Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807058771/lh2562sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807058771/lh2562Isup2.hkl |
CCDC reference: 672732
The title complex was prepared according to the literature method (Xu et al., 2004). When Cd(C2H3O2)2·2H2O(0.013 g, 0.05 mmol) was added to a stirred solution (pH = 9,containing NaOH) of H2L (0.018 g, 0.05 mmol) in H2O(15 ml), a white precipitate formed immediately. After the pH of the solution was adjusted to 4–5 using dilute HCl, the resulting precipitete was filtered off and dried. Crystals were obtanined by slow evaporation (two weeks) of a methanol solution(15 ml) of the complex (1) (0.047 g,0.1 mmol).
H atoms bonded to C atom were located at the geometrical positions with C—H =0.93 Å (aromatic), 0.97 Å (methylene) and Uiso(H) = 1.2Ueq(aromatic and methylene C). H atoms bonded to water O atoms were contrained at their indicative positions by using 'CALC-OH' programme in WinGX 2003 (Farrugia, 1999) and the Uiso(H) value were set 1.5 times of their carrier atoms. However, the calculated positions while sensible cause some H atoms, e.g. H12D, H17A, H18A, H18B and H32A, to be involved in fairly close intermolecular contacts.
Data collection: SMART (Bruker, 2000); cell refinement: SAINT-Plus (Bruker, 2000); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997), WinGX2003 (Farrugia, 1999); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: PLATON.
[Cd(C20H22N2O4)(H2O)2]·2.5H2O | F(000) = 2248 |
Mr = 547.87 | Dx = 1.511 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 5870 reflections |
a = 13.9704 (16) Å | θ = 2.2–23.7° |
b = 9.4600 (11) Å | µ = 0.95 mm−1 |
c = 36.471 (3) Å | T = 294 K |
β = 92.273 (2)° | Block, colorless |
V = 4816.2 (9) Å3 | 0.30 × 0.20 × 0.20 mm |
Z = 8 |
Bruker SMART-CCD diffractometer | 9436 independent reflections |
Radiation source: fine-focus sealed tube | 7654 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.075 |
ϕ and ω scans | θmax = 26.0°, θmin = 1.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2001) | h = −16→17 |
Tmin = 0.763, Tmax = 0.832 | k = −11→11 |
49413 measured reflections | l = −44→43 |
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)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.123 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0654P)2] where P = (Fo2 + 2Fc2)/3 |
9436 reflections | (Δ/σ)max = 0.001 |
568 parameters | Δρmax = 0.70 e Å−3 |
0 restraints | Δρmin = −0.85 e Å−3 |
[Cd(C20H22N2O4)(H2O)2]·2.5H2O | V = 4816.2 (9) Å3 |
Mr = 547.87 | Z = 8 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.9704 (16) Å | µ = 0.95 mm−1 |
b = 9.4600 (11) Å | T = 294 K |
c = 36.471 (3) Å | 0.30 × 0.20 × 0.20 mm |
β = 92.273 (2)° |
