Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807024361/wn2139sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807024361/wn2139Isup2.hkl |
CCDC reference: 650704
Erbium(III) oxide (0.163 g, 0.5 mmol), edta (0.286 g, 0.8 mmol) and perchloric acid (0.385 mmol) were dissolved in methanol (5 ml) and water (5 ml). This solution was sealed in a Teflon-lined, stainless-steel autoclave (20 ml capacity) and heated to 433 K for 4 days. It was cooled to room temperature at 5 K h-1 to obtain colorless block-shaped crystals. CH&N elemental analysis. Calc. for C10H17ErN2O10: C 24.38, H 3.48, N 5.69%. Found 24.20, H 3.50, N 5.66%.
The edta tetraanion is disordered across a mirror plane; only atoms O1, O2 and C1 have full site occupany, the other atoms having 0.5 occupancy. For the disordered atoms, the C—O distances were restrained to 1.25±0.01 Å, the C—N distances to 1.45±0.01 Å and the C—C distances to 1.50±0.01 Å. The displacement parameters of the ordered and disordered C, N and O atoms were restrained to be nearly isotropic.
Together with the [(C10H12N2O8)Er] monoanion, the formula unit has one hydronium ion and one water molecule. Because Z is 4, as well as the fact that O3o and O1w both lie on general positions, these two O atoms are disordered; the sum of their site occupancies should be unity. The occupancies refined to 0.67 (1) and 0.33 (1), and were then fixed at these values. The 'o' and 'w' labels are arbitrary and do not imply that O3o is the hydronium and O1w the water O atoms. Their H atoms could not be placed in any chemically sensible positions.
The carbon-bound H atoms were placed at calculated positions (C—H 0.97 Å), and they were included in the refinement in the riding model approximation with Uiso(H) set equal to 1.2Ueq(C).
The edta tetraanion chelates a large number of lanthanide atoms (CSD Version 5.28, November 2006; Allen, 2002); among these are several examples of [edta-Ln]- anions whose negative charge is balanced by a unipositive cation. One erbium(III) derivative has an ammonium cation as the counterion; the metal atom itself exists in an eight-coordinate environment, and the water-coordinated cation, anion and solvent water molecules are linked through hydrogen bonds into a three-dimensional network structure (Filippova et al., 1977; Polynova et al., 1986). A hydrothermal synthesis yields the expected [edta-Er]- as a hydronium monohydrate (Fig. 1). The edta chelates the metal atom, and it also functions as a bridge to link adjacent anions into a polyanionic layer. The disordered hydronium cation and water molecules occupy the space between the layers; the metal shows a square-antiprismatic coordination (Fig. 2).
For related literature, see: Allen (2002); Filippova et al. (1977); Polynova et al. (1986).
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).
