179.1 (7) |
C2—C3—O4—Gd1 | 30.3 (7) | Gd1—O13—C14—C15 | −36.9 (7) |
C2A—C3—O4—Gd1 | −13.0 (7) | O13—C14—C15—O16 | 47.7 (7) |
O19—Gd1—O4—C3 | −127.8 (5) | C14—C15—O16—C17 | 129.5 (5) |
O21—Gd1—O4—C3 | 29.5 (6) | C14—C15—O16—Gd1 | −42.1 (6) |
O20—Gd1—O4—C3 | 77.4 (5) | O19—Gd1—O16—C17 | 125.3 (4) |
O16—Gd1—O4—C3 | −57.1 (5) | O21—Gd1—O16—C17 | −79.3 (4) |
O10—Gd1—O4—C3 | 147.7 (4) | O20—Gd1—O16—C17 | −32.6 (4) |
O13—Gd1—O4—C3 | −114.4 (5) | O4—Gd1—O16—C17 | 53.9 (4) |
O7—Gd1—O4—C3 | 153.9 (5) | O10—Gd1—O16—C17 | −150.9 (4) |
O1—Gd1—O4—C3 | −7.9 (4) | O13—Gd1—O16—C17 | −154.6 (4) |
O19—Gd1—O4—C5 | 55.8 (4) | O7—Gd1—O16—C17 | 113.0 (4) |
O21—Gd1—O4—C5 | −146.9 (4) | O1—Gd1—O16—C17 | 5.1 (4) |
O20—Gd1—O4—C5 | −99.0 (5) | O19—Gd1—O16—C15 | −64.0 (4) |
O16—Gd1—O4—C5 | 126.5 (4) | O21—Gd1—O16—C15 | 91.3 (4) |
O10—Gd1—O4—C5 | −28.8 (5) | O20—Gd1—O16—C15 | 138.1 (4) |
O13—Gd1—O4—C5 | 69.2 (5) | O4—Gd1—O16—C15 | −135.5 (4) |
O7—Gd1—O4—C5 | −22.5 (4) | O10—Gd1—O16—C15 | 19.8 (4) |
O1—Gd1—O4—C5 | 175.7 (5) | O13—Gd1—O16—C15 | 16.1 (4) |
C3—O4—C5—C6 | −126.7 (5) | O7—Gd1—O16—C15 | −76.3 (4) |
Gd1—O4—C5—C6 | 50.0 (6) | O1—Gd1—O16—C15 | 175.8 (4) |
O4—C5—C6—O7 | −53.2 (6) | C15—O16—C17—C18A | 160.4 (5) |
C5—C6—O7—C8 | 176.4 (4) | Gd1—O16—C17—C18A | −28.4 (6) |
C5—C6—O7—Gd1 | 37.0 (5) | C15—O16—C17—C18 | −154.9 (6) |
O19—Gd1—O7—C6 | −91.6 (4) | Gd1—O16—C17—C18 | 16.3 (7) |
O21—Gd1—O7—C6 | 117.4 (3) | C2A—O1—C18—C17 | −135.0 (7) |
O20—Gd1—O7—C6 | 76.4 (3) | C18A—O1—C18—C17 | −55.6 (6) |
O16—Gd1—O7—C6 | −79.2 (4) | C2—O1—C18—C17 | −89.3 (9) |
O4—Gd1—O7—C6 | −9.1 (3) | Gd1—O1—C18—C17 | 47.4 (8) |
O10—Gd1—O7—C6 | 165.2 (4) | O16—C17—C18—O1 | −40.4 (9) |
O13—Gd1—O7—C6 | −155.8 (3) | C18A—C17—C18—O1 | 55.5 (6) |
O1—Gd1—O7—C6 | 9.9 (4) | C18—O1—C18A—C17 | 55.7 (6) |
O19—Gd1—O7—C8 | 130.4 (4) | C2A—O1—C18A—C17 | −178.7 (5) |
O21—Gd1—O7—C8 | −20.7 (4) | C2—O1—C18A—C17 | −157.2 (8) |
O20—Gd1—O7—C8 | −61.7 (3) | Gd1—O1—C18A—C17 | −44.1 (7) |
O16—Gd1—O7—C8 | 142.8 (3) | O16—C17—C18A—O1 | 44.9 (8) |
O4—Gd1—O7—C8 | −147.2 (4) | C18—C17—C18A—O1 | −54.5 (6) |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O19—H19A···N21 | 0.89 | 1.83 | 2.706 (7) | 170 |
O19—H19B···O42 | 0.83 | 1.78 | 2.594 (6) | 165 |
O20—H20A···O41 | 0.89 | 1.83 | 2.679 (5) | 160 |
O20—H20B···N33 | 0.89 | 1.85 | 2.723 (5) | 165 |
O21—H21A···O41 | 0.88 | 1.85 | 2.688 (5) | 158 |
O21—H21B···N32iii | 0.88 | 1.85 | 2.725 (5) | 173 |
O41—H41A···N22iv | 0.83 | 1.88 | 2.701 (5) | 169 |
O41—H41B···N33v | 0.81 | 2.57 | 3.230 (6) | 139 |
O42—H42A···N31vi | 0.85 | 1.99 | 2.846 (6) | 176 |
O42—H42B···N23vii | 0.82 | 2.00 | 2.809 (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, z−1; (vii) −x+1, −y+1, −z. |
[Gd(C12H24O6)(H2O)3][Co(CN)6]·2H2O | Z = 2 |
Mr = 726.69 | F(000) = 726 |
Triclinic, P1 | Dx = 1.742 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.8604 (2) Å | Cell parameters from 6164 reflections |
b = 11.0724 (3) Å | θ = 2.9–27.5° |
c = 13.9909 (2) Å | µ = 3.03 mm−1 |
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 |
Bruker–Nonius KappaCCD diffractometer | 6348 independent reflections |
Radiation source: Bruker–Nonius FR591 rotating anode | 6022 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
Detector resolution: 9.091 pixels mm-1 | θmax = 27.6°, θmin = 3.2° |
ϕ & ω scans | h = −14→14 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | k = −14→14 |
Tmin = 0.187, Tmax = 0.280 | l = −18→18 |
27907 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.020 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.047 | H-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 parameters | Δρmax = 1.00 e Å−3 |
8 restraints | Δρmin = −0.91 e Å−3 |