Bruker SMART-CCD diffractometer | 9436 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2001) | 7654 reflections with I > 2σ(I) |
Tmin = 0.763, Tmax = 0.832 | Rint = 0.075 |
49413 measured reflections |
R[F2 > 2σ(F2)] = 0.050 | 0 restraints |
wR(F2) = 0.123 | H-atom parameters constrained |
S = 1.06 | Δρmax = 0.70 e Å−3 |
9436 reflections | Δρmin = −0.85 e Å−3 |
568 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Cd1 | 0.14816 (2) | 0.07448 (3) | 0.123273 (9) | 0.03309 (11) | |
Cd2 | 0.92890 (2) | 0.51568 (3) | 0.096232 (8) | 0.03220 (11) | |
C1 | 0.3374 (3) | 0.1193 (5) | 0.16963 (13) | 0.0399 (11) | |
H1A | 0.3235 | 0.2176 | 0.1748 | 0.048* | |
H1B | 0.4047 | 0.1031 | 0.1759 | 0.048* | |
C2 | 0.2773 (3) | 0.0261 (5) | 0.19337 (13) | 0.0399 (11) | |
H2A | 0.2892 | −0.0722 | 0.1875 | 0.048* | |
H2B | 0.2967 | 0.0407 | 0.2189 | 0.048* | |
C3 | 0.3710 (3) | −0.0346 (5) | 0.11676 (14) | 0.0395 (11) | |
H3A | 0.3466 | −0.0571 | 0.0922 | 0.047* | |
H3B | 0.3558 | −0.1135 | 0.1325 | 0.047* | |
C4 | 0.4789 (3) | −0.0217 (4) | 0.11599 (15) | 0.0428 (12) | |
C5 | 0.5373 (4) | −0.0648 (5) | 0.14582 (17) | 0.0604 (15) | |
H5 | 0.5105 | −0.1022 | 0.1666 | 0.073* | |
C6 | 0.6385 (5) | −0.0509 (7) | 0.1440 (2) | 0.083 (2) | |
H6 | 0.6780 | −0.0791 | 0.1638 | 0.099* | |
C7 | 0.6783 (4) | 0.0040 (7) | 0.1131 (3) | 0.082 (2) | |
H7 | 0.7444 | 0.0141 | 0.1121 | 0.098* | |
C8 | 0.6208 (4) | 0.0428 (6) | 0.0845 (2) | 0.074 (2) | |
H8 | 0.6481 | 0.0785 | 0.0636 | 0.088* | |
C9 | 0.5230 (4) | 0.0313 (5) | 0.08524 (17) | 0.0552 (14) | |
H9 | 0.4855 | 0.0594 | 0.0649 | 0.066* | |
C10 | 0.3432 (3) | 0.2185 (4) | 0.10856 (13) | 0.0399 (11) | |
H10A | 0.3483 | 0.1918 | 0.0830 | 0.048* | |
H10B | 0.4055 | 0.2528 | 0.1172 | 0.048* | |
C11 | 0.2706 (3) | 0.3398 (5) | 0.11076 (12) | 0.0386 (10) | |
C12 | 0.1427 (3) | 0.1846 (5) | 0.20828 (13) | 0.0425 (11) | |
H12A | 0.0867 | 0.2236 | 0.1953 | 0.051* | |
H12B | 0.1934 | 0.2544 | 0.2074 | 0.051* | |
C13 | 0.1190 (3) | 0.1623 (5) | 0.24803 (13) | 0.0434 (11) | |
C14 | 0.1891 (4) | 0.1407 (5) | 0.27534 (14) | 0.0545 (13) | |
H14 | 0.2532 | 0.1462 | 0.2696 | 0.065* | |
C15 | 0.1660 (5) | 0.1116 (6) | 0.31056 (17) | 0.0727 (18) | |
H15 | 0.2142 | 0.0974 | 0.3285 | 0.087* | |
C16 | 0.0723 (6) | 0.1034 (7) | 0.31944 (18) | 0.084 (2) | |
H16 | 0.0567 | 0.0827 | 0.3434 | 0.101* | |
C17 | 0.0019 (5) | 0.1252 (7) | 0.2935 (2) | 0.084 (2) | |
H17 | −0.0618 | 0.1196 | 0.2999 | 0.100* | |
C18 | 0.0238 (4) | 0.1562 (6) | 0.25756 (16) | 0.0658 (16) | |
H18 | −0.0249 | 0.1726 | 0.2400 | 0.079* | |
C19 | 0.1158 (3) | −0.0682 (4) | 0.19762 (12) | 0.0391 (10) | |
H19A | 0.0499 | −0.0383 | 0.1999 | 0.047* | |
H19B | 0.1384 | −0.1037 | 0.2214 | 0.047* | |
