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metal-organic compounds
The DyIII atom in the title compound, (H3O)[Dy(C10H12N2O8)]·H2O, is N,N′,O,O′,O′′,O′′′-chelated by the edta tetraanion; it is also linked to the O atoms of two other tetraaanions in the polyanionic layer. The metal atom (site symmetry m) exists in a square-antiprismatic DyO6N2 geometry. The tetraanion is disordered over a mirror plane. The oxonium cation and water molecule are disordered, in a 2:1 ratio, and these occupy the space between adjacent layers. They probably interact with the layers by way of O—H
O hydrogen bonds, but the H atoms could not be located.
O hydrogen bonds, but the H atoms could not be located.Supporting information
 | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807025044/hb2422sup1.cif |
 | Structure factor file (CIF format) https://doi.org/10.1107/S1600536807025044/hb2422Isup2.hkl |
CCDC reference: 654711
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean
![[sigma]](//journals.iucr.org/logos/entities/sigma_rmgif.gif)
(O-C) = 0.004 Å - H-atom completeness 71%
- Disorder in main residue
- R factor = 0.017
- wR factor = 0.050
- Data-to-parameter ratio = 10.5
![[sigma]](http://journals.iucr.org/logos/entities/sigma_rmgif.gif){kind=small}
(O-C) = 0.004 ÅcheckCIF/PLATON results
No syntax errors found
Alert level B PLAT301_ALERT_3_B Main Residue Disorder ......................... 40.00 Perc.
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.425 0.648 Tmin and Tmax expected: 0.331 0.622 RR = 1.231 Please check that your absorption correction is appropriate. CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 487.76 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 10.00 120.11 H 1.01 12.00 12.10 N 14.01 2.00 28.01 O 16.00 10.00 159.99 Dy 162.50 1.00 162.50 Calculated formula weight 482.71 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 487.76 PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ? PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.23 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.96 PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT215_ALERT_3_C Disordered C2 has ADP max/min Ratio ....... 3.10 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.60 Ratio PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.66 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C3' PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C3 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.02 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O3O PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O1W PLAT430_ALERT_2_C Short Inter D...A Contact O2 .. O1W .. 2.87 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 3.20 Deg. C2' -C1 -C2 6.556 1.555 1.555
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C10 H17 Dy1 N2 O10 Atom count from the _atom_site data: C10 H12 Dy1 N2 O10 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C10 H17 Dy N2 O10 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 40.00 40.00 0.00 H 68.00 48.00 20.00 Dy 4.00 4.00 0.00 N 8.00 8.00 0.00 O 40.00 40.00 0.00 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 127
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 23 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 12 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Alert level B
Alert level C
Alert level G
Related literature top
For the isostructural erbium(III) and holonium(III) analogs, see: You et al. (2007a,b).
S2. Experimental top
Dysprosium(III) oxide (0.162 g, 0.5 mmol), ethylenediaminetetraacetic acid (edta) (0.286 g, 0.8 mmol), perchloric acid (0.385 mmol) and oxalic acid (0.042 g, 0.175 mmol) were dissolved in a mixture of 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 blocks of (I).
S3. Refinement top
The edta tetraanion is disordered about a mirror plane; only the O1, O2 and C1 atoms of the molecule have full occupany, the other atoms being given 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 vibration of the ordered and disordered C, N and O atoms were restrained to be nearly isotropic.
Along with the [(C10H12N2O8)Dy] monoanion, the formula unit should have one hydronium ion and one water molecule; their respective O atoms are disordered and the sum of their occupancies should be unity. As the occupancy refined to 0.67 (1):0.33 (1), the occupancies were then fixed at this ratio. The 'o' and 'w' labels are arbitrary and do not mean that the O3o is the hydronium and the O1w the water O atoms. Their H atoms could not be placed with any confidence.
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 U(H) set to 1.2Ueq(C).
Structure description top
The erbium(III) and holonium(III) derivatives of edta have recently been reported (You et al., 2007a, b). The dysprosium analog described here is isostructural.
For the isostructural erbium(III) and holonium(III) analogs, see: You et al. (2007a,b).
Computing details top
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).