[Gd(C12H24O6)(H2O)3][Co(CN)6]·2H2O | γ = 65.5666 (9)° |
Mr = 726.69 | V = 1385.20 (5) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.8604 (2) Å | Mo Kα radiation |
b = 11.0724 (3) Å | µ = 3.03 mm−1 |
c = 13.9909 (2) Å | T = 120 K |
α = 67.5857 (10)° | 0.60 × 0.54 × 0.42 mm |
β = 70.5870 (8)° |
Bruker–Nonius KappaCCD diffractometer | 6348 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | 6022 reflections with I > 2σ(I) |
Tmin = 0.187, Tmax = 0.280 | Rint = 0.033 |
27907 measured reflections |
R[F2 > 2σ(F2)] = 0.020 | 8 restraints |
wR(F2) = 0.047 | H-atom parameters constrained |
S = 1.09 | Δρmax = 1.00 e Å−3 |
6348 reflections | Δρmin = −0.91 e Å−3 |
334 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Gd1 | 0.204535 (10) | 0.727652 (10) | 0.276475 (8) | 0.00822 (4) | |
O1 | 0.05822 (16) | 0.56550 (15) | 0.36672 (12) | 0.0145 (3) | |
C2 | 0.0911 (3) | 0.4532 (3) | 0.3232 (3) | 0.0196 (8)* | 0.777 (6) |
C2A | 0.1288 (8) | 0.4225 (5) | 0.3849 (5) | 0.015 (3)* | 0.223 (6) |
C3 | 0.2409 (3) | 0.3959 (2) | 0.2899 (2) | 0.0230 (5) | |
O4 | 0.29066 (18) | 0.50784 (17) | 0.22885 (15) | 0.0239 (4) | |
C5 | 0.4213 (3) | 0.4760 (3) | 0.1564 (2) | 0.0228 (5) | |
C6 | 0.5233 (2) | 0.4976 (2) | 0.1919 (2) | 0.0211 (5) | |
O7 | 0.46241 (15) | 0.63674 (16) | 0.20197 (12) | 0.0139 (3) | |
C8 | 0.5485 (3) | 0.6706 (3) | 0.2393 (2) | 0.0223 (5) | |
C9 | 0.4943 (2) | 0.8238 (3) | 0.2179 (2) | 0.0241 (5) | |
O10 | 0.34693 (16) | 0.86517 (16) | 0.26154 (14) | 0.0178 (3) | |
C11 | 0.2942 (3) | 1.0150 (2) | 0.2307 (2) | 0.0250 (6) | |
C12 | 0.1410 (3) | 1.0610 (2) | 0.2646 (2) | 0.0210 (5) | |
O13 | 0.09491 (16) | 0.98866 (15) | 0.22438 (12) | 0.0143 (3) | |
C14 | −0.0504 (2) | 1.0504 (2) | 0.22211 (19) | 0.0182 (5) | |
C15 | −0.0819 (2) | 0.9613 (2) | 0.18275 (19) | 0.0183 (5) | |
O16 | −0.03335 (16) | 0.82085 (16) | 0.24904 (13) | 0.0158 (3) | |
C17 | −0.1311 (2) | 0.7489 (3) | 0.29388 (19) | 0.0236 (5) | |
C18 | −0.0862 (3) | 0.6340 (3) | 0.3892 (2) | 0.0189 (8)* | 0.777 (6) |
C18A | −0.0618 (8) | 0.5992 (6) | 0.3289 (9) | 0.023 (3)* | 0.223 (6) |
O19 | 0.22824 (16) | 0.79333 (17) | 0.09573 (12) | 0.0155 (3) | |
O20 | 0.31546 (16) | 0.57135 (16) | 0.41987 (12) | 0.0154 (3) | |
O21 | 0.07935 (16) | 0.79714 (16) | 0.43348 (12) | 0.0145 (3) | |
Co2 | 0.0000 | 0.5000 | 0.0000 | 0.00891 (8) | |
N21 | 0.0594 (2) | 0.7237 (2) | 0.03509 (16) | 0.0240 (5) | |
N22 | 0.1318 (2) | 0.5971 (2) | −0.23171 (15) | 0.0191 (4) | |
N23 | 0.2878 (2) | 0.3122 (2) | 0.03837 (18) | 0.0276 (5) | |
C21 | 0.0338 (2) | 0.6403 (2) | 0.02316 (17) | 0.0150 (4) | |
C22 | 0.0807 (2) | 0.5597 (2) | −0.14435 (17) | 0.0125 (4) | |
C23 | 0.1778 (2) | 0.3806 (2) | 0.02529 (17) | 0.0156 (5) | |
Co3 | 0.5000 | 0.0000 | 0.5000 | 0.00877 (8) | |
N31 | 0.4334 (2) | −0.0968 (2) | 0.74058 (15) | 0.0203 (4) | |
N32 | 0.1966 (2) | 0.0807 (2) | 0.49815 (16) | 0.0206 (4) | |
N33 | 0.4513 (2) | 0.2934 (2) | 0.49433 (17) | 0.0219 (4) | |
C31 | 0.4576 (2) | −0.0594 (2) | 0.64972 (18) | 0.0138 (4) | |
C32 | 0.3116 (2) | 0.0495 (2) | 0.49810 (17) | 0.0128 (4) | |
C33 | 0.4692 (2) | 0.1811 (2) | 0.49969 (17) | 0.0138 (4) | |
O41 | 0.25167 (17) | 0.70080 (18) | 0.56594 (12) | 0.0196 (4) | |
O42 | 0.43567 (18) | 0.8541 (2) | −0.04606 (13) | 0.0263 (4) | |
H2A | 0.0470 | 0.4881 | 0.2619 | 0.023* | 0.777 (6) |
H2B | 0.0549 | 0.3802 | 0.3772 | 0.023* | 0.777 (6) |
H2C | 0.0632 | 0.3740 | 0.3986 | 0.018* | 0.223 (6) |
H2D | 0.1699 | 0.3865 | 0.4478 | 0.018* | 0.223 (6) |
H3A | 0.2838 | 0.3430 | 0.3524 | 0.028* | 0.777 (6) |
H3B | 0.2638 | 0.3328 | 0.2473 | 0.028* | 0.777 (6) |
H3C | 0.3191 | 0.3137 | 0.3139 | 0.028* | 0.223 (6) |
H3D | 0.2049 | 0.3740 | 0.2443 | 0.028* | 0.223 (6) |
