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Three new metal-organic framework structures containing EuIII and the little explored methanetriacetate (C7H7O63-, mta3-) ligand have been synthesized. Gel synthesis yields a two-dimensional framework with the formula [Eu(mta)(H2O)3]n·2nH2O, (I), while two polymorphs of the three-dimensional framework material [Eu(mta)(H2O)]n·nH2O, (II) and (III), are obtained through hydrothermal synthesis at either 423 or 443 K. Compounds (I) and (II) are isomorphous with previously reported GdIII compounds, but compound (III) constitutes a new phase. Compound (I) can be described in terms of dinuclear [Eu2(H2O)4]6+ units bonded through mta3- ligands to form a two-dimensional framework with topology corresponding to a (6,3)-connected binodal (43)(466683)-kgd net, where the dinuclear [Eu2(H2O)4]6+ units are considered as a single node. Compounds (II) and (III) have distinct three-dimensional topologies, namely a (41263)(4966)-nia net for (II) and a (41065)(41164)-K2O2; 36641 net for (III). The crystal density of (III) is greater than that of (II), consistent with the increase of temperature, and thereby autogeneous pressure, in the hydrothermal synthesis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520613034550/bi5013sup1.cif
Contains datablocks I, II, III, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520613034550/bi5013Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520613034550/bi5013IIsup3.hkl
Contains datablock II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520613034550/bi5013IIIsup4.hkl
Contains datablock iii_adb

CCDC references: 978533; 978534; 978535

Computing details top

Data collection: COLLECT (Nonius, 1998) for (I), (III); Collect (Nonius, 1998) for (II). Cell refinement: EVALCCD for (I); HKL-2000 for (II), (III). Data reduction: EVALCCD (Duisenberg et al., 2003) for (I); HKL-2000 (Otwinowski & Minor, 1997) for (II), (III). For all compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008). Molecular graphics: DIAMOND (Brandenburg, 1999) for (I), (III); ORTEP-3 for Windows (Farrugia, 1997) for (II). Software used to prepare material for publication: WinGX (Farrugia, 1999), PARST95 (Nardelli, 1995) and PLATON (Spek, 2009) for (I), (III); WinGX (Farrugia, 1999) for (II).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
(I) top
Crystal data top
C7H13EuO9·2(H2O)Z = 2
Mr = 429.17F(000) = 420
Triclinic, P1Dx = 2.216 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.0917 (13) ÅCell parameters from 2943 reflections
b = 8.8680 (12) Åθ = 4.0–27.5°
c = 10.115 (2) ŵ = 4.93 mm1
α = 86.994 (17)°T = 293 K
β = 73.002 (16)°Needle, colourless
γ = 68.172 (15)°0.80 × 0.40 × 0.20 mm
V = 643.06 (19) Å3
Data collection top
Nonius KappaCCD
diffractometer
2943 independent reflections
Radiation source: fine-focus sealed tube2743 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
Detector resolution: 9 pixels mm-1θmax = 27.5°, θmin = 4.0°
thick–slice ω– and φ–scansh = 1010
Absorption correction: for a sphere
Dwiggins (1975)
k = 1111
Tmin = 0.110, Tmax = 0.439l = 1313
10427 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.059H-atom parameters constrained
S = 1.10 w = 1/[σ2(Fo2) + (0.0304P)2 + 0.1604P]
where P = (Fo2 + 2Fc2)/3
2943 reflections(Δ/σ)max < 0.001
172 parametersΔρmax = 1.28 e Å3
0 restraintsΔρmin = 0.56 e Å3
Crystal data top
C7H13EuO9·2(H2O)γ = 68.172 (15)°
Mr = 429.17V = 643.06 (19) Å3
Triclinic, P1Z = 2
a = 8.0917 (13) ÅMo Kα radiation
b = 8.8680 (12) ŵ = 4.93 mm1
c = 10.115 (2) ÅT = 293 K
α = 86.994 (17)°0.80 × 0.40 × 0.20 mm
β = 73.002 (16)°
Data collection top
Nonius KappaCCD
diffractometer
2943 independent reflections
Absorption correction: for a sphere
Dwiggins (1975)
2743 reflections with I > 2σ(I)
Tmin = 0.110, Tmax = 0.439Rint = 0.042
10427 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0240 restraints
wR(F2) = 0.059H-atom parameters constrained
S = 1.10Δρmax = 1.28 e Å3
2943 reflectionsΔρmin = 0.56 e Å3
172 parameters
Special details top

Experimental. Interpolation using International Tables Vol. C (1992) p. 523, Table 6.3.3.3 for values of muR in the range 0–2.5, and International Tables Vol. II (1959) p. 302, Table 5.3.6B for muR in the range 2.6–10.0. The interpolation procedure of C. W. Dwiggins Jr [Acta Cryst. (1975) A31, 146–148] is used with some modification.

