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
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).
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).
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).
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)[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 |
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 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 |
(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 |
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 |
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 |
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 |
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) |
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).
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. |
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.