H5A | 0.4121 | 0.5371 | 0.0841 | 0.027* | |
H5B | 0.4523 | 0.3788 | 0.1554 | 0.027* | |
H6A | 0.5411 | 0.4296 | 0.2606 | 0.025* | |
H6B | 0.6118 | 0.4874 | 0.1394 | 0.025* | |
H8A | 0.6459 | 0.6402 | 0.2015 | 0.027* | |
H8B | 0.5440 | 0.6248 | 0.3159 | 0.027* | |
H9A | 0.5413 | 0.8526 | 0.2509 | 0.029* | |
H9B | 0.5120 | 0.8687 | 0.1408 | 0.029* | |
H11A | 0.3210 | 1.0516 | 0.1531 | 0.030* | |
H11B | 0.3337 | 1.0507 | 0.2645 | 0.030* | |
H12A | 0.1132 | 1.0373 | 0.3426 | 0.025* | |
H12B | 0.1010 | 1.1622 | 0.2351 | 0.025* | |
H14A | −0.0704 | 1.1459 | 0.1743 | 0.022* | |
H14B | −0.1066 | 1.0533 | 0.2938 | 0.022* | |
H15A | −0.1826 | 0.9910 | 0.1875 | 0.022* | |
H15B | −0.0341 | 0.9674 | 0.1081 | 0.022* | |
H17A | −0.1343 | 0.7105 | 0.2417 | 0.028* | 0.777 (6) |
H17B | −0.2244 | 0.8127 | 0.3147 | 0.028* | 0.777 (6) |
H17C | −0.1840 | 0.7699 | 0.2407 | 0.028* | 0.223 (6) |
H17D | −0.1971 | 0.7809 | 0.3548 | 0.028* | 0.223 (6) |
H18A | −0.1104 | 0.6724 | 0.4489 | 0.023* | 0.777 (6) |
H18B | −0.1355 | 0.5670 | 0.4103 | 0.023* | 0.777 (6) |
H18C | −0.1271 | 0.5562 | 0.3859 | 0.028* | 0.223 (6) |
H18D | −0.0353 | 0.5602 | 0.2692 | 0.028* | 0.223 (6) |
H19A | 0.1770 | 0.7765 | 0.0690 | 0.042 (3)* | |
H19B | 0.2934 | 0.8064 | 0.0469 | 0.042 (3)* | |
H20A | 0.3079 | 0.6001 | 0.4728 | 0.042 (3)* | |
H20B | 0.3670 | 0.4845 | 0.4351 | 0.042 (3)* | |
H21A | 0.1160 | 0.7859 | 0.4838 | 0.042 (3)* | |
H21B | −0.0065 | 0.8435 | 0.4532 | 0.042 (3)* | |
H41A | 0.2201 | 0.6722 | 0.6290 | 0.042 (3)* | |
H41B | 0.3097 | 0.7295 | 0.5635 | 0.042 (3)* | |
H42A | 0.4302 | 0.8667 | −0.1076 | 0.042 (3)* | |
H42B | 0.5100 | 0.7942 | −0.0436 | 0.042 (3)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Gd1 | 0.00784 (6) | 0.00869 (5) | 0.00750 (5) | −0.00356 (4) | −0.00049 (4) | −0.00167 (4) |
O1 | 0.0161 (8) | 0.0162 (8) | 0.0137 (7) | −0.0097 (7) | −0.0020 (6) | −0.0029 (6) |
C3 | 0.0342 (15) | 0.0135 (11) | 0.0201 (12) | −0.0119 (11) | 0.0009 (11) | −0.0046 (9) |
O4 | 0.0192 (9) | 0.0183 (9) | 0.0354 (10) | −0.0109 (7) | 0.0082 (8) | −0.0155 (8) |
C5 | 0.0220 (13) | 0.0211 (12) | 0.0252 (13) | −0.0065 (11) | 0.0047 (10) | −0.0152 (10) |
C6 | 0.0150 (12) | 0.0176 (12) | 0.0259 (13) | −0.0014 (10) | 0.0010 (10) | −0.0101 (10) |
O7 | 0.0098 (7) | 0.0142 (8) | 0.0174 (8) | −0.0024 (6) | −0.0019 (6) | −0.0069 (6) |
C8 | 0.0139 (12) | 0.0263 (13) | 0.0301 (14) | −0.0070 (10) | −0.0032 (10) | −0.0123 (11) |
C9 | 0.0142 (12) | 0.0278 (13) | 0.0344 (15) | −0.0109 (11) | −0.0002 (10) | −0.0127 (11) |
O10 | 0.0109 (8) | 0.0138 (8) | 0.0300 (9) | −0.0040 (6) | −0.0037 (7) | −0.0083 (7) |
C11 | 0.0231 (13) | 0.0134 (11) | 0.0407 (16) | −0.0076 (10) | −0.0086 (11) | −0.0066 (11) |
C12 | 0.0233 (13) | 0.0112 (11) | 0.0311 (14) | −0.0050 (10) | −0.0085 (11) | −0.0072 (10) |
O13 | 0.0135 (8) | 0.0107 (7) | 0.0180 (8) | −0.0028 (6) | −0.0047 (6) | −0.0034 (6) |
C14 | 0.0147 (11) | 0.0137 (11) | 0.0194 (12) | −0.0005 (9) | −0.0047 (9) | −0.0014 (9) |
C15 | 0.0146 (11) | 0.0165 (11) | 0.0182 (12) | −0.0016 (9) | −0.0077 (9) | 0.0008 (9) |
O16 | 0.0103 (8) | 0.0136 (8) | 0.0225 (8) | −0.0050 (6) | −0.0055 (6) | −0.0013 (6) |
C17 | 0.0134 (12) | 0.0315 (14) | 0.0214 (12) | −0.0131 (11) | −0.0025 (10) | 0.0025 (10) |
O19 | 0.0147 (8) | 0.0252 (9) | 0.0083 (7) | −0.0106 (7) | 0.0003 (6) | −0.0044 (6) |
O20 | 0.0191 (8) | 0.0117 (7) | 0.0121 (8) | −0.0011 (7) | −0.0059 (6) | −0.0021 (6) |
O21 | 0.0097 (8) | 0.0200 (8) | 0.0124 (7) | −0.0013 (6) | −0.0025 (6) | −0.0069 (6) |
Co2 | 0.00843 (19) | 0.01094 (19) | 0.00770 (18) | −0.00513 (16) | −0.00152 (15) | −0.00100 (15) |
N21 | 0.0344 (13) | 0.0270 (11) | 0.0189 (11) | −0.0186 (10) | −0.0061 (9) | −0.0054 (9) |