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

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Eu10.064805 (19)0.706924 (17)0.100355 (16)0.02372 (7)
O10.0672 (3)0.5617 (3)0.0934 (2)0.0308 (5)
O1W0.2527 (3)0.9760 (3)0.0417 (3)0.0340 (5)
H1W0.20451.04780.02180.051*
H2W0.28840.97960.13100.051*
O20.1297 (3)0.7759 (3)0.0245 (3)0.0329 (5)
O2W0.3580 (3)0.8204 (4)0.1609 (3)0.0454 (7)
H3W0.44850.88850.10040.068*
H4W0.40550.80260.22010.068*
O30.0179 (3)1.0930 (3)0.2256 (3)0.0357 (5)
O3W0.0128 (4)0.6244 (3)0.3411 (3)0.0388 (6)
H5W0.08300.65930.39320.058*
H6W0.06740.53310.37950.058*
O40.1733 (3)0.9380 (3)0.3183 (3)0.0403 (6)
O50.6901 (3)0.7005 (3)0.1023 (3)0.0409 (6)
O60.7402 (3)0.4677 (3)0.2081 (2)0.0299 (5)
C10.1506 (4)0.6562 (4)0.0977 (3)0.0266 (6)
C20.2733 (5)0.6205 (4)0.1897 (4)0.0335 (8)
H2A0.39490.54290.13940.040*
H2B0.22280.56740.26870.040*
C30.3011 (4)0.7636 (4)0.2442 (3)0.0272 (6)
H30.33440.82730.16590.033*
C40.0324 (4)0.9747 (4)0.2945 (3)0.0275 (6)
C50.1274 (5)0.8759 (4)0.3513 (4)0.0346 (8)
H5A0.08400.81060.42280.042*
H5B0.16140.95040.39460.042*
C60.6463 (4)0.6155 (4)0.1980 (4)0.0272 (6)
C70.4628 (4)0.6990 (4)0.3075 (4)0.0295 (7)
H7A0.46920.78860.35420.035*
H7B0.44050.62250.37600.035*
O4W0.5470 (3)0.2555 (3)0.3264 (3)0.0406 (6)
H7W0.61020.31540.30020.061*
H8W0.62710.15970.32280.061*
O5W0.2117 (3)0.6850 (3)0.4707 (3)0.0385 (6)
H9W0.21000.77160.43120.058*
H10W0.32300.70930.52240.058*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Eu10.02339 (9)0.02241 (10)0.02717 (10)0.00904 (7)0.00950 (7)0.00192 (6)
O10.0371 (12)0.0301 (12)0.0345 (13)0.0176 (10)0.0179 (11)0.0041 (10)
O1W0.0353 (12)0.0310 (12)0.0365 (14)0.0160 (10)0.0064 (11)0.0005 (10)
O20.0437 (13)0.0294 (12)0.0361 (14)0.0191 (10)0.0207 (12)0.0064 (10)
O2W0.0305 (13)0.0550 (17)0.0465 (16)0.0042 (12)0.0181 (12)0.0120 (13)
O30.0378 (13)0.0296 (12)0.0404 (15)0.0145 (10)0.0109 (11)0.0078 (11)
O3W0.0429 (14)0.0368 (14)0.0331 (14)0.0050 (11)0.0187 (12)0.0006 (11)
O40.0329 (13)0.0430 (14)0.0492 (16)0.0188 (11)0.0141 (12)0.0141 (12)
O50.0323 (13)0.0335 (13)0.0466 (16)0.0087 (11)0.0023 (12)0.0090 (12)
O60.0256 (11)0.0276 (12)0.0331 (13)0.0070 (9)0.0069 (10)0.0007 (10)
C10.0254 (14)0.0232 (15)0.0315 (17)0.0091 (12)0.0077 (13)0.0032 (13)
C20.0359 (18)0.0262 (16)0.046 (2)0.0119 (14)0.0233 (16)0.0044 (15)
C30.0285 (15)0.0283 (16)0.0261 (16)0.0110 (13)0.0091 (13)0.0003 (13)
C40.0280 (15)0.0232 (15)0.0267 (16)0.0052 (12)0.0066 (13)0.0005 (12)
C50.0315 (17)0.0333 (18)0.0351 (19)0.0048 (14)0.0134 (15)0.0002 (14)
C60.0239 (14)0.0281 (16)0.0327 (17)0.0104 (12)0.0114 (13)0.0015 (13)
C70.0247 (15)0.0356 (18)0.0276 (16)0.0082 (13)0.0101 (13)0.0035 (13)
O4W0.0296 (12)0.0400 (14)0.0491 (16)0.0116 (11)0.0091 (12)0.0038 (12)
O5W0.0365 (13)0.0382 (14)0.0398 (14)0.0126 (11)0.0126 (11)0.0069 (11)
Geometric parameters (Å, º) top
Eu1—O3i2.314 (2)O5—C61.245 (4)
Eu1—O1ii2.386 (2)O5—Eu1v2.415 (2)
Eu1—O5iii2.415 (2)O6—C61.264 (4)
Eu1—O6iv2.442 (2)O6—Eu1iv2.442 (2)
Eu1—O3W2.450 (3)C1—C21.492 (5)
Eu1—O2W2.455 (3)C2—C31.524 (5)
Eu1—O22.530 (2)C2—H2A0.9700
Eu1—O1W2.541 (2)C2—H2B0.9700
Eu1—O12.565 (2)C3—C51.524 (5)
Eu1—Eu1ii4.0363 (8)C3—C71.531 (4)
O1—C11.266 (4)C3—H30.9800
O1—Eu1ii2.386 (2)C4—C51.520 (5)
O1W—H1W0.85C5—H5A0.9700
O1W—H2W0.86C5—H5B0.9700
O2—C11.249 (4)C6—C71.512 (5)
O2W—H3W0.85C7—H7A0.9700
O2W—H4W0.85C7—H7B0.9700
O3—C41.251 (4)O4W—H7W0.85
O3—Eu1i2.314 (2)O4W—H8W0.85
O3W—H5W0.85O5W—H9W0.85
O3W—H6W0.85O5W—H10W0.85
O4—C41.253 (4)
O3i—Eu1—O1ii149.31 (9)Eu1—O1W—H2W121.1
O3i—Eu1—O5iii135.97 (9)H1W—O1W—H2W104.9
O1ii—Eu1—O5iii72.17 (9)C1—O2—Eu195.95 (19)
O3i—Eu1—O6iv84.38 (8)Eu1—O2W—H3W115.0
O1ii—Eu1—O6iv75.71 (8)Eu1—O2W—H4W139.0
O5iii—Eu1—O6iv135.75 (8)H3W—O2W—H4W105.1
O3i—Eu1—O3W76.20 (9)C4—O3—Eu1i169.4 (2)
O1ii—Eu1—O3W74.92 (9)Eu1—O3W—H5W130.1
O5iii—Eu1—O3W128.23 (10)Eu1—O3W—H6W122.4
O6iv—Eu1—O3W68.73 (8)H5W—O3W—H6W105.1
O3i—Eu1—O2W87.04 (10)C6—O5—Eu1v144.1 (2)
O1ii—Eu1—O2W92.60 (9)C6—O6—Eu1iv132.9 (2)
O5iii—Eu1—O2W72.90 (9)O2—C1—O1119.5 (3)
O6iv—Eu1—O2W138.60 (9)O2—C1—C2121.7 (3)
O3W—Eu1—O2W69.89 (9)O1—C1—C2118.8 (3)
O3i—Eu1—O275.45 (8)O2—C1—Eu159.01 (17)
O1ii—Eu1—O2118.99 (8)O1—C1—Eu160.64 (17)
O5iii—Eu1—O297.31 (9)C2—C1—Eu1175.3 (2)
O6iv—Eu1—O272.76 (8)C1—C2—C3117.5 (3)
O3W—Eu1—O2133.73 (9)C1—C2—H2A107.9
O2W—Eu1—O2142.86 (9)C3—C2—H2A107.9
O3i—Eu1—O1W72.10 (9)C1—C2—H2B107.9
O1ii—Eu1—O1W137.01 (8)C3—C2—H2B107.9
O5iii—Eu1—O1W64.87 (8)H2A—C2—H2B107.2
O6iv—Eu1—O1W139.45 (8)C5—C3—C2113.1 (3)
O3W—Eu1—O1W132.42 (8)C5—C3—C7109.5 (3)
O2W—Eu1—O1W73.89 (9)C2—C3—C7109.2 (3)
O2—Eu1—O1W69.65 (8)C5—C3—H3108.3
O3i—Eu1—O1125.13 (8)C2—C3—H3108.3
O1ii—Eu1—O170.82 (9)C7—C3—H3108.3
O5iii—Eu1—O168.59 (8)O3—C4—O4122.2 (3)
O6iv—Eu1—O172.63 (8)O3—C4—C5117.6 (3)
O3W—Eu1—O1133.22 (8)O4—C4—C5120.2 (3)
O2W—Eu1—O1141.10 (9)C4—C5—C3115.0 (3)
O2—Eu1—O150.48 (7)C4—C5—H5A108.5