(H3O)[Er(C10H12N2O8)]·H2O | F(000) = 956 |
Mr = 492.52 | Dx = 2.103 Mg m−3 |
Orthorhombic, Pbcm | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2c 2b | Cell parameters from 4071 reflections |
a = 6.5783 (1) Å | θ = 3.4–27.6° |
b = 12.8191 (2) Å | µ = 5.45 mm−1 |
c = 18.4454 (3) Å | T = 295 K |
V = 1555.46 (4) Å3 | Block, colourless |
Z = 4 | 0.28 × 0.25 × 0.17 mm |
Bruker APEXII diffractometer | 1844 independent reflections |
Radiation source: medium-focus sealed tube | 1625 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.042 |
φ and ω scans | θmax = 27.5°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −8→8 |
Tmin = 0.397, Tmax = 0.516 | k = −15→16 |
13530 measured reflections | l = −23→21 |
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)] = 0.022 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.055 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0306P)2 + 0.6341P] where P = (Fo2 + 2Fc2)/3 |
1844 reflections | (Δ/σ)max = 0.001 |
178 parameters | Δρmax = 0.58 e Å−3 |
127 restraints | Δρmin = −0.60 e Å−3 |
(H3O)[Er(C10H12N2O8)]·H2O | V = 1555.46 (4) Å3 |
Mr = 492.52 | Z = 4 |
Orthorhombic, Pbcm | Mo Kα radiation |
a = 6.5783 (1) Å | µ = 5.45 mm−1 |
b = 12.8191 (2) Å | T = 295 K |
c = 18.4454 (3) Å | 0.28 × 0.25 × 0.17 mm |
Bruker APEXII diffractometer | 1844 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 1625 reflections with I > 2σ(I) |
Tmin = 0.397, Tmax = 0.516 | Rint = 0.042 |
13530 measured reflections |
R[F2 > 2σ(F2)] = 0.022 | 127 restraints |
wR(F2) = 0.055 | H-atom parameters constrained |
S = 1.05 | Δρmax = 0.58 e Å−3 |
1844 reflections | Δρmin = −0.60 e Å−3 |
178 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Er1 | 0.10963 (3) | 0.056040 (16) | 0.2500 | 0.01744 (9) | |
O1 | 0.0662 (5) | 0.0340 (3) | 0.12694 (17) | 0.0470 (8) | |
O2 | 0.1143 (5) | 0.0745 (3) | 0.0123 (2) | 0.0657 (12) | |
O3O | −0.2598 (19) | 0.2009 (9) | −0.0529 (6) | 0.193 (4) | 0.67 |
O1W | 0.467 (3) | 0.0586 (11) | −0.0724 (9) | 0.110 (5) | 0.33 |
C1 | 0.1464 (6) | 0.0880 (4) | 0.0798 (2) | 0.0353 (10) | |
O3 | 0.4409 (6) | 0.0109 (4) | 0.2763 (3) | 0.0257 (12) | 0.50 |
O4 | 0.7699 (6) | 0.0110 (3) | 0.2591 (12) | 0.023 (3) | 0.50 |