N22 | 0.0199 (11) | 0.0226 (10) | 0.0149 (10) | −0.0105 (9) | −0.0015 (8) | −0.0034 (8) |
N23 | 0.0158 (11) | 0.0263 (12) | 0.0317 (12) | −0.0054 (9) | −0.0080 (9) | 0.0020 (10) |
C21 | 0.0159 (11) | 0.0184 (11) | 0.0101 (10) | −0.0083 (9) | −0.0017 (8) | −0.0014 (9) |
C22 | 0.0114 (10) | 0.0133 (10) | 0.0147 (11) | −0.0048 (9) | −0.0047 (9) | −0.0036 (8) |
C23 | 0.0156 (12) | 0.0170 (11) | 0.0123 (10) | −0.0085 (10) | −0.0014 (9) | 0.0000 (9) |
Co3 | 0.00643 (19) | 0.00789 (18) | 0.00924 (19) | −0.00176 (15) | −0.00050 (15) | −0.00120 (15) |
N31 | 0.0167 (10) | 0.0264 (11) | 0.0135 (10) | −0.0066 (9) | −0.0012 (8) | −0.0032 (8) |
N32 | 0.0135 (10) | 0.0263 (11) | 0.0191 (10) | −0.0052 (9) | −0.0013 (8) | −0.0068 (9) |
N33 | 0.0232 (11) | 0.0140 (10) | 0.0272 (11) | −0.0048 (9) | −0.0075 (9) | −0.0039 (8) |
C31 | 0.0081 (10) | 0.0126 (10) | 0.0179 (12) | −0.0025 (8) | −0.0006 (8) | −0.0043 (9) |
C32 | 0.0140 (11) | 0.0121 (10) | 0.0102 (10) | −0.0055 (9) | 0.0000 (8) | −0.0018 (8) |
C33 | 0.0104 (10) | 0.0148 (11) | 0.0130 (10) | −0.0031 (9) | −0.0013 (8) | −0.0026 (8) |
O41 | 0.0207 (9) | 0.0316 (10) | 0.0100 (8) | −0.0161 (8) | −0.0014 (6) | −0.0027 (7) |
O42 | 0.0134 (9) | 0.0424 (11) | 0.0132 (8) | −0.0070 (8) | −0.0005 (7) | −0.0018 (8) |
Gd1—O19 | 2.3042 (15) | C14—C15 | 1.488 (3) |
Gd1—O21 | 2.3883 (15) | C14—H14A | 0.99 |
Gd1—O20 | 2.3887 (15) | C14—H14B | 0.99 |
Gd1—O16 | 2.4573 (15) | C15—O16 | 1.450 (3) |
Gd1—O4 | 2.4863 (16) | C15—H15A | 0.99 |
Gd1—O10 | 2.4989 (15) | C15—H15B | 0.99 |
Gd1—O13 | 2.5347 (15) | O16—C17 | 1.425 (3) |
Gd1—O7 | 2.5437 (15) | C17—C18A | 1.465 (5) |
Gd1—O1 | 2.5769 (14) | C17—C18 | 1.504 (3) |
O1—C2A | 1.406 (5) | C17—H17A | 0.99 |
O1—C18 | 1.416 (3) | C17—H17B | 0.99 |
O1—C18A | 1.423 (5) | C17—H17C | 0.99 |
O1—C2 | 1.452 (3) | C17—H17D | 0.99 |
C2—C3 | 1.461 (3) | C18—H18A | 0.99 |
C2—H2A | 0.99 | C18—H18B | 0.99 |
C2—H2B | 0.99 | C18A—H18C | 0.99 |
C2A—C3 | 1.504 (5) | C18A—H18D | 0.99 |
C2A—H2C | 0.99 | O19—H19A | 0.87 |
C2A—H2D | 0.99 | O19—H19B | 0.82 |
C3—O4 | 1.413 (3) | O20—H20A | 0.88 |
C3—H3A | 0.99 | O20—H20B | 0.87 |
C3—H3B | 0.99 | O21—H21A | 0.86 |
C3—H3C | 0.99 | O21—H21B | 0.87 |
C3—H3D | 0.99 | Co2—C22i | 1.889 (2) |
O4—C5 | 1.438 (3) | Co2—C22 | 1.889 (2) |
C5—C6 | 1.486 (4) | Co2—C23i | 1.894 (2) |
C5—H5A | 0.99 | Co2—C23 | 1.894 (2) |
C5—H5B | 0.99 | Co2—C21 | 1.894 (2) |
C6—O7 | 1.446 (3) | Co2—C21i | 1.894 (2) |
C6—H6A | 0.99 | N21—C21 | 1.148 (3) |
C6—H6B | 0.99 | N22—C22 | 1.152 (3) |
O7—C8 | 1.432 (3) | N23—C23 | 1.151 (3) |
C8—C9 | 1.490 (4) | Co3—C33 | 1.889 (2) |
C8—H8A | 0.99 | Co3—C33ii | 1.889 (2) |
C8—H8B | 0.99 | Co3—C32 | 1.894 (2) |
C9—O10 | 1.450 (3) | Co3—C32ii | 1.894 (2) |
C9—H9A | 0.99 | Co3—C31 | 1.895 (2) |
C9—H9B | 0.99 | Co3—C31ii | 1.895 (2) |
O10—C11 | 1.449 (3) | N31—C31 | 1.150 (3) |
C11—C12 | 1.486 (4) | N32—C32 | 1.150 (3) |
C11—H11A | 0.99 | N33—C33 | 1.153 (3) |
C11—H11B | 0.99 | O41—H41A | 0.82 |
C12—O13 | 1.439 (3) | O41—H41B | 0.80 |
C12—H12A | 0.99 | O42—H42A | 0.84 |
C12—H12B | 0.99 | O42—H42B | 0.81 |
O13—C14 | 1.443 (3) | ||
O19—Gd1—O21 | 144.40 (6) | O10—C11—H11A | 109.9 |
O19—Gd1—O20 | 144.12 (6) | C12—C11—H11A | 109.9 |
O21—Gd1—O20 | 70.48 (5) | O10—C11—H11B | 109.9 |
O19—Gd1—O16 | 75.42 (5) | C12—C11—H11B | 109.9 |
O21—Gd1—O16 | 79.20 (5) | H11A—C11—H11B | 108.3 |
O20—Gd1—O16 | 134.84 (5) | O13—C12—C11 | 105.83 (19) |
O19—Gd1—O4 | 74.85 (6) | O13—C12—H12A | 110.6 |
O21—Gd1—O4 | 134.90 (6) | C11—C12—H12A | 110.6 |
O20—Gd1—O4 | 79.77 (6) | O13—C12—H12B | 110.6 |
O16—Gd1—O4 | 100.61 (6) | C11—C12—H12B | 110.6 |
O19—Gd1—O10 | 91.82 (5) | H12A—C12—H12B | 108.7 |
O21—Gd1—O10 | 83.42 (5) | C12—O13—C14 | 112.82 (17) |