C20 | 0.1181 (3) | −0.1894 (4) | 0.16968 (12) | 0.0359 (10) | |
C21 | 0.7233 (3) | 0.5532 (4) | 0.12492 (12) | 0.0347 (10) | |
H21A | 0.7162 | 0.6526 | 0.1189 | 0.042* | |
H21B | 0.6731 | 0.5285 | 0.1414 | 0.042* | |
C22 | 0.7104 (3) | 0.4670 (4) | 0.09019 (12) | 0.0345 (10) | |
H22A | 0.7169 | 0.3676 | 0.0962 | 0.041* | |
H22B | 0.6462 | 0.4819 | 0.0798 | 0.041* | |
C23 | 0.8227 (3) | 0.3971 (4) | 0.16563 (13) | 0.0402 (11) | |
H23A | 0.8866 | 0.3896 | 0.1768 | 0.048* | |
H23B | 0.8143 | 0.3186 | 0.1487 | 0.048* | |
C24 | 0.7520 (3) | 0.3804 (5) | 0.19530 (12) | 0.0382 (10) | |
C25 | 0.6727 (4) | 0.2952 (5) | 0.18932 (15) | 0.0572 (14) | |
H25 | 0.6624 | 0.2515 | 0.1667 | 0.069* | |
C26 | 0.6077 (4) | 0.2739 (7) | 0.21691 (18) | 0.0701 (17) | |
H26 | 0.5549 | 0.2153 | 0.2128 | 0.084* | |
C27 | 0.6218 (4) | 0.3390 (7) | 0.24973 (16) | 0.0652 (16) | |
H27 | 0.5779 | 0.3258 | 0.2679 | 0.078* | |
C28 | 0.6994 (5) | 0.4238 (7) | 0.25645 (15) | 0.0663 (17) | |
H28 | 0.7089 | 0.4680 | 0.2791 | 0.080* | |
C29 | 0.7637 (4) | 0.4430 (6) | 0.22915 (14) | 0.0541 (13) | |
H29 | 0.8169 | 0.5004 | 0.2338 | 0.065* | |
C30 | 0.8477 (3) | 0.6557 (4) | 0.16554 (12) | 0.0362 (10) | |
H30A | 0.8977 | 0.6278 | 0.1833 | 0.043* | |
H30B | 0.7938 | 0.6897 | 0.1790 | 0.043* | |
C31 | 0.8850 (3) | 0.7769 (4) | 0.14203 (12) | 0.0330 (9) | |
C32 | 0.7600 (3) | 0.6413 (4) | 0.04399 (13) | 0.0378 (10) | |
H32A | 0.8104 | 0.6594 | 0.0270 | 0.045* | |
H32B | 0.7634 | 0.7151 | 0.0625 | 0.045* | |
C33 | 0.6642 (3) | 0.6535 (4) | 0.02302 (13) | 0.0394 (11) | |
C34 | 0.5872 (3) | 0.7167 (5) | 0.03930 (16) | 0.0562 (14) | |
H34 | 0.5933 | 0.7479 | 0.0635 | 0.067* | |
C35 | 0.5012 (4) | 0.7336 (6) | 0.0197 (2) | 0.0722 (18) | |
H35 | 0.4502 | 0.7778 | 0.0306 | 0.087* | |
C36 | 0.4905 (4) | 0.6864 (6) | −0.0153 (2) | 0.0695 (18) | |
H36 | 0.4320 | 0.6973 | −0.0280 | 0.083* | |
C37 | 0.5650 (4) | 0.6230 (6) | −0.03202 (15) | 0.0590 (15) | |
H37 | 0.5573 | 0.5908 | −0.0560 | 0.071* | |
C38 | 0.6524 (4) | 0.6072 (5) | −0.01280 (14) | 0.0494 (12) | |
H38 | 0.7034 | 0.5649 | −0.0242 | 0.059* | |
C39 | 0.7928 (3) | 0.3874 (4) | 0.03638 (12) | 0.0355 (10) | |
H39A | 0.8291 | 0.4212 | 0.0160 | 0.043* | |
H39B | 0.7304 | 0.3575 | 0.0267 | 0.043* | |
C40 | 0.8448 (3) | 0.2595 (4) | 0.05404 (12) | 0.0337 (10) | |
N1 | 0.3196 (2) | 0.0923 (3) | 0.12969 (10) | 0.0332 (8) | |
N2 | 0.1734 (2) | 0.0553 (3) | 0.18834 (10) | 0.0338 (8) | |
N3 | 0.8172 (2) | 0.5310 (3) | 0.14395 (10) | 0.0323 (8) | |
N4 | 0.7803 (2) | 0.5037 (3) | 0.06244 (10) | 0.0326 (8) | |
O1 | 0.1857 (2) | 0.3060 (3) | 0.11787 (9) | 0.0479 (8) | |
O2 | 0.2997 (2) | 0.4583 (3) | 0.10453 (10) | 0.0505 (9) | |
O3 | 0.1434 (2) | −0.1601 (3) | 0.13766 (8) | 0.0389 (7) | |