O1W—Eu1—O194.23 (8)C3—C5—H5A108.5
O3i—Eu1—Eu1ii150.93 (6)C4—C5—H5B108.5
O1ii—Eu1—Eu1ii36.88 (6)C3—C5—H5B108.5
O5iii—Eu1—Eu1ii65.61 (6)H5A—C5—H5B107.5
O6iv—Eu1—Eu1ii70.39 (6)O5—C6—O6125.4 (3)
O3W—Eu1—Eu1ii106.34 (6)O5—C6—C7115.8 (3)
O2W—Eu1—Eu1ii121.42 (7)O6—C6—C7118.9 (3)
O2—Eu1—Eu1ii83.23 (5)C6—C7—C3111.4 (3)
O1W—Eu1—Eu1ii118.64 (6)C6—C7—H7A109.4
O1—Eu1—Eu1ii33.94 (5)C3—C7—H7A109.4
C1—Eu1—Eu1ii58.41 (6)C6—C7—H7B109.4
C1—O1—Eu1ii149.4 (2)C3—C7—H7B109.4
C1—O1—Eu193.87 (19)H7A—C7—H7B108.0
Eu1ii—O1—Eu1109.18 (9)H7W—O4W—H8W105.1
Eu1—O1W—H1W114.6H9W—O5W—H10W105.1
O3i—Eu1—O1—C19.2 (2)Eu1ii—Eu1—O2—C17.16 (19)
O1ii—Eu1—O1—C1159.5 (2)Eu1—O2—C1—O14.9 (3)
O5iii—Eu1—O1—C1122.7 (2)Eu1—O2—C1—C2174.5 (3)
O6iv—Eu1—O1—C179.00 (19)Eu1ii—O1—C1—O2144.3 (3)
O3W—Eu1—O1—C1114.3 (2)Eu1—O1—C1—O24.8 (3)
O2W—Eu1—O1—C1131.3 (2)Eu1ii—O1—C1—C235.1 (6)
O2—Eu1—O1—C12.69 (18)Eu1—O1—C1—C2174.6 (3)
O1W—Eu1—O1—C161.83 (19)O2—C1—C2—C327.4 (5)
Eu1ii—Eu1—O1—C1159.5 (2)O1—C1—C2—C3153.1 (3)
O3i—Eu1—O1—Eu1ii150.29 (9)C1—C2—C3—C570.5 (4)
O1ii—Eu1—O1—Eu1ii0.0C1—C2—C3—C7167.2 (3)
O5iii—Eu1—O1—Eu1ii77.77 (10)Eu1i—O3—C4—O4171.9 (11)
O6iv—Eu1—O1—Eu1ii80.50 (10)Eu1i—O3—C4—C58.9 (15)
O3W—Eu1—O1—Eu1ii45.17 (15)O3—C4—C5—C374.6 (4)
O2W—Eu1—O1—Eu1ii69.24 (16)O4—C4—C5—C3106.2 (4)
O2—Eu1—O1—Eu1ii162.19 (15)C2—C3—C5—C469.6 (4)
O1W—Eu1—O1—Eu1ii138.67 (9)C7—C3—C5—C4168.4 (3)
C1—Eu1—O1—Eu1ii159.5 (2)Eu1v—O5—C6—O67.8 (6)
O3i—Eu1—O2—C1167.2 (2)Eu1v—O5—C6—C7173.6 (3)
O1ii—Eu1—O2—C116.5 (2)Eu1iv—O6—C6—O518.0 (5)
O5iii—Eu1—O2—C157.1 (2)Eu1iv—O6—C6—C7163.4 (2)
O6iv—Eu1—O2—C178.7 (2)O5—C6—C7—C358.0 (4)
O3W—Eu1—O2—C1113.3 (2)O6—C6—C7—C3120.7 (3)
O2W—Eu1—O2—C1128.3 (2)C5—C3—C7—C6168.4 (3)
O1W—Eu1—O2—C1116.8 (2)C2—C3—C7—C667.3 (4)
O1—Eu1—O2—C12.74 (18)
Symmetry codes: (i) x, y+2, z; (ii) x, y+1, z; (iii) x1, y, z; (iv) x+1, y+1, z; (v) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O2i0.851.872.714 (4)172
O1W—H2W···O40.862.303.024 (4)141
O2W—H3W···O1Wvi0.852.172.901 (4)144
O2W—H4W···O4Wii0.851.992.824 (4)168
O3W—H5W···O5Wvii0.851.912.747 (4)166
O3W—H6W···O5Wii0.851.962.797 (4)169
O4W—H7W···O60.852.042.877 (4)169
O4W—H8W···O4viii0.852.022.869 (4)177
O5W—H9W···O40.851.882.717 (4)170
O5W—H10W···O4Wix0.851.932.765 (4)166
Symmetry codes: (i) x, y+2, z; (ii) x, y+1, z; (vi) x1, y+2, z; (vii) x, y, z1; (viii) x+1, y1, z; (ix) x, y+1, z+1.
(II) top
Crystal data top
C7H9EuO7·H2OZ = 8
Mr = 375.12F(000) = 1440
Orthorhombic, Pca21Dx = 2.441 Mg m3
Hall symbol: P 2c -2acMo Kα radiation, λ = 0.71070 Å
a = 17.4543 (19) ŵ = 6.17 mm1
b = 7.8087 (6) ÅT = 293 K
c = 14.9761 (18) ÅPrism, yellow
V = 2041.2 (4) Å30.70 × 0.26 × 0.24 mm
Data collection top
KappaCCD
diffractometer
3215 independent reflections
Radiation source: fine-focus sealed tube3040 reflections with I > 2σ(I)
Horizonally mounted graphite crystal monochromatorRint = 0.076
Detector resolution: 9 pixels mm-1θmax = 28.3°, θmin = 3.5°
CCD rotation images, thick slices scansh = 2223
Absorption correction: for a cylinder mounted on the φ axis
Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3 for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959) p.302; Table 5.3.6 B for muR in the range 2.6-10.0. The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975) A31,146-148) is used with some modification.
k = 108
Tmin = 0.370, Tmax = 0.383l = 1519
8250 measured reflections
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.063 w = 1/[σ2(Fo2) + (0.0878P)2 + 3.3954P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.167(Δ/σ)max < 0.001
S = 1.14Δρmax = 1.39 e Å3
3215 reflectionsΔρmin = 1.82 e Å3
291 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
1 restraintExtinction coefficient: 0.054 (5)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Refined as an inversion twin.
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.38 (3)
Crystal data top
C7H9EuO7·H2OV = 2041.2 (4) Å3
Mr = 375.12Z = 8
Orthorhombic, Pca21Mo Kα radiation
a = 17.4543 (19) ŵ = 6.17 mm1
b = 7.8087 (6) ÅT = 293 K
c = 14.9761 (18) Å0.70 × 0.26 × 0.24 mm
Data collection top
KappaCCD
diffractometer
3215 independent reflections
Absorption correction: for a cylinder mounted on the φ axis
Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3 for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959) p.302; Table 5.3.6 B for muR in the range 2.6-10.0. The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975) A31,146-148) is used with some modification.
3040 reflections with I > 2σ(I)
Tmin = 0.370, Tmax = 0.383Rint = 0.076
8250 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.063H-atom parameters constrained
wR(F2) = 0.167Δρmax = 1.39 e Å3
S = 1.14Δρmin = 1.82 e Å3
3215 reflectionsAbsolute structure: Refined as an inversion twin.
291 parametersAbsolute structure parameter: 0.38 (3)
1 restraint
Special details top