Figures top
![[Figure 1]](http://journals.iucr.org/e/issues/2007/07/00/hb2422/hb2422fig1thm.gif)
| Fig. 1. View of a portion of the polyanionic structure of (I). Displacement ellipsoids are drawn at the 50% probability level, and H atoms are shown as spheres of arbitrary radius. Symmetry codes are as given in Table 1. The disordered hydronium and water species are not shown. |
Poly[hydronium [dysprosium(III)-µ3-(ethylenediaminetetraacetato-\k8N,N',O,O',O'',O''':O'''':O''''')] monohydrate] top
Crystal data top
| (H3O)[Dy(C10H12N2O8)]·H2O | F(000) = 948 |
| Mr = 487.76 | Dx = 2.039 Mg m−3 |
| Orthorhombic, Pbcm | Mo Kα radiation, λ = 0.71073 Å |
| Hall symbol: -P 2c 2b | Cell parameters from 8499 reflections |
| a = 6.6271 (3) Å | θ = 3.1–27.5° |
| b = 12.9233 (6) Å | µ = 4.76 mm−1 |
| c = 18.5496 (9) Å | T = 295 K |
| V = 1588.6 (1) Å3 | Block, colorless |
| Z = 4 | 0.30 × 0.20 × 0.10 mm |
Data collection top
| Bruker APEX II CCD diffractometer | 1873 independent reflections |
| Radiation source: medium-focus sealed tube | 1784 reflections with I > 2σ(I) |
| Graphite monochromator | Rint = 0.022 |
| φ and ω scans | θmax = 27.5°, θmin = 3.1° |
| Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −8→7 |
| Tmin = 0.425, Tmax = 0.648 | k = −16→16 |
| 13726 measured reflections | l = −23→23 |
Refinement top
| 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)] = 0.017 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.050 | H-atom parameters constrained |
| S = 1.05 | w = 1/[σ2(Fo2) + (0.036P)2 + 0.7002P] where P = (Fo2 + 2Fc2)/3 |
| 1873 reflections | (Δ/σ)max = 0.001 |
| 178 parameters | Δρmax = 0.66 e Å−3 |
| 127 restraints | Δρmin = −0.47 e Å−3 |
Crystal data top
| (H3O)[Dy(C10H12N2O8)]·H2O | V = 1588.6 (1) Å3 |
| Mr = 487.76 | Z = 4 |
| Orthorhombic, Pbcm | Mo Kα radiation |
| a = 6.6271 (3) Å | µ = 4.76 mm−1 |
| b = 12.9233 (6) Å | T = 295 K |
| c = 18.5496 (9) Å | 0.30 × 0.20 × 0.10 mm |
Data collection top
| Bruker APEX II CCD diffractometer | 1873 independent reflections |
| Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 1784 reflections with I > 2σ(I) |
| Tmin = 0.425, Tmax = 0.648 | Rint = 0.022 |
| 13726 measured reflections |
Refinement top
| R[F2 > 2σ(F2)] = 0.017 | 127 restraints |
| wR(F2) = 0.050 | H-atom parameters constrained |
| S = 1.05 | Δρmax = 0.66 e Å−3 |