O4 | 0.0931 (2) | −0.3067 (3) | 0.18056 (9) | 0.0473 (8) | |
O5 | −0.0086 (2) | 0.1096 (3) | 0.13117 (8) | 0.0409 (7) | |
H5A | −0.0358 | 0.1668 | 0.1175 | 0.061* | |
H5B | −0.0472 | 0.0522 | 0.1388 | 0.061* | |
O6 | 0.1234 (2) | 0.0431 (3) | 0.06219 (8) | 0.0467 (8) | |
H6A | 0.1720 | 0.0060 | 0.0545 | 0.070* | |
H6B | 0.0814 | 0.0475 | 0.0459 | 0.070* | |
O7 | 0.9119 (2) | 0.7488 (3) | 0.11012 (8) | 0.0393 (7) | |
O8 | 0.8889 (2) | 0.8951 (3) | 0.15652 (9) | 0.0440 (8) | |
O9 | 0.8997 (2) | 0.2819 (3) | 0.08162 (8) | 0.0377 (7) | |
O10 | 0.8308 (2) | 0.1429 (3) | 0.03897 (9) | 0.0455 (8) | |
O11 | 1.0454 (2) | 0.4736 (3) | 0.13859 (8) | 0.0409 (7) | |
H11A | 1.0896 | 0.4215 | 0.1326 | 0.061* | |
H11B | 1.0675 | 0.5445 | 0.1490 | 0.061* | |
O12 | 1.0267 (2) | 0.5476 (4) | 0.04948 (9) | 0.0505 (8) | |
H12C | 0.9959 | 0.5922 | 0.0338 | 0.076* | |
H12D | 1.0535 | 0.4824 | 0.0392 | 0.076* | |
O13 | 0.9549 (2) | 0.9130 (3) | 0.04959 (9) | 0.0491 (8) | |
H13A | 0.9154 | 0.9745 | 0.0440 | 0.074* | |
H13B | 0.9410 | 0.8746 | 0.0689 | 0.074* | |
O14 | 0.2542 (2) | 0.8830 (4) | 0.03073 (9) | 0.0566 (9) | |
H14A | 0.2619 | 0.8041 | 0.0397 | 0.085* | |
H14B | 0.2466 | 0.8736 | 0.0085 | 0.085* | |
O15 | 0.1875 (2) | 0.6709 (3) | 0.07808 (9) | 0.0483 (8) | |
H15A | 0.2135 | 0.6036 | 0.0886 | 0.072* | |
H15B | 0.1561 | 0.7131 | 0.0931 | 0.072* | |
O17 | 0.4568 (8) | 0.0413 (13) | 0.2579 (3) | 0.271 (6) | |
H17A | 0.5273 | 0.0413 | 0.2579 | 0.406* | |
H17B | 0.4361 | 0.0413 | 0.2833 | 0.406* | |
O18 | 0.0625 (3) | 0.2882 (4) | 0.01765 (10) | 0.0739 (12) | |
H18A | 0.1329 | 0.2881 | 0.0176 | 0.111* | |
H18B | 0.0417 | 0.2881 | 0.0431 | 0.111* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.03149 (18) | 0.03535 (18) | 0.0322 (2) | 0.00266 (12) | −0.00139 (13) | −0.00107 (13) |
Cd2 | 0.02739 (17) | 0.03698 (18) | 0.0323 (2) | 0.00211 (12) | 0.00186 (13) | −0.00149 (13) |
C1 | 0.034 (2) | 0.034 (2) | 0.051 (3) | −0.0021 (18) | −0.004 (2) | −0.006 (2) |
C2 | 0.046 (3) | 0.038 (2) | 0.035 (3) | 0.003 (2) | −0.007 (2) | −0.002 (2) |
C3 | 0.033 (2) | 0.035 (2) | 0.051 (3) | 0.0056 (18) | 0.001 (2) | −0.004 (2) |
C4 | 0.035 (2) | 0.027 (2) | 0.066 (4) | 0.0105 (18) | −0.007 (2) | −0.008 (2) |
C5 | 0.052 (3) | 0.048 (3) | 0.080 (4) | 0.017 (2) | −0.011 (3) | −0.002 (3) |
C6 | 0.061 (4) | 0.060 (4) | 0.123 (7) | 0.027 (3) | −0.042 (4) | −0.025 (4) |
C7 | 0.041 (3) | 0.054 (4) | 0.150 (8) | 0.007 (3) | 0.000 (4) | −0.020 (4) |
C8 | 0.049 (3) | 0.049 (3) | 0.125 (6) | 0.007 (3) | 0.031 (4) | −0.001 (4) |
C9 | 0.046 (3) | 0.046 (3) | 0.075 (4) | 0.013 (2) | 0.010 (3) | 0.000 (3) |
C10 | 0.035 (2) | 0.032 (2) | 0.053 (3) | 0.0050 (18) | 0.007 (2) | 0.005 (2) |
C11 | 0.040 (3) | 0.037 (2) | 0.039 (3) | 0.004 (2) | −0.001 (2) | −0.003 (2) |