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

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Eu10.15041 (3)0.24606 (3)0.00438 (4)0.0166 (2)
Eu20.09236 (3)0.25409 (3)0.04429 (4)0.0166 (2)
O10.1453 (3)0.0136 (9)0.1122 (5)0.0269 (14)
O1W0.2535 (4)0.4328 (8)0.0629 (6)0.0399 (19)
H1W0.24320.53740.05280.060*
H2W0.29670.43380.08930.060*
O20.1227 (4)0.2038 (8)0.2015 (5)0.0310 (12)
O2W0.0119 (4)0.0698 (9)0.1055 (6)0.0350 (17)
H3W0.00130.03480.09590.052*
H4W0.05320.06970.13570.052*
O30.2621 (4)0.0543 (8)0.4466 (6)0.0360 (17)
O40.2857 (5)0.2199 (8)0.4674 (9)0.0393 (19)
O50.0731 (3)0.0067 (9)0.4502 (5)0.0241 (12)
O60.0020 (3)0.2085 (8)0.4227 (6)0.0325 (13)
O70.2521 (3)0.2951 (7)0.1172 (5)0.0322 (13)
O80.1719 (3)0.5069 (7)0.1002 (4)0.0203 (11)
O90.5026 (3)0.4459 (7)0.0994 (5)0.0267 (14)
O100.5231 (4)0.7253 (7)0.0736 (8)0.0314 (18)
O110.3813 (3)0.3078 (8)0.3433 (4)0.0320 (12)
O120.4024 (3)0.5117 (9)0.4363 (5)0.0235 (13)
C10.1393 (4)0.0486 (9)0.1911 (5)0.0228 (13)
C20.1496 (5)0.0668 (11)0.2714 (6)0.0351 (19)
H2A0.20360.09440.27670.042*
H2B0.12250.17300.26020.042*
C30.1230 (3)0.0031 (9)0.3587 (6)0.0215 (14)
H30.12680.09060.40200.026*
C40.1721 (4)0.1490 (9)0.3947 (6)0.0345 (17)
H4A0.14150.21420.43670.041*
H4B0.18460.22460.34540.041*
C50.2451 (4)0.0989 (8)0.4400 (5)0.0239 (14)
C60.0376 (3)0.0602 (11)0.3577 (7)0.040 (2)
H6A0.01940.06050.29660.047*
H6B0.03420.17640.38020.047*
C70.0134 (3)0.0536 (9)0.4128 (5)0.0216 (13)
C80.2326 (3)0.4457 (9)0.1349 (5)0.0206 (13)
C90.2780 (3)0.5496 (9)0.2005 (5)0.0216 (13)
H9A0.26240.51790.26040.026*
H9B0.26550.66960.19220.026*
C100.3652 (3)0.5287 (9)0.1932 (5)0.0164 (12)
H100.37700.40770.18240.020*
C110.3967 (3)0.6353 (8)0.1152 (5)0.0195 (12)
H11A0.39130.75580.12950.023*
H11B0.36610.61250.06250.023*
C120.4813 (3)0.5982 (8)0.0934 (5)0.0199 (12)
C130.4041 (3)0.5848 (9)0.2806 (5)0.0203 (13)
H13A0.45840.60080.26940.024*
H13B0.38310.69460.29850.024*
C140.3947 (3)0.4599 (10)0.3571 (6)0.0213 (13)
O3W0.1033 (5)0.4584 (12)0.1368 (10)0.087 (4)
H5W0.07280.38100.11870.131*
H6W0.07570.52710.16690.131*
O4W0.8544 (3)0.9340 (8)0.2025 (5)0.0402 (15)
H7W0.82390.88680.16570.060*
H8W0.86620.85550.23940.060*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Eu10.0108 (3)0.0131 (3)0.0260 (4)0.00012 (8)0.00183 (18)0.00039 (17)
Eu20.0100 (3)0.0124 (3)0.0273 (4)0.00033 (7)0.0017 (2)0.00025 (17)
O10.023 (3)0.034 (3)0.025 (3)0.005 (2)0.001 (2)0.004 (2)
O1W0.023 (3)0.031 (3)0.066 (5)0.002 (3)0.016 (3)0.003 (3)
O20.045 (4)0.017 (2)0.030 (3)0.002 (3)0.004 (3)0.006 (2)
O2W0.023 (3)0.027 (3)0.055 (5)0.001 (2)0.016 (3)0.000 (3)
O30.022 (3)0.027 (3)0.059 (5)0.010 (2)0.017 (3)0.004 (3)
O40.035 (4)0.030 (3)0.053 (5)0.008 (3)0.017 (3)0.011 (4)
O50.009 (2)0.026 (3)0.037 (3)0.003 (2)0.005 (2)0.000 (2)
O60.023 (3)0.018 (2)0.057 (4)0.001 (3)0.015 (3)0.001 (3)
O70.024 (2)0.018 (2)0.054 (4)0.002 (3)0.018 (2)0.002 (3)
O80.017 (2)0.018 (2)0.026 (3)0.0002 (19)0.006 (2)0.005 (2)
O90.018 (3)0.025 (3)0.037 (4)0.003 (2)0.005 (2)0.003 (3)
O100.015 (3)0.015 (2)0.064 (5)0.003 (2)0.014 (3)0.003 (3)
O110.047 (3)0.018 (3)0.031 (3)0.001 (2)0.000 (2)0.002 (2)
O120.024 (3)0.023 (3)0.023 (3)0.005 (2)0.0017 (19)0.003 (2)
C10.021 (3)0.019 (3)0.028 (3)0.008 (3)0.001 (2)0.000 (3)
C20.046 (5)0.024 (4)0.035 (4)0.007 (3)0.007 (3)0.003 (3)
C30.007 (3)0.013 (3)0.045 (4)0.003 (2)0.000 (3)0.002 (3)
C40.036 (4)0.020 (3)0.048 (4)0.006 (3)0.017 (3)0.007 (3)
C50.017 (3)0.022 (3)0.033 (4)0.002 (2)0.004 (3)0.003 (3)
C60.010 (3)0.047 (5)0.061 (5)0.001 (3)0.013 (3)0.028 (4)
C70.009 (3)0.028 (3)0.028 (3)0.006 (2)0.002 (2)0.006 (3)
C80.012 (3)0.025 (3)0.025 (3)0.003 (2)0.001 (2)0.003 (3)
C90.009 (2)0.022 (3)0.034 (4)0.000 (2)0.001 (2)0.002 (3)
C100.009 (2)0.025 (3)0.015 (3)0.003 (2)0.003 (2)0.004 (2)
C110.012 (2)0.022 (3)0.024 (3)0.002 (2)0.001 (2)0.006 (2)
C120.018 (3)0.023 (3)0.019 (3)0.000 (2)0.003 (2)0.001 (2)
C130.017 (3)0.023 (3)0.021 (3)0.006 (2)0.005 (2)0.002 (3)
C140.010 (2)0.031 (4)0.023 (3)0.004 (2)0.002 (2)0.000 (3)
O3W0.047 (5)0.064 (7)0.151 (10)0.021 (4)0.033 (6)0.020 (6)
O4W0.025 (3)0.044 (4)0.052 (4)0.011 (2)0.001 (2)0.013 (3)
Geometric parameters (Å, º) top
Eu1—O3i2.307 (6)O9—C121.249 (8)
Eu1—O12.431 (7)O9—Eu2x2.319 (6)
Eu1—O5ii2.445 (6)O10—C121.267 (9)
Eu1—O10iii2.462 (8)O10—Eu1xi2.462 (8)
Eu1—O72.480 (6)O11—C141.228 (9)
Eu1—O12i2.488 (6)O11—Eu1viii2.521 (7)
Eu1—O82.520 (6)O12—C141.261 (10)
Eu1—O11i2.521 (7)O12—Eu2xii2.443 (7)
Eu1—O1W2.526 (7)O12—Eu1viii2.488 (6)
Eu1—C14i2.876 (8)C1—C21.514 (10)
Eu1—C82.883 (7)C2—C31.491 (13)
Eu1—Eu2iv4.0767 (5)C2—H2A0.9700
Eu2—O9v2.319 (6)C2—H2B0.9700
Eu2—O4i2.435 (9)C3—C41.525 (10)
Eu2—O12vi2.443 (7)C3—C61.555 (9)
Eu2—O22.445 (7)C3—H30.9800
Eu2—O8vii2.472 (6)C4—C51.496 (9)
Eu2—O6ii2.480 (7)C4—H4A0.9700
Eu2—O2W2.495 (7)C4—H4B0.9700
Eu2—O5ii2.499 (7)C6—C71.505 (9)
Eu2—O12.502 (7)C6—H6A0.9700
Eu2—C12.842 (8)C6—H6B0.9700
Eu2—C7ii2.868 (7)C7—Eu2ix2.868 (7)
Eu2—Eu1vii4.0767 (5)C8—C91.501 (9)
O1—C11.281 (9)C9—C101.535 (8)
O1W—H1W0.8500C9—H9A0.9700
O1W—H2W0.8501C9—H9B0.9700
O2—C11.255 (9)C10—C111.536 (9)
O2W—H3W0.8500C10—C131.538 (9)
O2W—H4W0.8499C10—H100.9800
O3—C51.236 (8)C11—C121.539 (8)
O3—Eu1viii2.307 (6)C11—H11A0.9700
O4—C51.250 (9)C11—H11B0.9700
O4—Eu2viii2.435 (9)C13—C141.513 (10)
O5—C71.272 (8)C13—H13A0.9700
O5—Eu1ix2.445 (6)C13—H13B0.9700
O5—Eu2ix2.499 (7)C14—Eu1viii2.876 (8)
O6—C71.248 (9)O3W—H5W0.8499
O6—Eu2ix2.480 (7)O3W—H6W0.8499
O7—C81.252 (9)O4W—H7W0.8499
O8—C81.274 (8)O4W—H8W0.8500
O8—Eu2iv2.472 (6)
O3i—Eu1—O177.8 (2)O1—Eu2—C7ii90.0 (2)
O3i—Eu1—O5ii75.2 (2)C1—Eu2—C7ii111.17 (19)
O1—Eu1—O5ii68.3 (2)O9v—Eu2—Eu1vii66.54 (14)
O3i—Eu1—O10iii144.5 (2)O4i—Eu2—Eu1vii79.53 (16)