| 1873 reflections | Δρmin = −0.47 e Å−3 |
| 178 parameters |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
| x | y | z | Uiso*/Ueq | Occ. (<1) | |
| Dy1 | 0.10881 (2) | 0.052175 (11) | 0.2500 | 0.01807 (8) | |
| O1 | 0.0672 (5) | 0.0318 (2) | 0.12603 (13) | 0.0541 (7) | |
| O2 | 0.1160 (4) | 0.0739 (3) | 0.01246 (15) | 0.0666 (9) | |
| O3O | −0.2534 (15) | 0.2034 (7) | −0.0555 (4) | 0.188 (4) | 0.67 |
| O1W | 0.477 (2) | 0.0661 (9) | −0.0728 (7) | 0.104 (4) | 0.33 |
| C1 | 0.1473 (5) | 0.0859 (3) | 0.07918 (16) | 0.0388 (6) | |
| O3 | 0.4405 (5) | 0.0077 (3) | 0.27636 (19) | 0.0268 (7) | 0.50 |
| O4 | 0.7680 (4) | 0.0071 (2) | 0.2593 (8) | 0.025 (2) | 0.50 |
| N1 | 0.3675 (6) | 0.1575 (3) | 0.1752 (2) | 0.0227 (8) | 0.50 |
| C2 | 0.301 (4) | 0.1750 (15) | 0.1018 (5) | 0.027 (3) | 0.50 |
| H2A | 0.4157 | 0.1749 | 0.0695 | 0.033* | 0.50 |
| H2B | 0.2346 | 0.2418 | 0.0983 | 0.033* | 0.50 |
| C3 | 0.426 (2) | 0.2566 (10) | 0.2083 (7) | 0.015 (3) | 0.50 |
| H3A | 0.3314 | 0.3100 | 0.1940 | 0.018* | 0.50 |
| H3B | 0.5590 | 0.2764 | 0.1913 | 0.018* | 0.50 |
| C4 | 0.5509 (7) | 0.0924 (4) | 0.1699 (3) | 0.0284 (10) | 0.50 |
| H4A | 0.6661 | 0.1361 | 0.1593 | 0.034* | 0.50 |
| H4B | 0.5351 | 0.0440 | 0.1304 | 0.034* | 0.50 |
| C5 | 0.5907 (6) | 0.0330 (3) | 0.2389 (5) | 0.022 (2) | 0.50 |
| O3' | −0.0529 (6) | 0.2069 (2) | 0.22572 (19) | 0.0298 (9) | 0.50 |
| O4' | −0.1173 (4) | 0.3735 (2) | 0.2400 (8) | 0.027 (2) | 0.50 |
| N1' | 0.2516 (6) | 0.2061 (3) | 0.3261 (2) | 0.0230 (8) | 0.50 |
| C2' | 0.274 (4) | 0.1684 (15) | 0.3997 (5) | 0.033 (5) | 0.50 |
| H2'1 | 0.4130 | 0.1465 | 0.4061 | 0.040* | 0.50 |
| H2'2 | 0.2509 | 0.2259 | 0.4322 | 0.040* | 0.50 |
| C3' | 0.429 (2) | 0.2477 (13) | 0.2885 (9) | 0.039 (6) | 0.50 |
| H3'1 | 0.5432 | 0.2049 | 0.3015 | 0.047* | 0.50 |
| H3'2 | 0.4544 | 0.3162 | 0.3078 | 0.047* | 0.50 |
| C4' | 0.0925 (7) | 0.2865 (4) | 0.3286 (3) | 0.0279 (11) | 0.50 |
| H4'1 | 0.1551 | 0.3535 | 0.3359 | 0.033* | 0.50 |
| H4'2 | 0.0049 | 0.2731 | 0.3694 | 0.033* | 0.50 |
| C5' | −0.0331 (6) | 0.2898 (3) | 0.2608 (5) | 0.0240 (19) | 0.50 |
Atomic displacement parameters (Å2) top
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Dy1 | 0.01006 (11) | 0.01040 (10) | 0.03376 (12) | −0.00049 (4) | 0.000 | 0.000 |
| O1 | 0.0714 (17) | 0.0513 (14) | 0.0395 (12) | −0.0385 (13) | −0.0086 (11) | −0.0020 (10) |