N1 | 0.3667 (8) | 0.1616 (5) | 0.1747 (3) | 0.0215 (12) | 0.50 |
C2 | 0.296 (5) | 0.178 (2) | 0.1012 (6) | 0.026 (6) | 0.50 |
H2A | 0.4104 | 0.1792 | 0.0681 | 0.031* | 0.50 |
H2B | 0.2265 | 0.2448 | 0.0979 | 0.031* | 0.50 |
C3 | 0.429 (3) | 0.2612 (12) | 0.2061 (14) | 0.018 (4) | 0.50 |
H3A | 0.3359 | 0.3158 | 0.1910 | 0.021* | 0.50 |
H3B | 0.5641 | 0.2794 | 0.1895 | 0.021* | 0.50 |
C4 | 0.5488 (10) | 0.0954 (6) | 0.1695 (4) | 0.0259 (16) | 0.50 |
H4A | 0.6652 | 0.1389 | 0.1581 | 0.031* | 0.50 |
H4B | 0.5310 | 0.0462 | 0.1300 | 0.031* | 0.50 |
C5 | 0.5917 (7) | 0.0360 (5) | 0.2383 (5) | 0.020 (2) | 0.50 |
O3' | −0.0518 (7) | 0.2097 (3) | 0.2261 (3) | 0.0277 (14) | 0.50 |
O4' | −0.1176 (5) | 0.3776 (3) | 0.2392 (8) | 0.023 (3) | 0.50 |
N1' | 0.2526 (8) | 0.2089 (4) | 0.3255 (3) | 0.0220 (12) | 0.50 |
C2' | 0.279 (5) | 0.171 (2) | 0.3991 (6) | 0.038 (9) | 0.50 |
H2'1 | 0.4188 | 0.1480 | 0.4047 | 0.046* | 0.50 |
H2'2 | 0.2592 | 0.2294 | 0.4322 | 0.046* | 0.50 |
C3' | 0.427 (3) | 0.2520 (16) | 0.2867 (15) | 0.031 (6) | 0.50 |
H3'1 | 0.5445 | 0.2101 | 0.3000 | 0.037* | 0.50 |
H3'2 | 0.4510 | 0.3213 | 0.3060 | 0.037* | 0.50 |
C4' | 0.0935 (9) | 0.2884 (6) | 0.3296 (4) | 0.0277 (16) | 0.50 |
H4'1 | 0.1557 | 0.3558 | 0.3384 | 0.033* | 0.50 |
H4'2 | 0.0051 | 0.2729 | 0.3703 | 0.033* | 0.50 |
C5' | −0.0325 (8) | 0.2940 (4) | 0.2612 (6) | 0.022 (2) | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Er1 | 0.01162 (11) | 0.01093 (13) | 0.02976 (15) | −0.00036 (8) | 0.000 | 0.000 |
O1 | 0.0624 (19) | 0.0457 (19) | 0.0329 (17) | −0.0331 (16) | −0.0058 (15) | −0.0023 (14) |
O2 | 0.093 (3) | 0.071 (3) | 0.0324 (19) | −0.039 (2) | −0.0147 (17) | 0.0000 (18) |
O3O | 0.181 (7) | 0.192 (8) | 0.206 (8) | 0.049 (7) | −0.044 (7) | 0.036 (7) |
O1W | 0.122 (8) | 0.108 (9) | 0.099 (8) | 0.043 (7) | 0.022 (8) | 0.007 (7) |
C1 | 0.039 (2) | 0.036 (2) | 0.031 (2) | −0.0068 (18) | −0.0096 (18) | −0.0033 (19) |
O3 | 0.017 (2) | 0.020 (2) | 0.041 (3) | 0.0008 (19) | 0.0019 (18) | 0.006 (2) |
O4 | 0.0124 (15) | 0.0214 (19) | 0.035 (9) | 0.0022 (14) | −0.002 (3) | −0.002 (3) |
N1 | 0.021 (3) | 0.021 (3) | 0.022 (3) | 0.000 (2) | −0.004 (2) | −0.003 (3) |
C2 | 0.032 (7) | 0.022 (7) | 0.024 (9) | −0.014 (5) | −0.006 (5) | −0.009 (5) |