O1—Eu1—O10iii75.8 (2)O12vi—Eu2—Eu1vii34.59 (15)
O5ii—Eu1—O10iii73.2 (2)O2—Eu2—Eu1vii103.95 (15)
O3i—Eu1—O783.2 (3)O8vii—Eu2—Eu1vii35.64 (13)
O1—Eu1—O771.9 (2)O6ii—Eu2—Eu1vii101.24 (15)
O5ii—Eu1—O7137.7 (2)O2W—Eu2—Eu1vii141.95 (15)
O10iii—Eu1—O7110.2 (3)O5ii—Eu2—Eu1vii136.96 (16)
O3i—Eu1—O12i129.3 (3)O1—Eu2—Eu1vii140.16 (14)
O1—Eu1—O12i151.7 (2)C1—Eu2—Eu1vii125.62 (14)
O5ii—Eu1—O12i107.3 (2)C7ii—Eu2—Eu1vii122.78 (14)
O10iii—Eu1—O12i76.3 (2)C1—O1—Eu1154.0 (5)
O7—Eu1—O12i114.5 (2)C1—O1—Eu291.6 (5)
O3i—Eu1—O8129.8 (2)Eu1—O1—Eu2111.5 (3)
O1—Eu1—O8103.3 (3)Eu1—O1W—H1W109.4
O5ii—Eu1—O8152.8 (2)Eu1—O1W—H2W145.2
O10iii—Eu1—O879.7 (2)H1W—O1W—H2W105.1
O7—Eu1—O851.74 (19)C1—O2—Eu294.9 (5)
O12i—Eu1—O867.3 (2)Eu2—O2W—H3W109.4
O3i—Eu1—O11i84.9 (3)Eu2—O2W—H4W144.5
O1—Eu1—O11i140.4 (2)H3W—O2W—H4W105.9
O5ii—Eu1—O11i73.0 (2)C5—O3—Eu1viii144.8 (6)
O10iii—Eu1—O11i100.8 (3)C5—O4—Eu2viii137.1 (6)
O7—Eu1—O11i141.2 (2)C7—O5—Eu1ix151.7 (5)
O12i—Eu1—O11i50.8 (2)C7—O5—Eu2ix93.3 (5)
O8—Eu1—O11i115.03 (19)Eu1ix—O5—Eu2ix111.2 (2)
O3i—Eu1—O1W75.7 (3)C7—O6—Eu2ix94.8 (4)
O1—Eu1—O1W136.2 (2)C8—O7—Eu195.5 (4)
O5ii—Eu1—O1W134.6 (3)C8—O8—Eu2iv152.7 (5)
O10iii—Eu1—O1W139.3 (2)C8—O8—Eu193.0 (4)
O7—Eu1—O1W70.9 (3)Eu2iv—O8—Eu1109.5 (2)
O12i—Eu1—O1W67.6 (2)C12—O9—Eu2x142.2 (5)
O8—Eu1—O1W69.8 (2)C12—O10—Eu1xi133.6 (5)
O11i—Eu1—O1W70.4 (3)C14—O11—Eu1viii93.8 (5)
O3i—Eu1—C14i105.7 (3)C14—O12—Eu2xii150.1 (5)
O1—Eu1—C14i158.86 (19)C14—O12—Eu1viii94.5 (5)
O5ii—Eu1—C14i92.2 (2)Eu2xii—O12—Eu1viii111.5 (3)
O10iii—Eu1—C14i91.3 (3)O2—C1—O1120.0 (7)
O7—Eu1—C14i129.0 (2)O2—C1—C2120.2 (7)
O12i—Eu1—C14i25.9 (2)O1—C1—C2119.8 (7)
O8—Eu1—C14i90.5 (2)O2—C1—Eu259.0 (4)
O11i—Eu1—C14i25.2 (2)O1—C1—Eu261.6 (4)
O1W—Eu1—C14i63.5 (2)C2—C1—Eu2170.1 (5)
O3i—Eu1—C8106.0 (2)C3—C2—C1116.2 (7)
O1—Eu1—C888.4 (2)C3—C2—H2A108.2
O5ii—Eu1—C8156.0 (2)C1—C2—H2A108.2
O10iii—Eu1—C896.6 (3)C3—C2—H2B108.2
O7—Eu1—C825.62 (18)C1—C2—H2B108.2
O12i—Eu1—C890.7 (2)H2A—C2—H2B107.4
O8—Eu1—C826.18 (17)C2—C3—C4114.1 (6)
O11i—Eu1—C8130.89 (19)C2—C3—C6113.3 (7)
O1W—Eu1—C866.7 (2)C4—C3—C6109.1 (6)
C14i—Eu1—C8110.0 (2)C2—C3—H3106.6
O3i—Eu1—Eu2iv147.25 (16)C4—C3—H3106.6
O1—Eu1—Eu2iv127.46 (17)C6—C3—H3106.6
O5ii—Eu1—Eu2iv130.06 (13)C5—C4—C3116.4 (6)
O10iii—Eu1—Eu2iv68.10 (13)C5—C4—H4A108.2
O7—Eu1—Eu2iv85.99 (13)C3—C4—H4A108.2
O12i—Eu1—Eu2iv33.88 (16)C5—C4—H4B108.2
O8—Eu1—Eu2iv34.86 (13)C3—C4—H4B108.2
O11i—Eu1—Eu2iv84.42 (13)H4A—C4—H4B107.4
O1W—Eu1—Eu2iv71.51 (15)O3—C5—O4124.7 (8)
C14i—Eu1—Eu2iv59.24 (16)O3—C5—C4119.6 (7)
C8—Eu1—Eu2iv60.43 (13)O4—C5—C4115.7 (7)
O9v—Eu2—O4i146.1 (2)C7—C6—C3113.1 (6)
O9v—Eu2—O12vi77.1 (2)C7—C6—H6A109.0
O4i—Eu2—O12vi74.7 (3)C3—C6—H6A109.0
O9v—Eu2—O284.7 (2)C7—C6—H6B109.0
O4i—Eu2—O2104.4 (3)C3—C6—H6B109.0
O12vi—Eu2—O2138.5 (2)H6A—C6—H6B107.8
O9v—Eu2—O8vii76.8 (2)O6—C7—O5118.8 (7)
O4i—Eu2—O8vii75.7 (2)O6—C7—C6120.7 (6)
O12vi—Eu2—O8vii68.78 (19)O5—C7—C6120.5 (7)
O2—Eu2—O8vii70.9 (2)O6—C7—Eu2ix59.5 (4)
O9v—Eu2—O6ii84.6 (2)O5—C7—Eu2ix60.5 (4)
O4i—Eu2—O6ii102.6 (4)C6—C7—Eu2ix169.5 (5)
O12vi—Eu2—O6ii69.3 (2)O7—C8—O8119.5 (6)
O2—Eu2—O6ii145.9 (2)O7—C8—C9120.2 (6)
O8vii—Eu2—O6ii136.9 (2)O8—C8—C9120.2 (6)
O9v—Eu2—O2W75.4 (2)O7—C8—Eu158.9 (4)
O4i—Eu2—O2W138.5 (2)O8—C8—Eu160.8 (4)
O12vi—Eu2—O2W134.6 (2)C9—C8—Eu1177.8 (4)
O2—Eu2—O2W73.2 (3)C8—C9—C10114.8 (5)
O8vii—Eu2—O2W136.1 (2)C8—C9—H9A108.6
O6ii—Eu2—O2W72.7 (3)C10—C9—H9A108.6
O9v—Eu2—O5ii129.5 (2)C8—C9—H9B108.6
O4i—Eu2—O5ii76.2 (2)C10—C9—H9B108.6
O12vi—Eu2—O5ii104.0 (3)H9A—C9—H9B107.5
O2—Eu2—O5ii116.2 (2)C9—C10—C11110.6 (5)
O8vii—Eu2—O5ii151.9 (2)C9—C10—C13110.3 (5)
O6ii—Eu2—O5ii51.65 (19)C11—C10—C13109.6 (5)
O2W—Eu2—O5ii68.8 (2)C9—C10—H10108.8
O9v—Eu2—O1130.1 (2)C11—C10—H10108.8
O4i—Eu2—O177.2 (3)C13—C10—H10108.8
O12vi—Eu2—O1151.8 (2)C10—C11—C12113.7 (5)
O2—Eu2—O152.7 (2)C10—C11—H11A108.8
O8vii—Eu2—O1106.6 (2)C12—C11—H11A108.8
O6ii—Eu2—O1115.1 (2)C10—C11—H11B108.8
O2W—Eu2—O168.8 (2)C12—C11—H11B108.8
O5ii—Eu2—O166.3 (2)H11A—C11—H11B107.7
O9v—Eu2—C1106.5 (3)O9—C12—O10126.2 (7)
O4i—Eu2—C193.0 (3)O9—C12—C11116.7 (6)
O12vi—Eu2—C1157.49 (19)O10—C12—C11117.0 (6)
O2—Eu2—C126.1 (2)C14—C13—C10114.4 (5)
O8vii—Eu2—C190.1 (2)C14—C13—H13A108.7
O6ii—Eu2—C1132.7 (2)C10—C13—H13A108.7
O2W—Eu2—C166.4 (2)C14—C13—H13B108.7
O5ii—Eu2—C190.9 (2)C10—C13—H13B108.7
O1—Eu2—C126.8 (2)H13A—C13—H13B107.6
O9v—Eu2—C7ii105.8 (2)O11—C14—O12119.2 (7)
O4i—Eu2—C7ii92.0 (3)O11—C14—C13121.1 (7)
O12vi—Eu2—C7ii88.4 (2)O12—C14—C13119.6 (7)
O2—Eu2—C7ii132.6 (2)O11—C14—Eu1viii61.0 (4)
O8vii—Eu2—C7ii156.1 (2)O12—C14—Eu1viii59.6 (4)
O6ii—Eu2—C7ii25.7 (2)C13—C14—Eu1viii169.8 (4)
O2W—Eu2—C7ii65.6 (2)H5W—O3W—H6W105.2
O5ii—Eu2—C7ii26.29 (18)H7W—O4W—H8W105.1
O3i—Eu1—O1—C1143.1 (12)O6ii—Eu2—C1—O156.8 (5)
O5ii—Eu1—O1—C1138.1 (12)O2W—Eu2—C1—O189.3 (4)
O10iii—Eu1—O1—C160.9 (11)O5ii—Eu2—C1—O122.9 (4)
O7—Eu1—O1—C156.3 (11)C7ii—Eu2—C1—O140.0 (5)
O12i—Eu1—O1—C152.0 (13)Eu1vii—Eu2—C1—O1132.6 (4)
O8—Eu1—O1—C114.7 (11)O9v—Eu2—C1—C254 (3)
O11i—Eu1—O1—C1150.7 (11)O4i—Eu2—C1—C2154 (3)
O1W—Eu1—O1—C189.3 (12)O12vi—Eu2—C1—C2150 (3)
C14i—Eu1—O1—C1114.8 (12)O2—Eu2—C1—C288 (3)
C8—Eu1—O1—C136.3 (11)O8vii—Eu2—C1—C2130 (3)
Eu2iv—Eu1—O1—C113.6 (12)O6ii—Eu2—C1—C244 (3)
O3i—Eu1—O1—Eu265.8 (3)O2W—Eu2—C1—C212 (3)
O5ii—Eu1—O1—Eu213.0 (2)O5ii—Eu2—C1—C278 (3)
O10iii—Eu1—O1—Eu290.3 (3)O1—Eu2—C1—C2101 (3)
O7—Eu1—O1—Eu2152.6 (3)C7ii—Eu2—C1—C261 (3)
O12i—Eu1—O1—Eu299.1 (5)Eu1vii—Eu2—C1—C2126 (3)
O8—Eu1—O1—Eu2165.8 (2)O2—C1—C2—C312.7 (11)
O11i—Eu1—O1—Eu20.4 (4)O1—C1—C2—C3165.3 (7)
O1W—Eu1—O1—Eu2119.6 (3)Eu2—C1—C2—C370 (3)
C14i—Eu1—O1—Eu236.3 (7)C1—C2—C3—C470.2 (9)
C8—Eu1—O1—Eu2172.5 (2)C1—C2—C3—C655.5 (9)
Eu2iv—Eu1—O1—Eu2137.53 (16)C2—C3—C4—C579.8 (9)
O9v—Eu2—O1—C132.3 (5)C6—C3—C4—C5152.4 (7)
O4i—Eu2—O1—C1124.7 (5)Eu1viii—O3—C5—O45.3 (19)