| O2 | 0.089 (2) | 0.0727 (18) | 0.0382 (13) | −0.0347 (14) | −0.0185 (12) | −0.0018 (13) |
| O3O | 0.176 (7) | 0.184 (7) | 0.205 (6) | 0.055 (6) | −0.056 (6) | 0.042 (6) |
| O1W | 0.118 (8) | 0.109 (7) | 0.085 (6) | 0.051 (6) | 0.027 (6) | 0.014 (5) |
| C1 | 0.0443 (17) | 0.0365 (15) | 0.0358 (14) | −0.0062 (13) | −0.0085 (12) | −0.0046 (12) |
| O3 | 0.0142 (16) | 0.0209 (16) | 0.0454 (19) | −0.0004 (13) | 0.0003 (13) | 0.0086 (13) |
| O4 | 0.0123 (12) | 0.0225 (12) | 0.039 (7) | 0.0004 (10) | −0.0009 (18) | −0.0005 (19) |
| N1 | 0.021 (2) | 0.019 (2) | 0.0284 (19) | −0.0039 (16) | −0.0030 (14) | 0.0010 (16) |
| C2 | 0.023 (5) | 0.024 (4) | 0.035 (5) | −0.016 (4) | −0.008 (3) | −0.006 (3) |
| C3 | 0.021 (5) | 0.009 (4) | 0.016 (4) | −0.008 (3) | −0.004 (3) | 0.004 (3) |
| C4 | 0.020 (2) | 0.029 (2) | 0.037 (3) | 0.000 (2) | 0.006 (2) | −0.001 (2) |
| C5 | 0.0141 (19) | 0.0139 (15) | 0.039 (6) | −0.0026 (12) | 0.000 (2) | −0.003 (2) |
| O3' | 0.0194 (14) | 0.0153 (15) | 0.055 (2) | 0.0032 (12) | −0.0113 (14) | −0.0050 (12) |
| O4' | 0.0225 (14) | 0.0111 (12) | 0.048 (7) | 0.0018 (9) | −0.0040 (18) | −0.0006 (19) |
| N1' | 0.021 (2) | 0.0184 (18) | 0.0290 (19) | −0.0022 (17) | 0.0016 (16) | 0.0023 (15) |
| C2' | 0.034 (8) | 0.039 (7) | 0.027 (5) | −0.010 (5) | 0.004 (3) | −0.007 (4) |
| C3' | 0.032 (7) | 0.033 (7) | 0.051 (8) | −0.012 (5) | −0.006 (5) | −0.002 (5) |
| C4' | 0.028 (3) | 0.018 (2) | 0.037 (3) | 0.0006 (17) | 0.0060 (19) | −0.005 (2) |
| C5' | 0.0150 (16) | 0.0134 (16) | 0.044 (6) | −0.0012 (13) | 0.004 (2) | −0.002 (2) |
Geometric parameters (Å, º) top
| Dy1—O1 | 2.331 (2) | C3—H3A | 0.9700 |
| Dy1—O1i | 2.331 (2) | C3—H3B | 0.9700 |
| Dy1—O3 | 2.324 (3) | C4—C5 | 1.516 (7) |
| Dy1—O4ii | 2.339 (3) | C4—H4A | 0.9700 |
| Dy1—O3' | 2.313 (3) | C4—H4B | 0.9700 |
| Dy1—O4'iii | 2.318 (3) | O3'—C5' | 1.260 (6) |
| Dy1—N1 | 2.592 (4) | O4'—C5' | 1.276 (6) |
| Dy1—N1' | 2.617 (4) | O4'—Dy1iv | 2.318 (3) |
| O1—C1 | 1.235 (4) | N1'—C2' | 1.457 (9) |
| O2—C1 | 1.265 (4) | N1'—C3' | 1.466 (9) |
| C1—C2'i | 1.41 (2) | N1'—C4' | 1.481 (5) |
| C1—C2 | 1.59 (2) | C2'—C1i | 1.41 (2) |
| O3—C5 | 1.257 (6) | C2'—H2'1 | 0.9700 |
| O4—C5 | 1.279 (6) | C2'—H2'2 | 0.9700 |
| N1—C2 | 1.451 (9) | C3'—H3'1 | 0.9700 |
| N1—C3 | 1.471 (8) | C3'—H3'2 | 0.9700 |
| N1—C4 | 1.481 (5) | C4'—C5' | 1.509 (8) |