C3 | 0.024 (6) | 0.016 (6) | 0.013 (5) | −0.005 (5) | −0.005 (4) | 0.008 (5) |
C4 | 0.022 (3) | 0.025 (4) | 0.030 (4) | 0.000 (3) | 0.006 (3) | −0.003 (3) |
C5 | 0.015 (2) | 0.011 (3) | 0.033 (7) | −0.0030 (18) | 0.001 (3) | −0.005 (3) |
O3' | 0.0187 (17) | 0.016 (2) | 0.048 (4) | 0.0036 (18) | −0.0081 (18) | −0.006 (2) |
O4' | 0.0220 (17) | 0.0112 (18) | 0.037 (8) | 0.0022 (14) | −0.004 (3) | 0.003 (3) |
N1' | 0.022 (2) | 0.017 (3) | 0.027 (3) | −0.008 (3) | 0.000 (2) | 0.001 (3) |
C2' | 0.040 (10) | 0.043 (12) | 0.032 (10) | −0.008 (7) | 0.004 (6) | −0.008 (7) |
C3' | 0.031 (7) | 0.022 (7) | 0.040 (10) | −0.016 (5) | −0.005 (5) | −0.006 (6) |
C4' | 0.028 (3) | 0.019 (4) | 0.036 (4) | 0.003 (3) | 0.007 (3) | −0.003 (3) |
C5' | 0.0131 (19) | 0.016 (3) | 0.036 (7) | −0.001 (2) | 0.003 (3) | 0.001 (4) |
Er1—O1 | 2.305 (3) | C3—C3' | 1.491 (8) |
Er1—O1i | 2.305 (3) | C3—H3A | 0.9700 |
Er1—O3 | 2.307 (4) | C3—H3B | 0.9700 |
Er1—O4ii | 2.314 (4) | C4—C5 | 1.508 (8) |
Er1—O3' | 2.281 (4) | C4—H4A | 0.9700 |
Er1—O4'iii | 2.297 (5) | C4—H4B | 0.9700 |
Er1—N1 | 2.574 (6) | O3'—C5' | 1.266 (7) |
Er1—N1' | 2.582 (6) | O4'—C5' | 1.274 (7) |
O1—C1 | 1.231 (5) | O4'—Er1v | 2.297 (5) |
O2—C1 | 1.273 (6) | N1'—C2' | 1.452 (10) |
C1—C2'i | 1.44 (3) | N1'—C4' | 1.462 (7) |
C1—C2 | 1.57 (3) | N1'—C3' | 1.464 (10) |
O3—C5 | 1.256 (7) | C2'—C1i | 1.44 (3) |
O4—C5 | 1.274 (7) | C2'—H2'1 | 0.9700 |
O4—Er1iv | 2.314 (4) | C2'—H2'2 | 0.9700 |
N1—C3 | 1.461 (9) | C3'—H3'1 | 0.9700 |
N1—C2 | 1.449 (10) | C3'—H3'2 | 0.9700 |
N1—C4 | 1.471 (7) | C4'—C5' | 1.512 (8) |
C2—H2A | 0.9700 | C4'—H4'1 | 0.9700 |
C2—H2B | 0.9700 | C4'—H4'2 | 0.9700 |
O3'i—Er1—O3' | 22.3 (2) | N1i—Er1—N1 | 65.4 (2) |
O3'i—Er1—O4'iii | 152.57 (17) | C1—O1—Er1 | 125.0 (3) |
O3'—Er1—O4'iii | 148.6 (2) | O1—C1—O2 | 122.9 (4) |
O3'i—Er1—O4'vi | 148.6 (2) | O1—C1—C2'i | 119.3 (8) |
O3'—Er1—O4'vi | 152.57 (17) | O2—C1—C2'i | 117.8 (8) |
O4'iii—Er1—O4'vi | 10.0 (8) | O1—C1—C2 | 120.4 (7) |
O3'i—Er1—O1i | 81.84 (15) | O2—C1—C2 | 116.7 (7) |
O3'—Er1—O1i | 103.82 (15) | C5—O3—Er1 | 124.3 (4) |
O4'iii—Er1—O1i | 88.1 (4) | C5—O4—Er1iv | 143.5 (9) |
O4'vi—Er1—O1i | 78.2 (4) | C3—N1—C2 | 109.5 (15) |
O3'i—Er1—O1 | 103.82 (15) | C3—N1—C4 | 107.6 (9) |