O12vi—Eu2—O1—C1130.1 (5)Eu1viii—O3—C5—C4176.0 (9)
O2—Eu2—O1—C15.1 (4)Eu2viii—O4—C5—O31.0 (19)
O8vii—Eu2—O1—C154.2 (4)Eu2viii—O4—C5—C4179.8 (9)
O6ii—Eu2—O1—C1137.2 (4)C3—C4—C5—O30.3 (12)
O2W—Eu2—O1—C179.5 (4)C3—C4—C5—O4178.5 (9)
O5ii—Eu2—O1—C1154.9 (5)C2—C3—C6—C7110.4 (8)
C7ii—Eu2—O1—C1143.2 (4)C4—C3—C6—C7121.3 (8)
Eu1vii—Eu2—O1—C169.0 (5)Eu2ix—O6—C7—O512.2 (7)
O9v—Eu2—O1—Eu1135.4 (3)Eu2ix—O6—C7—C6167.8 (6)
O4i—Eu2—O1—Eu167.5 (3)Eu1ix—O5—C7—O6162.6 (8)
O12vi—Eu2—O1—Eu162.2 (5)Eu2ix—O5—C7—O612.0 (7)
O2—Eu2—O1—Eu1172.9 (3)Eu1ix—O5—C7—C617.4 (15)
O8vii—Eu2—O1—Eu1138.1 (2)Eu2ix—O5—C7—C6167.9 (6)
O6ii—Eu2—O1—Eu130.5 (3)Eu1ix—O5—C7—Eu2ix150.5 (11)
O2W—Eu2—O1—Eu188.2 (3)C3—C6—C7—O629.9 (11)
O5ii—Eu2—O1—Eu112.9 (2)C3—C6—C7—O5150.0 (7)
C1—Eu2—O1—Eu1167.7 (6)C3—C6—C7—Eu2ix58 (3)
C7ii—Eu2—O1—Eu124.6 (3)Eu1—O7—C8—O85.8 (7)
Eu1vii—Eu2—O1—Eu1123.20 (19)Eu1—O7—C8—C9177.6 (5)
O9v—Eu2—O2—C1146.9 (5)Eu2iv—O8—C8—O7151.9 (8)
O4i—Eu2—O2—C166.4 (5)Eu1—O8—C8—O75.7 (7)
O12vi—Eu2—O2—C1149.4 (4)Eu2iv—O8—C8—C931.5 (14)
O8vii—Eu2—O2—C1135.3 (5)Eu1—O8—C8—C9177.7 (5)
O6ii—Eu2—O2—C174.7 (6)Eu2iv—O8—C8—Eu1146.2 (11)
O2W—Eu2—O2—C170.5 (5)O3i—Eu1—C8—O728.1 (5)
O5ii—Eu2—O2—C115.1 (5)O1—Eu1—C8—O748.7 (5)
O1—Eu2—O2—C15.3 (4)O5ii—Eu1—C8—O761.4 (7)
C7ii—Eu2—O2—C140.2 (6)O10iii—Eu1—C8—O7124.2 (5)
Eu1vii—Eu2—O2—C1148.9 (4)O12i—Eu1—C8—O7159.5 (5)
O3i—Eu1—O7—C8152.9 (5)O8—Eu1—C8—O7174.2 (7)
O1—Eu1—O7—C8127.8 (5)O11i—Eu1—C8—O7125.3 (5)
O5ii—Eu1—O7—C8148.0 (4)O1W—Eu1—C8—O794.3 (5)
O10iii—Eu1—O7—C861.0 (5)C14i—Eu1—C8—O7141.9 (5)
O12i—Eu1—O7—C822.6 (5)Eu2iv—Eu1—C8—O7175.6 (5)
O8—Eu1—O7—C83.3 (4)O3i—Eu1—C8—O8157.7 (4)
O11i—Eu1—O7—C879.8 (6)O1—Eu1—C8—O8125.5 (4)
O1W—Eu1—O7—C875.7 (5)O5ii—Eu1—C8—O8112.8 (6)
C14i—Eu1—O7—C848.1 (6)O10iii—Eu1—C8—O850.0 (4)
Eu2iv—Eu1—O7—C83.9 (4)O7—Eu1—C8—O8174.2 (7)
O3i—Eu1—O8—C828.3 (6)O12i—Eu1—C8—O826.3 (4)
O1—Eu1—O8—C856.8 (4)O11i—Eu1—C8—O860.5 (5)
O5ii—Eu1—O8—C8124.9 (5)O1W—Eu1—C8—O891.5 (4)
O10iii—Eu1—O8—C8129.4 (5)C14i—Eu1—C8—O843.9 (4)
O7—Eu1—O8—C83.2 (4)Eu2iv—Eu1—C8—O810.2 (4)
O12i—Eu1—O8—C8151.3 (5)O3i—Eu1—C8—C939 (12)
O11i—Eu1—O8—C8133.4 (4)O1—Eu1—C8—C9116 (12)
O1W—Eu1—O8—C877.9 (4)O5ii—Eu1—C8—C9129 (12)
C14i—Eu1—O8—C8139.4 (4)O10iii—Eu1—C8—C9169 (12)
Eu2iv—Eu1—O8—C8164.3 (5)O7—Eu1—C8—C967 (12)
O3i—Eu1—O8—Eu2iv136.0 (3)O12i—Eu1—C8—C992 (12)
O1—Eu1—O8—Eu2iv138.9 (2)O8—Eu1—C8—C9119 (12)
O5ii—Eu1—O8—Eu2iv70.8 (6)O11i—Eu1—C8—C958 (12)
O10iii—Eu1—O8—Eu2iv66.3 (3)O1W—Eu1—C8—C927 (12)
O7—Eu1—O8—Eu2iv167.5 (3)C14i—Eu1—C8—C975 (12)
O12i—Eu1—O8—Eu2iv13.0 (2)Eu2iv—Eu1—C8—C9108 (12)
O11i—Eu1—O8—Eu2iv30.9 (3)O7—C8—C9—C1040.6 (9)
O1W—Eu1—O8—Eu2iv86.4 (3)O8—C8—C9—C10142.9 (6)
C14i—Eu1—O8—Eu2iv24.9 (2)Eu1—C8—C9—C1025 (12)
C8—Eu1—O8—Eu2iv164.3 (5)C8—C9—C10—C1178.9 (7)
Eu2—O2—C1—O19.5 (7)C8—C9—C10—C13159.7 (6)
Eu2—O2—C1—C2168.5 (6)C9—C10—C11—C12170.3 (5)
Eu1—O1—C1—O2162.5 (8)C13—C10—C11—C1267.9 (7)
Eu2—O1—C1—O29.2 (7)Eu2x—O9—C12—O1028.6 (15)
Eu1—O1—C1—C215.5 (16)Eu2x—O9—C12—C11153.5 (6)
Eu2—O1—C1—C2168.8 (6)Eu1xi—O10—C12—O916.7 (17)
Eu1—O1—C1—Eu2153.3 (12)Eu1xi—O10—C12—C11165.3 (7)
O9v—Eu2—C1—O234.6 (5)C10—C11—C12—O938.1 (9)
O4i—Eu2—C1—O2117.3 (5)C10—C11—C12—O10140.1 (9)
O12vi—Eu2—C1—O261.6 (8)C9—C10—C13—C1474.0 (7)
O8vii—Eu2—C1—O241.6 (5)C11—C10—C13—C14164.1 (5)
O6ii—Eu2—C1—O2132.6 (5)Eu1viii—O11—C14—O1213.0 (6)
O2W—Eu2—C1—O2100.1 (5)Eu1viii—O11—C14—C13168.4 (5)
O5ii—Eu2—C1—O2166.5 (4)Eu2xii—O12—C14—O11164.4 (6)
O1—Eu2—C1—O2170.7 (7)Eu1viii—O12—C14—O1113.2 (6)
C7ii—Eu2—C1—O2149.4 (4)Eu2xii—O12—C14—C1317.1 (12)
Eu1vii—Eu2—C1—O238.0 (5)Eu1viii—O12—C14—C13168.2 (5)
O9v—Eu2—C1—O1154.7 (4)Eu2xii—O12—C14—Eu1viii151.2 (9)
O4i—Eu2—C1—O153.4 (5)C10—C13—C14—O1123.3 (9)
O12vi—Eu2—C1—O1109.0 (7)C10—C13—C14—O12158.2 (6)
O2—Eu2—C1—O1170.7 (7)C10—C13—C14—Eu1viii76 (3)
O8vii—Eu2—C1—O1129.0 (4)
Symmetry codes: (i) x+1/2, y, z1/2; (ii) x, y, z1/2; (iii) x1/2, y+1, z; (iv) x, y+1, z; (v) x1/2, y, z; (vi) x+1/2, y1, z1/2; (vii) x, y1, z; (viii) x+1/2, y, z+1/2; (ix) x, y, z+1/2; (x) x+1/2, y, z; (xi) x+1/2, y+1, z; (xii) x+1/2, y+1, z+1/2.
(III) top
Crystal data top
C7H9EuO7·H2OZ = 8
Mr = 375.12F(000) = 1440
Orthorhombic, PbcnDx = 2.520 Mg m3
Hall symbol: -P 2n 2abMo Kα radiation, λ = 0.71073 Å
a = 14.1085 (3) ŵ = 6.37 mm1
b = 7.7825 (2) ÅT = 293 K
c = 18.0083 (4) ÅPrism, yellow
V = 1977.30 (8) Å30.32 × 0.30 × 0.24 mm
Data collection top
Nonius KappaCCD
diffractometer
3133 independent reflections
Radiation source: fine-focus sealed tube2860 reflections with I > 2σ(I)
Horizonally mounted graphite crystal monochromatorRint = 0.041
Detector resolution: 9 pixels mm-1θmax = 31.1°, θmin = 3.7°
thick–slice ω– and φ–scansh = 1920
Absorption correction: for a sphere
Dwiggins (1975)
k = 119
Tmin = 0.235, Tmax = 0.310l = 2522
15892 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.029Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.074H-atom parameters constrained
S = 1.13 w = 1/[σ2(Fo2) + (0.0279P)2 + 4.6261P]
where P = (Fo2 + 2Fc2)/3
3133 reflections(Δ/σ)max < 0.001
145 parametersΔρmax = 0.96 e Å3
0 restraintsΔρmin = 1.16 e Å3
Crystal data top
C7H9EuO7·H2OV = 1977.30 (8) Å3
Mr = 375.12Z = 8
Orthorhombic, PbcnMo Kα radiation
a = 14.1085 (3) ŵ = 6.37 mm1
b = 7.7825 (2) ÅT = 293 K
c = 18.0083 (4) Å0.32 × 0.30 × 0.24 mm
Data collection top
Nonius KappaCCD
diffractometer
3133 independent reflections
Absorption correction: for a sphere
Dwiggins (1975)
2860 reflections with I > 2σ(I)
Tmin = 0.235, Tmax = 0.310Rint = 0.041
15892 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0290 restraints
wR(F2) = 0.074H-atom parameters constrained
S = 1.13Δρmax = 0.96 e Å3
3133 reflectionsΔρmin = 1.16 e Å3
145 parameters
Special details top