O20—Gd1—O10 | 83.16 (5) | C12—O13—Gd1 | 115.41 (13) |
O16—Gd1—O10 | 126.28 (5) | C14—O13—Gd1 | 119.92 (12) |
O4—Gd1—O10 | 126.42 (5) | O13—C14—C15 | 105.97 (18) |
O19—Gd1—O13 | 74.74 (5) | O13—C14—H14A | 110.5 |
O21—Gd1—O13 | 71.67 (5) | C15—C14—H14A | 110.5 |
O20—Gd1—O13 | 131.35 (5) | O13—C14—H14B | 110.5 |
O16—Gd1—O13 | 63.19 (5) | C15—C14—H14B | 110.5 |
O4—Gd1—O13 | 148.37 (6) | H14A—C14—H14B | 108.7 |
O10—Gd1—O13 | 63.11 (5) | O16—C15—C14 | 106.81 (18) |
O19—Gd1—O7 | 74.17 (5) | O16—C15—H15A | 110.4 |
O21—Gd1—O7 | 131.78 (5) | C14—C15—H15A | 110.4 |
O20—Gd1—O7 | 71.91 (5) | O16—C15—H15B | 110.4 |
O16—Gd1—O7 | 148.47 (5) | C14—C15—H15B | 110.4 |
O4—Gd1—O7 | 63.38 (5) | H15A—C15—H15B | 108.6 |
O10—Gd1—O7 | 63.05 (5) | C17—O16—C15 | 115.79 (17) |
O13—Gd1—O7 | 115.49 (5) | C17—O16—Gd1 | 125.58 (13) |
O19—Gd1—O1 | 110.22 (5) | C15—O16—Gd1 | 118.62 (12) |
O21—Gd1—O1 | 78.83 (5) | O16—C17—C18A | 111.0 (4) |
O20—Gd1—O1 | 78.68 (5) | O16—C17—C18 | 107.74 (19) |
O16—Gd1—O1 | 62.88 (5) | O16—C17—H17A | 110.2 |
O4—Gd1—O1 | 62.32 (5) | C18—C17—H17A | 110.2 |
O10—Gd1—O1 | 157.96 (5) | O16—C17—H17B | 110.2 |
O13—Gd1—O1 | 121.95 (5) | C18—C17—H17B | 110.2 |
O7—Gd1—O1 | 121.47 (5) | H17A—C17—H17B | 108.5 |
C2A—O1—C18A | 108.7 (5) | O16—C17—H17C | 109.4 |
C18—O1—C2 | 111.3 (2) | C18A—C17—H17C | 109.4 |
C2A—O1—Gd1 | 117.4 (3) | O16—C17—H17D | 109.4 |
C18—O1—Gd1 | 114.62 (14) | C18A—C17—H17D | 109.4 |
C18A—O1—Gd1 | 118.2 (4) | H17C—C17—H17D | 108.0 |
C2—O1—Gd1 | 117.66 (14) | O1—C18—C17 | 110.4 (2) |
O1—C2—C3 | 109.5 (2) | O1—C18—H18A | 109.6 |
O1—C2—H2A | 109.8 | C17—C18—H18A | 109.6 |
C3—C2—H2A | 109.8 | O1—C18—H18B | 109.6 |
O1—C2—H2B | 109.8 | C17—C18—H18B | 109.6 |
C3—C2—H2B | 109.8 | H18A—C18—H18B | 108.1 |
H2A—C2—H2B | 108.2 | O1—C18A—C17 | 112.3 (4) |
O1—C2A—C3 | 109.6 (4) | O1—C18A—H18C | 109.2 |
O1—C2A—H2C | 109.8 | C17—C18A—H18C | 109.2 |
C3—C2A—H2C | 109.8 | O1—C18A—H18D | 109.2 |
O1—C2A—H2D | 109.8 | C17—C18A—H18D | 109.2 |
C3—C2A—H2D | 109.8 | H18C—C18A—H18D | 107.9 |
H2C—C2A—H2D | 108.2 | Gd1—O19—H19A | 119.5 |
O4—C3—C2 | 107.6 (2) | Gd1—O19—H19B | 131.7 |
O4—C3—C2A | 114.1 (3) | H19A—O19—H19B | 105.1 |
O4—C3—H3A | 110.2 | Gd1—O20—H20A | 120.0 |
C2—C3—H3A | 110.2 | Gd1—O20—H20B | 134.8 |
O4—C3—H3B | 110.2 | H20A—O20—H20B | 105.2 |
C2—C3—H3B | 110.2 | Gd1—O21—H21A | 124.9 |
H3A—C3—H3B | 108.5 | Gd1—O21—H21B | 132.2 |
O4—C3—H3C | 108.7 | H21A—O21—H21B | 102.7 |
C2A—C3—H3C | 108.7 | C22i—Co2—C22 | 180.00 (19) |
O4—C3—H3D | 108.7 | C22i—Co2—C23i | 88.93 (9) |
C2A—C3—H3D | 108.7 | C22—Co2—C23i | 91.07 (9) |
H3C—C3—H3D | 107.6 | C22i—Co2—C23 | 91.07 (9) |
C3—O4—C5 | 116.14 (18) | C22—Co2—C23 | 88.93 (9) |
C3—O4—Gd1 | 123.01 (14) | C23i—Co2—C23 | 180.00 (15) |
C5—O4—Gd1 | 118.33 (13) | C22i—Co2—C21 | 91.47 (9) |
O4—C5—C6 | 108.12 (19) | C22—Co2—C21 | 88.53 (9) |
O4—C5—H5A | 110.1 | C23i—Co2—C21 | 91.72 (10) |
C6—C5—H5A | 110.1 | C23—Co2—C21 | 88.28 (10) |
O4—C5—H5B | 110.1 | C22i—Co2—C21i | 88.53 (9) |
C6—C5—H5B | 110.1 | C22—Co2—C21i | 91.47 (9) |
H5A—C5—H5B | 108.4 | C23i—Co2—C21i | 88.28 (10) |
O7—C6—C5 | 106.04 (19) | C23—Co2—C21i | 91.72 (10) |
O7—C6—H6A | 110.5 | C21—Co2—C21i | 180.00 (12) |
C5—C6—H6A | 110.5 | N21—C21—Co2 | 177.4 (2) |
O7—C6—H6B | 110.5 | N22—C22—Co2 | 178.45 (19) |
C5—C6—H6B | 110.5 | N23—C23—Co2 | 177.4 (2) |
H6A—C6—H6B | 108.7 | C33—Co3—C33ii | 180.0 |
C8—O7—C6 | 112.16 (18) | C33—Co3—C32 | 90.05 (9) |
C8—O7—Gd1 | 115.27 (13) | C33ii—Co3—C32 | 89.95 (9) |
C6—O7—Gd1 | 119.24 (13) | C33—Co3—C32ii | 89.95 (9) |
O7—C8—C9 | 106.1 (2) | C33ii—Co3—C32ii | 90.05 (9) |
O7—C8—H8A | 110.5 | C32—Co3—C32ii | 180.00 (14) |
C9—C8—H8A | 110.5 | C33—Co3—C31 | 91.50 (9) |