O3'—Er1—O1 | 81.84 (15) | C2—N1—C4 | 106.6 (10) |
O4'iii—Er1—O1 | 78.2 (4) | C3—N1—Er1 | 115.4 (12) |
O4'vi—Er1—O1 | 88.1 (4) | C2—N1—Er1 | 111.7 (15) |
O1i—Er1—O1 | 159.90 (15) | C4—N1—Er1 | 105.5 (4) |
O3'i—Er1—O4vii | 77.28 (19) | N1—C2—C1 | 109.2 (19) |
O3'—Er1—O4vii | 75.62 (19) | N1—C2—H2A | 109.8 |
O4'iii—Er1—O4vii | 76.55 (14) | C1—C2—H2A | 109.8 |
O4'vi—Er1—O4vii | 77.29 (16) | N1—C2—H2B | 109.8 |
O1i—Er1—O4vii | 85.5 (5) | C1—C2—H2B | 109.8 |
O1—Er1—O4vii | 77.2 (5) | H2A—C2—H2B | 108.3 |
O3'i—Er1—O4ii | 75.62 (19) | N1—C3—C3' | 109 (2) |
O3'—Er1—O4ii | 77.28 (19) | N1—C3—H3A | 109.9 |
O4'iii—Er1—O4ii | 77.29 (16) | C3'—C3—H3A | 109.9 |
O4'vi—Er1—O4ii | 76.55 (14) | N1—C3—H3B | 109.9 |
O1i—Er1—O4ii | 77.2 (5) | C3'—C3—H3B | 109.9 |
O1—Er1—O4ii | 85.5 (5) | H3A—C3—H3B | 108.3 |
O4vii—Er1—O4ii | 8.3 (11) | N1—C4—C5 | 112.9 (5) |
O3'i—Er1—O3 | 128.02 (17) | N1—C4—H4A | 109.0 |
O3'—Er1—O3 | 134.21 (16) | C5—C4—H4A | 109.0 |
O4'iii—Er1—O3 | 75.33 (18) | N1—C4—H4B | 109.0 |
O4'vi—Er1—O3 | 73.15 (17) | C5—C4—H4B | 109.0 |
O1i—Er1—O3 | 83.05 (14) | H4A—C4—H4B | 107.8 |
O1—Er1—O3 | 107.07 (15) | O4—C5—O3 | 119.6 (10) |
O4vii—Er1—O3 | 149.9 (2) | O4—C5—C4 | 123.6 (9) |
O4ii—Er1—O3 | 146.6 (3) | O3—C5—C4 | 116.8 (5) |
O3'i—Er1—O3i | 134.21 (16) | C5'—O3'—Er1 | 126.3 (4) |
O3'—Er1—O3i | 128.02 (17) | C5'—O4'—Er1v | 143.0 (7) |
O4'iii—Er1—O3i | 73.15 (17) | C2'—N1'—C4' | 105.6 (11) |
O4'vi—Er1—O3i | 75.33 (18) | C2'—N1'—C3' | 119.2 (19) |
O1i—Er1—O3i | 107.07 (15) | C4'—N1'—C3' | 109.0 (11) |
O1—Er1—O3i | 83.05 (14) | C2'—N1'—Er1 | 107.3 (14) |
O4vii—Er1—O3i | 146.6 (3) | C4'—N1'—Er1 | 107.2 (4) |
O4ii—Er1—O3i | 149.9 (2) | C3'—N1'—Er1 | 108.0 (11) |
O3—Er1—O3i | 24.3 (2) | C1i—C2'—N1' | 115 (2) |
O3'i—Er1—N1i | 75.35 (18) | C1i—C2'—H2'1 | 108.5 |
O3'—Er1—N1i | 87.47 (17) | N1'—C2'—H2'1 | 108.5 |
O4'iii—Er1—N1i | 123.8 (3) | C1i—C2'—H2'2 | 108.5 |
O4'vi—Er1—N1i | 117.5 (3) | N1'—C2'—H2'2 | 108.5 |
O1i—Er1—N1i | 67.31 (14) | H2'1—C2'—H2'2 | 107.5 |
O1—Er1—N1i | 132.67 (14) | N1'—C3'—C3 | 122 (2) |
O4vii—Er1—N1i | 143.6 (4) | N1'—C3'—H3'1 | 107.0 |
O4ii—Er1—N1i | 136.6 (5) | C3—C3'—H3'1 | 107.0 |
O3—Er1—N1i | 52.96 (18) | N1'—C3'—H3'2 | 107.0 |
O3i—Er1—N1i | 67.97 (16) | C3—C3'—H3'2 | 107.0 |