| C2—H2A | 0.9700 | C4'—H4'1 | 0.9700 |
| C2—H2B | 0.9700 | C4'—H4'2 | 0.9700 |
| C3—C3' | 1.493 (7) | ||
| O3'i—Dy1—O3' | 22.46 (17) | C1—O1—Dy1 | 125.4 (2) |
| O3'i—Dy1—O4'v | 149.0 (2) | O1—C1—O2 | 123.2 (3) |
| O3'—Dy1—O4'v | 152.68 (14) | O1—C1—C2'i | 119.2 (5) |
| O3'i—Dy1—O4'iii | 152.68 (14) | O2—C1—C2'i | 117.5 (6) |
| O3'—Dy1—O4'iii | 149.0 (2) | O1—C1—C2 | 119.9 (5) |
| O4'v—Dy1—O4'iii | 9.2 (7) | O2—C1—C2 | 116.8 (5) |
| O3'i—Dy1—O3 | 127.66 (13) | C2'i—C1—C2 | 3.2 (14) |
| O3'—Dy1—O3 | 133.86 (12) | C5—O3—Dy1 | 124.6 (3) |
| O4'v—Dy1—O3 | 73.36 (12) | C5—O4—Dy1vii | 143.1 (6) |
| O4'iii—Dy1—O3 | 75.36 (14) | C2—N1—C3 | 109.7 (10) |
| O3'i—Dy1—O3i | 133.86 (12) | C2—N1—C4 | 106.0 (8) |
| O3'—Dy1—O3i | 127.66 (13) | C3—N1—C4 | 107.8 (6) |
| O4'v—Dy1—O3i | 75.36 (14) | C2—N1—Dy1 | 112.4 (10) |
| O4'iii—Dy1—O3i | 73.36 (12) | C3—N1—Dy1 | 114.1 (7) |
| O3—Dy1—O3i | 24.29 (17) | C4—N1—Dy1 | 106.3 (3) |
| O3'i—Dy1—O1i | 81.42 (11) | N1—C2—C1 | 109.3 (13) |
| O3'—Dy1—O1i | 103.60 (12) | N1—C2—H2A | 109.8 |
| O4'v—Dy1—O1i | 79.1 (3) | C1—C2—H2A | 109.8 |
| O4'iii—Dy1—O1i | 88.2 (3) | N1—C2—H2B | 109.8 |
| O3—Dy1—O1i | 82.89 (11) | C1—C2—H2B | 109.8 |
| O3i—Dy1—O1i | 106.94 (12) | H2A—C2—H2B | 108.3 |
| O3'i—Dy1—O1 | 103.60 (12) | N1—C3—C3' | 110.6 (15) |
| O3'—Dy1—O1 | 81.42 (11) | N1—C3—H3A | 109.5 |
| O4'v—Dy1—O1 | 88.2 (4) | C3'—C3—H3A | 109.5 |
| O4'iii—Dy1—O1 | 79.1 (3) | N1—C3—H3B | 109.5 |
| O3—Dy1—O1 | 106.94 (12) | C3'—C3—H3B | 109.5 |
| O3i—Dy1—O1 | 82.89 (11) | H3A—C3—H3B | 108.1 |
| O1i—Dy1—O1 | 161.18 (12) | N1—C4—C5 | 112.0 (4) |
| O3'i—Dy1—O4vi | 77.44 (14) | N1—C4—H4A | 109.2 |
| O3'—Dy1—O4vi | 75.74 (14) | C5—C4—H4A | 109.2 |
| O4'v—Dy1—O4vi | 77.36 (11) | N1—C4—H4B | 109.2 |
| O4'iii—Dy1—O4vi | 76.67 (10) | C5—C4—H4B | 109.2 |
| O3—Dy1—O4vi | 150.15 (16) | H4A—C4—H4B | 107.9 |
| O3i—Dy1—O4vi | 146.7 (2) | O3—C5—O4 | 119.6 (7) |
| O1i—Dy1—O4vi | 86.0 (4) | O3—C5—C4 | 117.5 (4) |
| O1—Dy1—O4vi | 77.6 (4) | O4—C5—C4 | 122.9 (7) |
| O3'i—Dy1—O4ii | 75.74 (14) | C5'—O3'—Dy1 | 125.9 (3) |
| O3'—Dy1—O4ii | 77.44 (14) | C5'—O4'—Dy1iv | 144.0 (6) |
| O4'v—Dy1—O4ii | 76.67 (10) | C2'—N1'—C3' | 119.1 (13) |
| O4'iii—Dy1—O4ii | 77.36 (11) | C2'—N1'—C4' | 106.2 (8) |
| O3—Dy1—O4ii | 146.7 (2) | C3'—N1'—C4' | 109.1 (8) |
| O3i—Dy1—O4ii | 150.15 (16) | C2'—N1'—Dy1 | 106.7 (9) |