O7—C8—H8B | 110.5 | C33ii—Co3—C31 | 88.50 (9) |
C9—C8—H8B | 110.5 | C32—Co3—C31 | 89.97 (9) |
H8A—C8—H8B | 108.7 | C32ii—Co3—C31 | 90.03 (9) |
O10—C9—C8 | 108.49 (19) | C33—Co3—C31ii | 88.50 (9) |
O10—C9—H9A | 110.0 | C33ii—Co3—C31ii | 91.50 (9) |
C8—C9—H9A | 110.0 | C32—Co3—C31ii | 90.03 (9) |
O10—C9—H9B | 110.0 | C32ii—Co3—C31ii | 89.97 (9) |
C8—C9—H9B | 110.0 | C31—Co3—C31ii | 180.0 |
H9A—C9—H9B | 108.4 | N31—C31—Co3 | 179.1 (2) |
C11—O10—C9 | 107.47 (18) | N32—C32—Co3 | 178.9 (2) |
C11—O10—Gd1 | 121.04 (13) | N33—C33—Co3 | 176.7 (2) |
C9—O10—Gd1 | 121.22 (13) | H41A—O41—H41B | 105.4 |
O10—C11—C12 | 108.82 (19) | H42A—O42—H42B | 100.2 |
O19—Gd1—O1—C2A | 91.0 (4) | O10—Gd1—O7—C6 | 167.04 (17) |
O21—Gd1—O1—C2A | −124.9 (4) | O13—Gd1—O7—C6 | −156.53 (15) |
O20—Gd1—O1—C2A | −52.8 (4) | O1—Gd1—O7—C6 | 11.81 (17) |
O16—Gd1—O1—C2A | 151.6 (4) | C6—O7—C8—C9 | 164.81 (19) |
O4—Gd1—O1—C2A | 31.5 (4) | Gd1—O7—C8—C9 | −54.3 (2) |
O10—Gd1—O1—C2A | −87.9 (4) | O7—C8—C9—O10 | 51.8 (3) |
O13—Gd1—O1—C2A | 175.2 (4) | C8—C9—O10—C11 | −174.4 (2) |
O7—Gd1—O1—C2A | 7.6 (4) | C8—C9—O10—Gd1 | −29.0 (3) |
O19—Gd1—O1—C18 | −87.30 (17) | O19—Gd1—O10—C11 | 70.95 (18) |
O21—Gd1—O1—C18 | 56.84 (17) | O21—Gd1—O10—C11 | −73.66 (17) |
O20—Gd1—O1—C18 | 128.91 (17) | O20—Gd1—O10—C11 | −144.70 (18) |
O16—Gd1—O1—C18 | −26.65 (16) | O16—Gd1—O10—C11 | −2.24 (19) |
O4—Gd1—O1—C18 | −146.80 (18) | O4—Gd1—O10—C11 | 143.41 (17) |
O10—Gd1—O1—C18 | 93.8 (2) | O13—Gd1—O10—C11 | −0.91 (16) |
O13—Gd1—O1—C18 | −3.09 (18) | O7—Gd1—O10—C11 | 142.15 (19) |
O7—Gd1—O1—C18 | −170.68 (16) | O1—Gd1—O10—C11 | −110.1 (2) |
O19—Gd1—O1—C18A | −42.5 (5) | O19—Gd1—O10—C9 | −69.81 (17) |
O21—Gd1—O1—C18A | 101.6 (5) | O21—Gd1—O10—C9 | 145.58 (17) |
O20—Gd1—O1—C18A | 173.7 (5) | O20—Gd1—O10—C9 | 74.54 (17) |
O16—Gd1—O1—C18A | 18.2 (5) | O16—Gd1—O10—C9 | −143.00 (16) |
O4—Gd1—O1—C18A | −102.0 (5) | O4—Gd1—O10—C9 | 2.64 (19) |
O10—Gd1—O1—C18A | 138.6 (5) | O13—Gd1—O10—C9 | −141.67 (18) |
O13—Gd1—O1—C18A | 41.7 (5) | O7—Gd1—O10—C9 | 1.39 (16) |
O7—Gd1—O1—C18A | −125.9 (5) | O1—Gd1—O10—C9 | 109.1 (2) |
O19—Gd1—O1—C2 | 46.41 (18) | C9—O10—C11—C12 | 174.1 (2) |
O21—Gd1—O1—C2 | −169.45 (18) | Gd1—O10—C11—C12 | 28.7 (3) |
O20—Gd1—O1—C2 | −97.38 (17) | O10—C11—C12—O13 | −51.5 (3) |
O16—Gd1—O1—C2 | 107.06 (18) | C11—C12—O13—C14 | −162.51 (19) |
O4—Gd1—O1—C2 | −13.09 (17) | C11—C12—O13—Gd1 | 54.5 (2) |
O10—Gd1—O1—C2 | −132.48 (18) | O19—Gd1—O13—C12 | −129.52 (15) |
O13—Gd1—O1—C2 | 130.62 (17) | O21—Gd1—O13—C12 | 62.45 (15) |
O7—Gd1—O1—C2 | −36.97 (18) | O20—Gd1—O13—C12 | 21.96 (17) |
C2A—O1—C2—C3 | −62.0 (5) | O16—Gd1—O13—C12 | 149.37 (16) |
C18—O1—C2—C3 | 173.5 (2) | O4—Gd1—O13—C12 | −145.91 (15) |
C18A—O1—C2—C3 | 153.3 (5) | O10—Gd1—O13—C12 | −29.43 (14) |
Gd1—O1—C2—C3 | 38.4 (3) | O7—Gd1—O13—C12 | −65.84 (15) |
C18—O1—C2A—C3 | 136.0 (4) | O1—Gd1—O13—C12 | 125.88 (14) |
C18A—O1—C2A—C3 | 95.5 (8) | O19—Gd1—O13—C14 | 90.24 (15) |
C2—O1—C2A—C3 | 59.1 (4) | O21—Gd1—O13—C14 | −77.79 (15) |
Gd1—O1—C2A—C3 | −42.0 (8) | O20—Gd1—O13—C14 | −118.29 (15) |
O1—C2—C3—O4 | −48.5 (3) | O16—Gd1—O13—C14 | 9.13 (14) |
O1—C2—C3—C2A | 58.4 (4) | O4—Gd1—O13—C14 | 73.85 (18) |
O1—C2A—C3—O4 | 26.1 (8) | O10—Gd1—O13—C14 | −169.67 (16) |
O1—C2A—C3—C2 | −61.8 (5) | O7—Gd1—O13—C14 | 153.92 (14) |
C2—C3—O4—C5 | −157.0 (2) | O1—Gd1—O13—C14 | −14.36 (16) |
C2A—C3—O4—C5 | 163.0 (5) | C12—O13—C14—C15 | −177.99 (18) |
C2—C3—O4—Gd1 | 41.3 (3) | Gd1—O13—C14—C15 | −36.8 (2) |
C2A—C3—O4—Gd1 | 1.3 (5) | O13—C14—C15—O16 | 53.0 (2) |
O19—Gd1—O4—C3 | −139.28 (19) | C14—C15—O16—C17 | 128.5 (2) |
O21—Gd1—O4—C3 | 17.6 (2) | C14—C15—O16—Gd1 | −50.9 (2) |
O20—Gd1—O4—C3 | 66.33 (18) | O19—Gd1—O16—C17 | 123.76 (18) |