O3'i—Er1—N1 | 87.47 (17) | H3'1—C3'—H3'2 | 106.7 |
O3'—Er1—N1 | 75.35 (18) | N1'—C4'—C5' | 112.5 (5) |
O4'iii—Er1—N1 | 117.5 (3) | N1'—C4'—H4'1 | 109.1 |
O4'vi—Er1—N1 | 123.8 (3) | C5'—C4'—H4'1 | 109.1 |
O1i—Er1—N1 | 132.67 (14) | N1'—C4'—H4'2 | 109.1 |
O1—Er1—N1 | 67.31 (14) | C5'—C4'—H4'2 | 109.1 |
O4vii—Er1—N1 | 136.6 (5) | H4'1—C4'—H4'2 | 107.8 |
O4ii—Er1—N1 | 143.6 (4) | O4'—C5'—O3' | 120.7 (8) |
O3—Er1—N1 | 67.97 (16) | O4'—C5'—C4' | 123.2 (8) |
O3i—Er1—N1 | 52.96 (18) | O3'—C5'—C4' | 116.1 (5) |
O3'i—Er1—O1—C1 | 68.8 (4) | Er1iv—O4—C5—O3 | −155.3 (15) |
O3'—Er1—O1—C1 | 65.0 (4) | Er1iv—O4—C5—C4 | 25 (2) |
O4'iii—Er1—O1—C1 | −139.2 (4) | Er1—O3—C5—O4 | 177.0 (7) |
O4'vi—Er1—O1—C1 | −140.5 (4) | Er1—O3—C5—C4 | −2.8 (9) |
O1i—Er1—O1—C1 | 173.1 (3) | N1—C4—C5—O4 | −149.2 (9) |
O4vii—Er1—O1—C1 | 142.1 (4) | N1—C4—C5—O3 | 30.6 (9) |
O4ii—Er1—O1—C1 | 142.8 (4) | O3'i—Er1—O3'—C5' | 37.7 (6) |
O3—Er1—O1—C1 | −68.8 (4) | O4'iii—Er1—O3'—C5' | 157.3 (9) |
O3i—Er1—O1—C1 | −65.1 (4) | O4'vi—Er1—O3'—C5' | 138.5 (9) |
N1i—Er1—O1—C1 | −13.8 (5) | O1i—Er1—O3'—C5' | 47.6 (6) |
N1—Er1—O1—C1 | −12.4 (4) | O1—Er1—O3'—C5' | −152.0 (6) |
Er1—O1—C1—O2 | −178.3 (3) | O4vii—Er1—O3'—C5' | 129.2 (8) |
Er1—O1—C1—C2'i | 0.6 (13) | O4ii—Er1—O3'—C5' | 120.8 (8) |
Er1—O1—C1—C2 | 1.8 (11) | O3—Er1—O3'—C5' | −46.1 (7) |
O3'i—Er1—O3—C5 | −81.7 (6) | O3i—Er1—O3'—C5' | −77.5 (6) |
O3'—Er1—O3—C5 | −53.1 (6) | N1i—Er1—O3'—C5' | −18.3 (6) |
O4'iii—Er1—O3—C5 | 114.5 (7) | N1—Er1—O3'—C5' | −83.5 (6) |
O4'vi—Er1—O3—C5 | 124.6 (7) | O3'i—Er1—N1'—C2' | 116.0 (12) |
O1i—Er1—O3—C5 | −155.7 (6) | O3'—Er1—N1'—C2' | 136.3 (12) |
O1—Er1—O3—C5 | 42.1 (6) | O4'iii—Er1—N1'—C2' | −32.6 (13) |
O4vii—Er1—O3—C5 | 135.9 (11) | O4'vi—Er1—N1'—C2' | −23.9 (13) |
O4ii—Er1—O3—C5 | 150.5 (10) | O1i—Er1—N1'—C2' | 19.0 (12) |
O3i—Er1—O3—C5 | 33.1 (6) | O1—Er1—N1'—C2' | −169.1 (12) |
N1i—Er1—O3—C5 | −88.9 (6) | O4vii—Er1—N1'—C2' | 84.9 (13) |
N1—Er1—O3—C5 | −13.9 (6) | O4ii—Er1—N1'—C2' | 77.2 (13) |
O3'i—Er1—N1—C3 | 40.9 (8) | O3—Er1—N1'—C2' | −69.9 (12) |
O3'—Er1—N1—C3 | 59.8 (8) | O3i—Er1—N1'—C2' | −90.6 (12) |
O4'iii—Er1—N1—C3 | −151.0 (9) | N1i—Er1—N1'—C2' | −67.5 (13) |
O4'vi—Er1—N1—C3 | −141.9 (9) | N1—Er1—N1'—C2' | −141.7 (12) |