Experimental. Interpolation using International Tables Vol. C (1992) p. 523, Table 6.3.3.3 for values of muR in the range 0–2.5, and International Tables Vol. II (1959) p. 302, Table 5.3.6B for muR in the range 2.6–10.0. The interpolation procedure of C. W. Dwiggins Jr [Acta Cryst. (1975) A31, 146–148] is used with some modification.

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

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Eu10.705403 (11)0.491484 (17)0.346199 (8)0.02112 (6)
O10.75706 (16)0.7403 (3)0.26618 (13)0.0291 (5)
O1W0.56042 (18)0.3178 (3)0.32334 (15)0.0386 (6)
H1W0.57920.21470.32850.058*
H2W0.51220.32680.35140.058*
O20.6496 (2)0.5665 (3)0.22157 (14)0.0365 (5)
O30.3755 (2)0.9645 (4)0.15833 (16)0.0374 (6)
O40.41657 (17)0.6967 (3)0.13148 (15)0.0337 (5)
O50.72517 (18)0.7822 (3)0.08010 (13)0.0291 (4)
O60.6495 (2)0.5735 (3)0.02627 (14)0.0390 (6)
C10.7023 (2)0.6938 (4)0.21331 (17)0.0261 (6)
C20.7052 (2)0.7861 (5)0.13973 (17)0.0274 (6)
H2A0.72680.90300.14770.033*
H2B0.75070.72950.10760.033*
C30.6088 (2)0.7904 (4)0.10094 (14)0.0220 (5)
H30.58320.67350.09910.026*
C40.5394 (2)0.9053 (4)0.14418 (16)0.0251 (5)
H4A0.54321.02060.12400.030*
H4B0.56030.91070.19540.030*
C50.4362 (2)0.8496 (4)0.14335 (16)0.0240 (5)
C60.6210 (2)0.8568 (4)0.02113 (16)0.0278 (6)
H6A0.65800.96180.02230.033*
H6B0.55910.88460.00100.033*
C70.6688 (2)0.7302 (4)0.02954 (15)0.0242 (5)
O2W0.4212 (4)0.3136 (8)0.4347 (4)0.130 (2)
H3W0.39980.39250.46270.196*
H4W0.40420.37350.39750.196*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Eu10.02385 (9)0.01739 (9)0.02210 (9)0.00021 (4)0.00005 (5)0.00193 (4)
O10.0318 (12)0.0309 (12)0.0246 (10)0.0005 (10)0.0029 (8)0.0014 (8)
O1W0.0356 (13)0.0336 (13)0.0466 (14)0.0070 (10)0.0023 (11)0.0011 (11)
O20.0497 (15)0.0286 (12)0.0311 (11)0.0092 (11)0.0112 (11)0.0072 (9)
O30.0274 (12)0.0290 (11)0.0558 (17)0.0031 (10)0.0043 (11)0.0007 (11)
O40.0269 (11)0.0254 (11)0.0488 (14)0.0038 (9)0.0037 (10)0.0026 (10)
O50.0350 (11)0.0276 (11)0.0248 (10)0.0035 (9)0.0057 (9)0.0020 (9)
O60.0625 (17)0.0226 (11)0.0318 (12)0.0045 (11)0.0178 (11)0.0027 (9)
C10.0300 (14)0.0243 (14)0.0240 (13)0.0044 (11)0.0008 (11)0.0001 (10)
C20.0268 (14)0.0320 (16)0.0233 (13)0.0009 (11)0.0006 (10)0.0033 (11)
C30.0246 (13)0.0226 (12)0.0187 (11)0.0014 (11)0.0010 (9)0.0007 (9)
C40.0237 (13)0.0263 (13)0.0253 (13)0.0007 (11)0.0028 (10)0.0040 (10)
C50.0248 (13)0.0252 (13)0.0220 (12)0.0005 (11)0.0006 (10)0.0020 (10)
C60.0373 (16)0.0242 (13)0.0217 (12)0.0056 (12)0.0018 (11)0.0013 (10)
C70.0296 (14)0.0228 (13)0.0202 (12)0.0001 (11)0.0003 (10)0.0002 (10)
O2W0.081 (3)0.111 (4)0.199 (6)0.002 (3)0.030 (4)0.089 (4)
Geometric parameters (Å, º) top
Eu1—O4i2.382 (2)O5—C71.275 (4)
Eu1—O3ii2.411 (3)O5—Eu1viii2.413 (2)
Eu1—O5iii2.413 (2)O5—Eu1ix2.525 (2)
Eu1—O22.449 (2)O6—C71.251 (4)
Eu1—O6iv2.480 (2)O6—Eu1ix2.480 (2)
Eu1—O1v2.485 (2)C1—C21.508 (4)
Eu1—O1W2.486 (3)C2—C31.529 (4)
Eu1—O12.521 (2)C2—H2A0.9700
Eu1—O5iv2.525 (2)C2—H2B0.9700
Eu1—Eu1vi4.0897 (1)C3—C61.537 (4)
Eu1—H1W2.8133C3—C41.537 (4)
O1—C11.279 (4)C3—H30.9800
O1—Eu1vi2.485 (2)C4—C51.520 (4)
O1W—H1W0.8500C4—H4A0.9700
O1W—H2W0.8500C4—H4B0.9700
O2—C11.248 (4)C6—C71.502 (4)
O3—C51.267 (4)C6—H6A0.9700
O3—Eu1vii2.411 (3)C6—H6B0.9700
O4—C51.240 (4)O2W—H3W0.85
O4—Eu1i2.382 (2)O2W—H4W0.85
O4i—Eu1—O3ii141.58 (9)C1—O2—Eu196.13 (19)
O4i—Eu1—O5iii73.21 (9)C5—O3—Eu1vii136.6 (2)
O3ii—Eu1—O5iii71.22 (9)C5—O4—Eu1i140.8 (2)
O4i—Eu1—O276.26 (10)C7—O5—Eu1viii151.4 (2)
O3ii—Eu1—O2108.06 (10)C7—O5—Eu1ix92.21 (18)
O5iii—Eu1—O2117.43 (8)Eu1viii—O5—Eu1ix111.80 (9)
O4i—Eu1—O6iv75.57 (9)C7—O6—Eu1ix94.95 (18)
O3ii—Eu1—O6iv109.27 (10)O2—C1—O1119.8 (3)
O5iii—Eu1—O6iv76.62 (9)O2—C1—C2119.9 (3)
O2—Eu1—O6iv142.65 (10)O1—C1—C2120.2 (3)
O4i—Eu1—O1v141.18 (8)C1—C2—C3112.8 (3)
O3ii—Eu1—O1v72.52 (9)C1—C2—H2A109.0
O5iii—Eu1—O1v143.74 (8)C3—C2—H2A109.0
O2—Eu1—O1v74.02 (8)C1—C2—H2B109.0
O6iv—Eu1—O1v116.37 (8)C3—C2—H2B109.0
O4i—Eu1—O1W78.36 (9)H2A—C2—H2B107.8
O3ii—Eu1—O1W140.01 (9)C2—C3—C6109.6 (2)
O5iii—Eu1—O1W145.28 (9)C2—C3—C4110.4 (2)
O2—Eu1—O1W73.34 (9)C6—C3—C4110.5 (2)
O6iv—Eu1—O1W77.34 (10)C2—C3—H3108.8
O1v—Eu1—O1W69.61 (8)C6—C3—H3108.8
O4i—Eu1—O177.89 (8)C4—C3—H3108.8
O3ii—Eu1—O176.11 (8)C5—C4—C3116.1 (3)
O5iii—Eu1—O168.68 (8)C5—C4—H4A108.3
O2—Eu1—O152.14 (8)C3—C4—H4A108.3
O6iv—Eu1—O1141.05 (8)C5—C4—H4B108.3
O1v—Eu1—O1102.19 (8)C3—C4—H4B108.3
O1W—Eu1—O1124.11 (8)H4A—C4—H4B107.4
O4i—Eu1—O5iv123.83 (8)O4—C5—O3124.3 (3)
O3ii—Eu1—O5iv80.46 (9)O4—C5—C4119.3 (3)
O5iii—Eu1—O5iv106.36 (8)O3—C5—C4116.4 (3)
O2—Eu1—O5iv135.90 (8)C7—C6—C3113.4 (2)
O6iv—Eu1—O5iv51.42 (8)C7—C6—H6A108.9
O1v—Eu1—O5iv67.53 (8)C3—C6—H6A108.9
O1W—Eu1—O5iv73.69 (9)C7—C6—H6B108.9
O1—Eu1—O5iv156.39 (7)C3—C6—H6B108.9
C1—O1—Eu1vi141.6 (2)H6A—C6—H6B107.7
C1—O1—Eu191.91 (18)O6—C7—O5118.6 (3)
Eu1vi—O1—Eu1109.53 (9)O6—C7—C6120.9 (3)
Eu1—O1W—H1W103.8O5—C7—C6120.4 (3)
Eu1—O1W—H2W121.0H3W—O2W—H4W88.4
H1W—O1W—H2W105.2
O4i—Eu1—O1—C183.30 (18)Eu1—O2—C1—O12.6 (3)
O3ii—Eu1—O1—C1125.24 (19)Eu1—O2—C1—C2174.0 (2)
O5iii—Eu1—O1—C1159.80 (19)Eu1vi—O1—C1—O2123.0 (3)
O2—Eu1—O1—C11.40 (17)Eu1—O1—C1—O22.5 (3)
O6iv—Eu1—O1—C1131.2 (2)Eu1vi—O1—C1—C260.4 (4)
O1v—Eu1—O1—C156.95 (15)Eu1—O1—C1—C2174.1 (3)
O1W—Eu1—O1—C116.5 (2)O2—C1—C2—C335.3 (4)
O5iv—Eu1—O1—C1118.1 (2)O1—C1—C2—C3148.1 (3)
C7iv—Eu1—O1—C1160.9 (3)C1—C2—C3—C6169.9 (3)
Eu1vi—Eu1—O1—C1147.5 (2)C1—C2—C3—C468.2 (3)
O4i—Eu1—O1—Eu1vi64.20 (10)C2—C3—C4—C5145.9 (3)
O3ii—Eu1—O1—Eu1vi87.26 (10)C6—C3—C4—C592.7 (3)
O5iii—Eu1—O1—Eu1vi12.30 (9)Eu1i—O4—C5—O320.9 (6)
O2—Eu1—O1—Eu1vi146.10 (14)Eu1i—O4—C5—C4155.9 (2)
O6iv—Eu1—O1—Eu1vi16.32 (18)Eu1vii—O3—C5—O412.6 (5)
O1v—Eu1—O1—Eu1vi155.55 (11)Eu1vii—O3—C5—C4170.5 (2)
O1W—Eu1—O1—Eu1vi130.96 (10)C3—C4—C5—O423.6 (4)
O5iv—Eu1—O1—Eu1vi94.38 (19)C3—C4—C5—O3159.4 (3)
C1—Eu1—O1—Eu1vi147.5 (2)C2—C3—C6—C771.8 (3)
C7iv—Eu1—O1—Eu1vi13.4 (3)C4—C3—C6—C7166.4 (3)
O4i—Eu1—O2—C186.7 (2)Eu1ix—O6—C7—O517.1 (3)
O3ii—Eu1—O2—C153.6 (2)Eu1ix—O6—C7—C6158.3 (3)
O5iii—Eu1—O2—C124.2 (2)Eu1viii—O5—C7—O6164.6 (3)
O6iv—Eu1—O2—C1128.7 (2)Eu1ix—O5—C7—O616.8 (3)
O1v—Eu1—O2—C1118.6 (2)Eu1viii—O5—C7—C610.9 (6)
O1W—Eu1—O2—C1168.4 (2)Eu1ix—O5—C7—C6158.7 (3)
O1—Eu1—O2—C11.44 (18)C3—C6—C7—O640.3 (4)
O5iv—Eu1—O2—C1148.50 (18)C3—C6—C7—O5144.3 (3)
C7iv—Eu1—O2—C1171.89 (18)
Symmetry codes: (i) x+1, y, z1/2; (ii) x+1/2, y1/2, z1/2; (iii) x+3/2, y+3/2, z1/2; (iv) x, y+1, z1/2; (v) x+3/2, y1/2, z; (vi) x+3/2, y+1/2, z; (vii) x1/2, y+1/2, z1/2; (viii) x+3/2, y+3/2, z+1/2; (ix) x, y+1, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O3x0.852.062.913 (4)180
O1W—H2W···O2W0.851.982.807 (7)165
O2W—H3W···O6i0.851.942.794 (7)180
Symmetry codes: (i) x+1, y, z1/2; (x) x+1, y1, z1/2.