| O1i—Dy1—O4ii | 77.6 (4) | C3'—N1'—Dy1 | 108.1 (8) |
| O1—Dy1—O4ii | 86.0 (4) | C4'—N1'—Dy1 | 107.0 (3) |
| O4vi—Dy1—O4ii | 8.5 (7) | C1i—C2'—N1' | 116.9 (15) |
| O3'i—Dy1—N1i | 75.41 (13) | C1i—C2'—H2'1 | 108.1 |
| O3'—Dy1—N1i | 87.50 (12) | N1'—C2'—H2'1 | 108.1 |
| O4'v—Dy1—N1i | 117.7 (2) | C1i—C2'—H2'2 | 108.1 |
| O4'iii—Dy1—N1i | 123.4 (2) | N1'—C2'—H2'2 | 108.1 |
| O3—Dy1—N1i | 52.53 (12) | H2'1—C2'—H2'2 | 107.3 |
| O3i—Dy1—N1i | 67.47 (12) | N1'—C3'—C3 | 119.6 (17) |
| O1i—Dy1—N1i | 67.02 (10) | N1'—C3'—H3'1 | 107.4 |
| O1—Dy1—N1i | 131.72 (11) | C3—C3'—H3'1 | 107.4 |
| O4vi—Dy1—N1i | 144.0 (3) | N1'—C3'—H3'2 | 107.4 |
| O4ii—Dy1—N1i | 136.9 (3) | C3—C3'—H3'2 | 107.4 |
| O3'i—Dy1—N1 | 87.50 (12) | H3'1—C3'—H3'2 | 107.0 |
| O3'—Dy1—N1 | 75.41 (13) | N1'—C4'—C5' | 112.8 (4) |
| O4'v—Dy1—N1 | 123.4 (2) | N1'—C4'—H4'1 | 109.0 |
| O4'iii—Dy1—N1 | 117.7 (2) | C5'—C4'—H4'1 | 109.0 |
| O3—Dy1—N1 | 67.47 (12) | N1'—C4'—H4'2 | 109.0 |
| O3i—Dy1—N1 | 52.53 (13) | C5'—C4'—H4'2 | 109.0 |
| O1i—Dy1—N1 | 131.72 (11) | H4'1—C4'—H4'2 | 107.8 |
| O1—Dy1—N1 | 67.02 (10) | O3'—C5'—O4' | 121.2 (8) |
| O4vi—Dy1—N1 | 136.9 (3) | O3'—C5'—C4' | 117.6 (4) |
| O4ii—Dy1—N1 | 144.0 (3) | O4'—C5'—C4' | 121.2 (7) |
| N1i—Dy1—N1 | 64.71 (17) | ||
| O3'i—Dy1—O1—C1 | 68.6 (3) | Dy1—O3—C5—O4 | 177.9 (5) |
| O3'—Dy1—O1—C1 | 65.0 (3) | Dy1—O3—C5—C4 | −2.9 (7) |
| O4'v—Dy1—O1—C1 | −140.4 (3) | Dy1vii—O4—C5—O3 | −155.4 (11) |
| O4'iii—Dy1—O1—C1 | −139.3 (3) | Dy1vii—O4—C5—C4 | 25.5 (17) |
| O3—Dy1—O1—C1 | −68.4 (3) | N1—C4—C5—O3 | 30.2 (7) |
| O3i—Dy1—O1—C1 | −64.9 (3) | N1—C4—C5—O4 | −150.7 (6) |
| O1i—Dy1—O1—C1 | 172.1 (3) | O3'i—Dy1—O3'—C5' | 37.5 (5) |
| O4vi—Dy1—O1—C1 | 142.1 (3) | O4'v—Dy1—O3'—C5' | 139.4 (8) |
| O4ii—Dy1—O1—C1 | 142.8 (3) | O4'iii—Dy1—O3'—C5' | 156.8 (7) |
| N1i—Dy1—O1—C1 | −13.9 (4) | O3—Dy1—O3'—C5' | −46.4 (5) |
| N1—Dy1—O1—C1 | −12.7 (3) | O3i—Dy1—O3'—C5' | −77.6 (5) |
| Dy1—O1—C1—O2 | −177.9 (3) | O1i—Dy1—O3'—C5' | 46.8 (5) |
| Dy1—O1—C1—C2'i | −0.6 (10) | O1—Dy1—O3'—C5' | −151.7 (5) |
| Dy1—O1—C1—C2 | 2.9 (9) | O4vi—Dy1—O3'—C5' | 129.1 (6) |
| O3'i—Dy1—O3—C5 | −81.4 (5) | O4ii—Dy1—O3'—C5' | 120.5 (6) |
| O3'—Dy1—O3—C5 | −52.7 (5) | N1i—Dy1—O3'—C5' | −18.8 (5) |
| O4'v—Dy1—O3—C5 | 124.5 (6) | N1—Dy1—O3'—C5' | −83.3 (5) |
| O4'iii—Dy1—O3—C5 | 115.2 (6) | O3'i—Dy1—N1'—C2' | 115.0 (9) |