O1i—Er1—N1—C3 | −35.6 (9) | O3'i—Er1—N1'—C4' | 2.9 (4) |
O1—Er1—N1—C3 | 147.0 (8) | O3'—Er1—N1'—C4' | 23.2 (4) |
O4vii—Er1—N1—C3 | 109.3 (9) | O4'iii—Er1—N1'—C4' | −145.7 (5) |
O4ii—Er1—N1—C3 | 102.3 (10) | O4'vi—Er1—N1'—C4' | −137.0 (5) |
O3—Er1—N1—C3 | −92.2 (8) | O1i—Er1—N1'—C4' | −94.1 (4) |
O3i—Er1—N1—C3 | −114.3 (9) | O1—Er1—N1'—C4' | 77.8 (5) |
N1i—Er1—N1—C3 | −34.2 (8) | O4vii—Er1—N1'—C4' | −28.2 (7) |
O3'i—Er1—N1—C2 | −85.1 (9) | O4ii—Er1—N1'—C4' | −35.8 (6) |
O3'—Er1—N1—C2 | −66.1 (9) | O3—Er1—N1'—C4' | 177.0 (4) |
O4'iii—Er1—N1—C2 | 83.1 (10) | O3i—Er1—N1'—C4' | 156.3 (4) |
O4'vi—Er1—N1—C2 | 92.1 (10) | N1i—Er1—N1'—C4' | 179.4 (8) |
O1i—Er1—N1—C2 | −161.6 (9) | N1—Er1—N1'—C4' | 105.2 (4) |
O1—Er1—N1—C2 | 21.0 (9) | O3'i—Er1—N1'—C3' | −114.4 (12) |
O4vii—Er1—N1—C2 | −16.7 (10) | O3'—Er1—N1'—C3' | −94.1 (11) |
O4ii—Er1—N1—C2 | −23.7 (11) | O4'iii—Er1—N1'—C3' | 97.0 (12) |
O3—Er1—N1—C2 | 141.8 (9) | O4'vi—Er1—N1'—C3' | 105.7 (12) |
O3i—Er1—N1—C2 | 119.7 (9) | O1i—Er1—N1'—C3' | 148.6 (11) |
N1i—Er1—N1—C2 | −160.1 (9) | O1—Er1—N1'—C3' | −39.5 (12) |
O3'i—Er1—N1—C4 | 159.4 (4) | O4vii—Er1—N1'—C3' | −145.5 (12) |
O3'—Er1—N1—C4 | 178.4 (4) | O4ii—Er1—N1'—C3' | −153.1 (12) |
O4'iii—Er1—N1—C4 | −32.4 (6) | O3—Er1—N1'—C3' | 59.7 (11) |
O4'vi—Er1—N1—C4 | −23.3 (6) | O3i—Er1—N1'—C3' | 39.0 (11) |
O1i—Er1—N1—C4 | 83.0 (5) | N1i—Er1—N1'—C3' | 62.1 (12) |
O1—Er1—N1—C4 | −94.5 (4) | N1—Er1—N1'—C3' | −12.1 (11) |
O4vii—Er1—N1—C4 | −132.1 (5) | C4'—N1'—C2'—C1i | 86.9 (16) |
O4ii—Er1—N1—C4 | −139.2 (7) | C3'—N1'—C2'—C1i | −150.2 (16) |
O3—Er1—N1—C4 | 26.4 (4) | Er1—N1'—C2'—C1i | −27.2 (18) |
O3i—Er1—N1—C4 | 4.2 (4) | C2'—N1'—C3'—C3 | 161 (2) |
N1i—Er1—N1—C4 | 84.4 (4) | C4'—N1'—C3'—C3 | −78 (2) |
C3—N1—C2—C1 | −155.5 (14) | Er1—N1'—C3'—C3 | 38 (3) |
C4—N1—C2—C1 | 88.4 (15) | N1—C3—C3'—N1' | −49 (3) |
Er1—N1—C2—C1 | −26.4 (15) | C2'—N1'—C4'—C5' | −148.8 (16) |
O1—C1—C2—N1 | 18.6 (18) | C3'—N1'—C4'—C5' | 82.1 (14) |
O2—C1—C2—N1 | −161.3 (9) | Er1—N1'—C4'—C5' | −34.6 (6) |
C2—N1—C3—C3' | 159 (2) | Er1v—O4'—C5'—O3' | −161.0 (10) |
C4—N1—C3—C3' | −85 (2) | Er1v—O4'—C5'—C4' | 19.5 (18) |
Er1—N1—C3—C3' | 32 (2) | Er1—O3'—C5'—O4' | 174.1 (6) |
C3—N1—C4—C5 | 85.9 (13) | Er1—O3'—C5'—C4' | −6.5 (9) |