Experimental details

(I)(II)(III)
Crystal data
Chemical formulaC7H13EuO9·2(H2O)C7H9EuO7·H2OC7H9EuO7·H2O
Mr429.17375.12375.12
Crystal system, space groupTriclinic, P1Orthorhombic, Pca21Orthorhombic, Pbcn
Temperature (K)293293293
a, b, c (Å)8.0917 (13), 8.8680 (12), 10.115 (2)17.4543 (19), 7.8087 (6), 14.9761 (18)14.1085 (3), 7.7825 (2), 18.0083 (4)
α, β, γ (°)86.994 (17), 73.002 (16), 68.172 (15)90, 90, 9090, 90, 90
V3)643.06 (19)2041.2 (4)1977.30 (8)
Z288
Radiation typeMo KαMo KαMo Kα
µ (mm1)4.936.176.37
Crystal size (mm)0.80 × 0.40 × 0.200.70 × 0.26 × 0.240.32 × 0.30 × 0.24
Data collection
DiffractometerNonius KappaCCD
diffractometer
KappaCCD
diffractometer
Nonius KappaCCD
diffractometer
Absorption correctionFor a sphere
Dwiggins (1975)
For a cylinder mounted on the φ axis
Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3 for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959) p.302; Table 5.3.6 B for muR in the range 2.6-10.0. The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975) A31,146-148) is used with some modification.
For a sphere
Dwiggins (1975)
Tmin, Tmax0.110, 0.4390.370, 0.3830.235, 0.310
No. of measured, independent and
observed [I > 2σ(I)] reflections
10427, 2943, 2743 8250, 3215, 3040 15892, 3133, 2860
Rint0.0420.0760.041
(sin θ/λ)max1)0.6490.6670.726
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.024, 0.059, 1.10 0.063, 0.167, 1.14 0.029, 0.074, 1.13
No. of reflections294332153133
No. of parameters172291145
No. of restraints010
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.28, 0.561.39, 1.820.96, 1.16
Absolute structure?Refined as an inversion twin.?
Absolute structure parameter?0.38 (3)?

Computer programs: COLLECT (Nonius, 1998), Collect (Nonius, 1998), EVALCCD (Duisenberg et al., 2003), HKL-2000 (Otwinowski & Minor, 1997), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 1999), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999), PARST95 (Nardelli, 1995) and PLATON (Spek, 2009).

Hydrogen-bond geometry (Å, º) for (I) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O2i0.851.872.714 (4)172
O1W—H2W···O40.862.303.024 (4)141
O2W—H3W···O1Wii0.852.172.901 (4)144
O2W—H4W···O4Wiii0.851.992.824 (4)168
O3W—H5W···O5Wiv0.851.912.747 (4)166
O3W—H6W···O5Wiii0.851.962.797 (4)169
O4W—H7W···O60.852.042.877 (4)169
O4W—H8W···O4v0.852.022.869 (4)177
O5W—H9W···O40.851.882.717 (4)170
O5W—H10W···O4Wvi0.851.932.765 (4)166
Symmetry codes: (i) x, y+2, z; (ii) x1, y+2, z; (iii) x, y+1, z; (iv) x, y, z1; (v) x+1, y1, z; (vi) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) for (III) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O3i0.852.062.913 (4)180
O1W—H2W···O2W0.851.982.807 (7)165
O2W—H3W···O6ii0.851.942.794 (7)180
Symmetry codes: (i) x+1, y1, z1/2; (ii) x+1, y, z1/2.
 

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