| O3i—Dy1—O3—C5 | 33.3 (4) | O3'—Dy1—N1'—C2' | 135.5 (9) |
| O1i—Dy1—O3—C5 | −154.8 (5) | O4'v—Dy1—N1'—C2' | −25.2 (10) |
| O1—Dy1—O3—C5 | 41.6 (5) | O4'iii—Dy1—N1'—C2' | −33.2 (10) |
| O4vi—Dy1—O3—C5 | 136.2 (8) | O3—Dy1—N1'—C2' | −71.1 (9) |
| O4ii—Dy1—O3—C5 | 151.1 (7) | O3i—Dy1—N1'—C2' | −91.7 (9) |
| N1i—Dy1—O3—C5 | −88.4 (5) | O1i—Dy1—N1'—C2' | 17.9 (9) |
| N1—Dy1—O3—C5 | −13.7 (4) | O1—Dy1—N1'—C2' | −170.2 (9) |
| O3'i—Dy1—N1—C2 | −85.2 (7) | O4vi—Dy1—N1'—C2' | 84.0 (10) |
| O3'—Dy1—N1—C2 | −66.1 (7) | O4ii—Dy1—N1'—C2' | 76.2 (10) |
| O4'v—Dy1—N1—C2 | 92.0 (8) | N1i—Dy1—N1'—C2' | −69.4 (10) |
| O4'iii—Dy1—N1—C2 | 83.7 (8) | N1—Dy1—N1'—C2' | −142.3 (9) |
| O3—Dy1—N1—C2 | 141.9 (8) | O3'i—Dy1—N1'—C3' | −115.7 (8) |
| O3i—Dy1—N1—C2 | 119.6 (8) | O3'—Dy1—N1'—C3' | −95.3 (8) |
| O1i—Dy1—N1—C2 | −161.4 (7) | O4'v—Dy1—N1'—C3' | 104.1 (9) |
| O1—Dy1—N1—C2 | 20.7 (7) | O4'iii—Dy1—N1'—C3' | 96.0 (9) |
| O4vi—Dy1—N1—C2 | −16.7 (8) | O3—Dy1—N1'—C3' | 58.2 (8) |
| O4ii—Dy1—N1—C2 | −23.9 (9) | O3i—Dy1—N1'—C3' | 37.5 (8) |
| N1i—Dy1—N1—C2 | −160.3 (7) | O1i—Dy1—N1'—C3' | 147.2 (8) |
| O3'i—Dy1—N1—C3 | 40.5 (6) | O1—Dy1—N1'—C3' | −40.9 (8) |
| O3'—Dy1—N1—C3 | 59.7 (6) | O4vi—Dy1—N1'—C3' | −146.8 (9) |
| O4'v—Dy1—N1—C3 | −142.2 (7) | O4ii—Dy1—N1'—C3' | −154.5 (9) |
| O4'iii—Dy1—N1—C3 | −150.6 (6) | N1i—Dy1—N1'—C3' | 59.9 (9) |
| O3—Dy1—N1—C3 | −92.3 (6) | N1—Dy1—N1'—C3' | −13.1 (8) |
| O3i—Dy1—N1—C3 | −114.6 (6) | O3'i—Dy1—N1'—C4' | 1.7 (3) |
| O1i—Dy1—N1—C3 | −35.7 (6) | O3'—Dy1—N1'—C4' | 22.1 (3) |
| O1—Dy1—N1—C3 | 146.4 (6) | O4'v—Dy1—N1'—C4' | −138.5 (4) |
| O4vi—Dy1—N1—C3 | 109.1 (7) | O4'iii—Dy1—N1'—C4' | −146.6 (4) |
| O4ii—Dy1—N1—C3 | 101.8 (7) | O3—Dy1—N1'—C4' | 175.6 (3) |
| N1i—Dy1—N1—C3 | −34.5 (6) | O3i—Dy1—N1'—C4' | 154.9 (3) |
| O3'i—Dy1—N1—C4 | 159.2 (3) | O1i—Dy1—N1'—C4' | −95.4 (3) |
| O3'—Dy1—N1—C4 | 178.3 (3) | O1—Dy1—N1'—C4' | 76.5 (3) |
| O4'v—Dy1—N1—C4 | −23.6 (5) | O4vi—Dy1—N1'—C4' | −29.3 (5) |
| O4'iii—Dy1—N1—C4 | −31.9 (4) | O4ii—Dy1—N1'—C4' | −37.1 (4) |
| O3—Dy1—N1—C4 | 26.3 (3) | N1i—Dy1—N1'—C4' | 177.3 (5) |
| O3i—Dy1—N1—C4 | 4.0 (3) | N1—Dy1—N1'—C4' | 104.3 (3) |
| O1i—Dy1—N1—C4 | 83.0 (3) | C3'—N1'—C2'—C1i | −148.5 (13) |
| O1—Dy1—N1—C4 | −94.9 (3) | C4'—N1'—C2'—C1i | 88.0 (12) |
| O4vi—Dy1—N1—C4 | −132.3 (4) | Dy1—N1'—C2'—C1i | −25.8 (15) |
| O4ii—Dy1—N1—C4 | −139.5 (5) | C2'—N1'—C3'—C3 | 161.5 (16) |