C2—N1—C4—C5 | −156.7 (15) | N1'—C4'—C5'—O4' | −150.5 (8) |
Er1—N1—C4—C5 | −37.8 (6) | N1'—C4'—C5'—O3' | 30.0 (9) |
Symmetry codes: (i) x, y, −z+1/2; (ii) x−1, y, z; (iii) −x, y−1/2, z; (iv) x+1, y, z; (v) −x, y+1/2, z; (vi) −x, y−1/2, −z+1/2; (vii) x−1, y, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | (H3O)[Er(C10H12N2O8)]·H2O |
Mr | 492.52 |
Crystal system, space group | Orthorhombic, Pbcm |
Temperature (K) | 295 |
a, b, c (Å) | 6.5783 (1), 12.8191 (2), 18.4454 (3) |
V (Å3) | 1555.46 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 5.45 |
Crystal size (mm) | 0.28 × 0.25 × 0.17 |
Data collection | |
Diffractometer | Bruker APEXII |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.397, 0.516 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13530, 1844, 1625 |
Rint | 0.042 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.022, 0.055, 1.05 |
No. of reflections | 1844 |
No. of parameters | 178 |
No. of restraints | 127 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.58, −0.60 |
Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).
Er1—O1 | 2.305 (3) | Er1—O4'ii | 2.297 (5) |
Er1—O3 | 2.307 (4) | Er1—N1 | 2.574 (6) |
Er1—O4i | 2.314 (4) | Er1—N1' | 2.582 (6) |
Er1—O3' | 2.281 (4) |
Symmetry codes: (i) x−1, y, z; (ii) −x, y−1/2, z. |
The edta tetraanion chelates a large number of lanthanide atoms (CSD Version 5.28, November 2006; Allen, 2002); among these are several examples of [edta-Ln]- anions whose negative charge is balanced by a unipositive cation. One erbium(III) derivative has an ammonium cation as the counterion; the metal atom itself exists in an eight-coordinate environment, and the water-coordinated cation, anion and solvent water molecules are linked through hydrogen bonds into a three-dimensional network structure (Filippova et al., 1977; Polynova et al., 1986). A hydrothermal synthesis yields the expected [edta-Er]- as a hydronium monohydrate (Fig. 1). The edta chelates the metal atom, and it also functions as a bridge to link adjacent anions into a polyanionic layer. The disordered hydronium cation and water molecules occupy the space between the layers; the metal shows a square-antiprismatic coordination (Fig. 2).