O16—Gd1—O4—C3 | −67.71 (19) | O21—Gd1—O16—C17 | −81.42 (18) |
O10—Gd1—O4—C3 | 139.86 (17) | O20—Gd1—O16—C17 | −33.4 (2) |
O13—Gd1—O4—C3 | −122.90 (18) | O4—Gd1—O16—C17 | 52.64 (18) |
O7—Gd1—O4—C3 | 141.1 (2) | O10—Gd1—O16—C17 | −154.88 (17) |
O1—Gd1—O4—C3 | −16.17 (17) | O13—Gd1—O16—C17 | −156.21 (19) |
O19—Gd1—O4—C5 | 59.44 (17) | O7—Gd1—O16—C17 | 108.14 (19) |
O21—Gd1—O4—C5 | −143.72 (16) | O1—Gd1—O16—C17 | 1.46 (17) |
O20—Gd1—O4—C5 | −94.95 (18) | O19—Gd1—O16—C15 | −56.87 (15) |
O16—Gd1—O4—C5 | 131.01 (17) | O21—Gd1—O16—C15 | 97.94 (15) |
O10—Gd1—O4—C5 | −21.4 (2) | O20—Gd1—O16—C15 | 145.92 (14) |
O13—Gd1—O4—C5 | 75.8 (2) | O4—Gd1—O16—C15 | −128.00 (15) |
O7—Gd1—O4—C5 | −20.17 (16) | O10—Gd1—O16—C15 | 24.48 (17) |
O1—Gd1—O4—C5 | −177.45 (19) | O13—Gd1—O16—C15 | 23.15 (14) |
C3—O4—C5—C6 | −114.3 (2) | O7—Gd1—O16—C15 | −72.50 (18) |
Gd1—O4—C5—C6 | 48.3 (2) | O1—Gd1—O16—C15 | −179.18 (16) |
O4—C5—C6—O7 | −53.6 (2) | C15—O16—C17—C18A | 161.4 (5) |
C5—C6—O7—C8 | 178.14 (19) | Gd1—O16—C17—C18A | −19.2 (5) |
C5—C6—O7—Gd1 | 39.0 (2) | C15—O16—C17—C18 | −158.2 (2) |
O19—Gd1—O7—C8 | 129.55 (15) | Gd1—O16—C17—C18 | 21.2 (3) |
O21—Gd1—O7—C8 | −22.10 (17) | C2A—O1—C18—C17 | −130.0 (5) |
O20—Gd1—O7—C8 | −62.35 (15) | C18A—O1—C18—C17 | −57.1 (5) |
O16—Gd1—O7—C8 | 145.26 (14) | C2—O1—C18—C17 | −88.5 (3) |
O4—Gd1—O7—C8 | −149.76 (16) | Gd1—O1—C18—C17 | 48.1 (3) |
O10—Gd1—O7—C8 | 29.11 (14) | O16—C17—C18—O1 | −43.6 (3) |
O13—Gd1—O7—C8 | 65.54 (16) | C18A—C17—C18—O1 | 58.0 (5) |
O1—Gd1—O7—C8 | −126.12 (14) | C2A—O1—C18A—C17 | −172.0 (6) |
O19—Gd1—O7—C6 | −92.52 (15) | C18—O1—C18A—C17 | 60.8 (5) |
O21—Gd1—O7—C6 | 115.83 (15) | C2—O1—C18A—C17 | −149.2 (9) |
O20—Gd1—O7—C6 | 75.58 (15) | Gd1—O1—C18A—C17 | −34.9 (10) |
O16—Gd1—O7—C6 | −76.81 (18) | O16—C17—C18A—O1 | 33.6 (9) |
O4—Gd1—O7—C6 | −11.83 (15) | C18—C17—C18A—O1 | −58.7 (5) |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O19—H19A···N21 | 0.87 | 1.85 | 2.717 (3) | 170 |
O19—H19B···O42 | 0.82 | 1.78 | 2.594 (2) | 169 |
O20—H20A···O41 | 0.88 | 1.83 | 2.680 (2) | 163 |
O20—H20B···N33 | 0.87 | 1.89 | 2.748 (3) | 168 |
O21—H21A···O41 | 0.86 | 1.88 | 2.687 (2) | 155 |
O21—H21B···N32iii | 0.87 | 1.87 | 2.730 (3) | 172 |
O41—H41A···N22iv | 0.82 | 1.89 | 2.708 (2) | 172 |
O41—H41B···N33v | 0.80 | 2.38 | 3.072 (3) | 145 |
O42—H42A···N31vi | 0.84 | 2.00 | 2.830 (3) | 174 |
O42—H42B···N23vii | 0.81 | 2.03 | 2.813 (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, z−1; (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 |
Mr | 724.50 | 728.62 | 716.71 | 718.32 |
Crystal system, space group | Monoclinic, C2/c | Monoclinic, C2/c | Triclinic, P1 | Triclinic, P1 |
Temperature (K) | 120 | 120 | 120 | 120 |
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), 90 | 90, 113.4189 (11), 90 | 67.9012 (13), 70.7291 (13), 65.7231 (14) | 67.8201 (18), 70.635 (2), 65.743 (2) |
V (Å3) | 2957.09 (13) | 2943.55 (12) | 1404.77 (6) | 1400.57 (8) |
Z | 4 | 4 | 2 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 2.07 | 2.30 | 2.65 | 2.80 |
Crystal size (mm) | 0.20 × 0.10 × 0.10 | 0.34 × 0.34 × 0.25 | 0.10 × 0.06 × 0.04 | 0.25 × 0.20 × 0.20 |
Data collection | ||||
Diffractometer | Bruker–Nonius KappaCCD diffractometer | Bruker–Nonius KappaCCD diffractometer | Bruker–Nonius KappaCCD diffractometer | Bruker–Nonius KappaCCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2003) | Multi-scan (SADABS; Sheldrick, 2003) | Multi-scan (SADABS; Sheldrick, 2003) | Multi-scan (SADABS; Sheldrick, 2003) |
Tmin, Tmax | 0.682, 0.820 | 0.478, 0.561 | 0.836, 0.900 | 0.509, 0.568 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 15557, 3385, 3079 | 21701, 3360, 3168 | 28348, 6453, 5624 | 27604, 6420, 5973 |