| N1i—Dy1—N1—C4 | 84.1 (3) | C4'—N1'—C3'—C3 | −76.4 (19) |
| C3—N1—C2—C1 | −153.6 (9) | Dy1—N1'—C3'—C3 | 40 (2) |
| C4—N1—C2—C1 | 90.2 (11) | N1—C3—C3'—N1' | −52 (2) |
| Dy1—N1—C2—C1 | −25.5 (12) | C2'—N1'—C4'—C5' | −146.6 (11) |
| O1—C1—C2—N1 | 17.1 (14) | C3'—N1'—C4'—C5' | 83.9 (9) |
| O2—C1—C2—N1 | −162.1 (8) | Dy1—N1'—C4'—C5' | −32.9 (5) |
| C2'i—C1—C2—N1 | 94 (17) | Dy1—O3'—C5'—O4' | 174.7 (5) |
| C2—N1—C3—C3' | 161.0 (16) | Dy1—O3'—C5'—C4' | −5.8 (8) |
| C4—N1—C3—C3' | −84.0 (15) | Dy1iv—O4'—C5'—O3' | −159.8 (10) |
| Dy1—N1—C3—C3' | 33.8 (16) | Dy1iv—O4'—C5'—C4' | 20.7 (16) |
| C2—N1—C4—C5 | −157.2 (11) | N1'—C4'—C5'—O3' | 28.6 (7) |
| C3—N1—C4—C5 | 85.4 (8) | N1'—C4'—C5'—O4' | −151.9 (6) |
| Dy1—N1—C4—C5 | −37.3 (5) |
| Symmetry codes: (i) x, y, −z+1/2; (ii) x−1, y, z; (iii) −x, y−1/2, z; (iv) −x, y+1/2, z; (v) −x, y−1/2, −z+1/2; (vi) x−1, y, −z+1/2; (vii) x+1, y, z. |
Experimental details
| Crystal data | |
| Chemical formula | (H3O)[Dy(C10H12N2O8)]·H2O |
| Mr | 487.76 |
| Crystal system, space group | Orthorhombic, Pbcm |
| Temperature (K) | 295 |
| a, b, c (Å) | 6.6271 (3), 12.9233 (6), 18.5496 (9) |
| V (Å3) | 1588.6 (1) |
| Z | 4 |
| Radiation type | Mo Kα |
| µ (mm−1) | 4.76 |
| Crystal size (mm) | 0.30 × 0.20 × 0.10 |
| Data collection | |
| Diffractometer | Bruker APEX II CCD |
| Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
| Tmin, Tmax | 0.425, 0.648 |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 13726, 1873, 1784 |
| Rint | 0.022 |
| (sin θ/λ)max (Å−1) | 0.650 |
| Refinement | |
| R[F2 > 2σ(F2)], wR(F2), S | 0.017, 0.050, 1.05 |
| No. of reflections | 1873 |
| No. of parameters | 178 |
| No. of restraints | 127 |
| H-atom treatment | H-atom parameters constrained |
| Δρmax, Δρmin (e Å−3) | 0.66, −0.47 |
Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).
Selected bond lengths (Å) top
| Dy1—O1 | 2.331 (2) | Dy1—O3' | 2.313 (3) |
| Dy1—O1i | 2.331 (2) | Dy1—O4'iii | 2.318 (3) |
| Dy1—O3 | 2.324 (3) | Dy1—N1 | 2.592 (4) |
| Dy1—O4ii | 2.339 (3) | Dy1—N1' | 2.617 (4) |
| Symmetry codes: (i) x, y, −z+1/2; (ii) x−1, y, z; (iii) −x, y−1/2, z. |
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The erbium(III) and holonium(III) derivatives of edta have recently been reported (You et al., 2007a, b). The dysprosium analog described here is isostructural.