Rint | 0.036 | 0.031 | 0.050 | 0.060 |
(sin θ/λ)max (Å−1) | 0.650 | 0.650 | 0.650 | 0.652 |
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 reflections | 3385 | 3360 | 6453 | 6420 |
No. of parameters | 176 | 176 | 334 | 334 |
No. of restraints | 0 | 0 | 8 | 8 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained | H-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 Å−3) | 0.81, −0.87 | 0.83, −1.07 | 0.95, −0.91 | 11.43, −3.03 |
(V) | (VII) | |
Crystal data | ||
Chemical formula | [Gd(C12H24O6)(H2O)3][Cr(CN)6]·2H2O | [Gd(C12H24O6)(H2O)3][Co(CN)6]·2H2O |
Mr | 719.76 | 726.69 |
Crystal system, space group | Triclinic, P1 | Triclinic, P1 |
Temperature (K) | 120 | 120 |
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) |
V (Å3) | 1450.92 (5) | 1385.20 (5) |
Z | 2 | 2 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 2.70 | 3.03 |
Crystal size (mm) | 0.16 × 0.15 × 0.04 | 0.60 × 0.54 × 0.42 |
Data collection | ||
Diffractometer | Bruker–Nonius KappaCCD diffractometer | Bruker–Nonius KappaCCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2003) | Multi-scan (SADABS; Sheldrick, 2003) |
Tmin, Tmax | 0.672, 0.899 | 0.187, 0.280 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 34884, 6646, 6382 | 27907, 6348, 6022 |
Rint | 0.038 | 0.033 |
(sin θ/λ)max (Å−1) | 0.650 | 0.651 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.040, 0.108, 1.04 | 0.020, 0.047, 1.09 |
No. of reflections | 6646 | 6348 |
No. of parameters | 334 | 334 |
No. of restraints | 8 | 8 |
H-atom treatment | H-atom parameters constrained | H-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 Å−3) | 3.60, −1.63 | 1.00, −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).
D—H···A | D—H | H···A | D···A | D—H···A |
O19—H19A···O21i | 0.81 | 1.91 | 2.700 (2) | 163 |
O19—H19B···N11 | 0.81 | 2.14 | 2.917 (2) | 161 |
O20—H20A···O21ii | 0.82 | 1.96 | 2.768 (2) | 168 |
O20—H20B···N12iii | 0.82 | 1.92 | 2.739 (2) | 171 |
O21—H21A···N13ii | 0.82 | 1.94 | 2.757 (2) | 173 |
O21—H21B···N11 | 0.82 | 2.07 | 2.888 (2) | 175 |
Symmetry codes: (i) −x, −y+1, −z; (ii) x, −y+1, z+1/2; (iii) x, −y, z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O19—H19A···O21i | 0.81 | 1.92 | 2.697 (2) | 161 |
O19—H19B···N11 | 0.84 | 2.09 | 2.904 (2) | 161 |
O20—H20A···O21ii | 0.83 | 1.96 | 2.773 (2) | 166 |
O20—H20B···N12iii | 0.84 | 1.90 | 2.734 (2) | 169 |
O21—H21A···N13ii | 0.83 | 1.93 | 2.753 (2) | 173 |
O21—H21B···N11 | 0.80 | 2.10 | 2.893 (2) | 175 |
Symmetry codes: (i) −x, −y+1, −z; (ii) x, −y+1, z+1/2; (iii) x, −y, z+1/2. |
Distance | (I) | (II) |
Ln1—O1 | 2.5784 (13) | 2.5515 (12) |
Ln1—O4 | 2.6811 (14) | 2.6620 (13) |
Ln1—O7 | 2.5619 (13) | 2.5312 (12) |
Ln1—O19 | 2.5389 (14) | 2.5062 (12) |
Ln1—O20 | 2.4962 (14) | 2.4615 (12) |
Distance | (III) | (IV) | (V) | (VI) | (VII) |
Ln1—O1 | 2.602 (2) | 2.590 (5) | 2.581 (3) | 2.5790 (17) | 2.5769 (14) |
Ln1—O4 | 2.505 (2) | 2.502 (6) | 2.489 (4) | 2.4882 (19) | 2.4863 (16) |
Ln1—O7 | 2.563 (2) | 2.553 (5) | 2.548 (3) | 2.5476 (17) | 2.5437 (15) |
Ln1—O10 | 2.529 (2) | 2.511 (5) | 2.504 (3) | 2.5007 (17) | 2.4989 (15) |
Ln1—O13 | 2.552 (2) | 2.550 (5) | 2.543 (3) | 2.5361 (17) | 2.5347 (15) |
Ln1—O16 | 2.481 (2) | 2.467 (6) | 2.476 (3) | 2.4608 (17) | 2.4573 (15) |
Ln1—O19 | 2.327 (2) | 2.318 (6) | 2.307 (3) | 2.3088 (17) | 2.3042 (15) |
Ln1—O20 | 2.409 (2) | 2.405 (5) | 2.381 (3) | 2.3884 (17) | 2.3887 (15) |
Ln1—O21 | 2.408 (2) | 2.392 (5) | 2.377 (3) | 2.3881 (17) | 2.3883 (15) |
Data for compound (VI) are taken from Koner et al. (2005). |
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+g−g+g−g+g+ in (I) and (II), and g−g−g+g−g+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.