C12 | 0.045 (3) | 0.037 (2) | 0.046 (3) | 0.005 (2) | 0.001 (2) | −0.009 (2) |
C13 | 0.051 (3) | 0.038 (2) | 0.041 (3) | −0.005 (2) | 0.006 (2) | −0.014 (2) |
C14 | 0.073 (4) | 0.054 (3) | 0.036 (3) | −0.013 (3) | 0.004 (3) | −0.011 (2) |
C15 | 0.109 (5) | 0.060 (4) | 0.049 (4) | −0.019 (4) | −0.001 (4) | −0.013 (3) |
C16 | 0.124 (6) | 0.084 (5) | 0.046 (4) | −0.041 (4) | 0.021 (4) | −0.019 (3) |
C17 | 0.079 (4) | 0.100 (5) | 0.074 (5) | −0.027 (4) | 0.039 (4) | −0.036 (4) |
C18 | 0.066 (4) | 0.081 (4) | 0.051 (4) | −0.004 (3) | 0.008 (3) | −0.030 (3) |
C19 | 0.048 (3) | 0.035 (2) | 0.034 (3) | −0.0018 (19) | 0.002 (2) | −0.0057 (19) |
C20 | 0.034 (2) | 0.036 (2) | 0.037 (3) | 0.0086 (18) | −0.007 (2) | −0.004 (2) |
C21 | 0.032 (2) | 0.036 (2) | 0.037 (3) | 0.0044 (18) | 0.0097 (19) | 0.0029 (19) |
C22 | 0.027 (2) | 0.034 (2) | 0.043 (3) | −0.0012 (17) | 0.0058 (19) | 0.002 (2) |
C23 | 0.047 (3) | 0.033 (2) | 0.041 (3) | 0.0050 (19) | 0.006 (2) | 0.004 (2) |
C24 | 0.048 (3) | 0.037 (2) | 0.029 (3) | 0.002 (2) | 0.002 (2) | 0.008 (2) |
C25 | 0.075 (4) | 0.052 (3) | 0.045 (3) | −0.020 (3) | 0.008 (3) | 0.004 (3) |
C26 | 0.060 (4) | 0.076 (4) | 0.076 (5) | −0.017 (3) | 0.015 (3) | 0.021 (4) |
C27 | 0.068 (4) | 0.080 (4) | 0.050 (4) | 0.018 (3) | 0.025 (3) | 0.025 (3) |
C28 | 0.089 (5) | 0.078 (4) | 0.032 (3) | 0.015 (4) | 0.011 (3) | 0.016 (3) |
C29 | 0.065 (3) | 0.061 (3) | 0.036 (3) | −0.007 (3) | 0.001 (3) | 0.010 (3) |
C30 | 0.041 (2) | 0.038 (2) | 0.030 (2) | 0.0013 (19) | 0.0041 (19) | 0.0007 (19) |
C31 | 0.027 (2) | 0.035 (2) | 0.037 (3) | 0.0012 (17) | 0.0014 (19) | 0.005 (2) |
C32 | 0.037 (2) | 0.035 (2) | 0.041 (3) | −0.0020 (18) | 0.000 (2) | 0.007 (2) |
C33 | 0.036 (2) | 0.034 (2) | 0.048 (3) | 0.0012 (18) | −0.005 (2) | 0.012 (2) |
C34 | 0.051 (3) | 0.048 (3) | 0.069 (4) | 0.012 (2) | −0.008 (3) | −0.005 (3) |
C35 | 0.044 (3) | 0.062 (4) | 0.110 (6) | 0.017 (3) | −0.007 (3) | 0.008 (4) |
C36 | 0.049 (3) | 0.064 (4) | 0.092 (5) | −0.009 (3) | −0.028 (3) | 0.032 (4) |
C37 | 0.058 (3) | 0.066 (3) | 0.052 (3) | −0.016 (3) | −0.019 (3) | 0.021 (3) |
C38 | 0.052 (3) | 0.053 (3) | 0.043 (3) | −0.003 (2) | −0.002 (2) | 0.014 (2) |
C39 | 0.033 (2) | 0.039 (2) | 0.035 (3) | 0.0023 (18) | 0.0026 (19) | 0.001 (2) |
C40 | 0.029 (2) | 0.037 (2) | 0.035 (3) | 0.0016 (18) | 0.0046 (19) | 0.001 (2) |
N1 | 0.0298 (18) | 0.0297 (18) | 0.040 (2) | 0.0057 (14) | 0.0031 (16) | 0.0033 (16) |
N2 | 0.039 (2) | 0.0314 (18) | 0.031 (2) | −0.0004 (15) | 0.0013 (16) | −0.0031 (15) |
N3 | 0.0331 (19) | 0.0297 (17) | 0.034 (2) | 0.0001 (14) | 0.0045 (16) | 0.0036 (16) |
N4 | 0.0302 (18) | 0.0365 (19) | 0.031 (2) | 0.0048 (14) | 0.0012 (16) | 0.0024 (16) |
O1 | 0.0391 (17) | 0.0316 (16) | 0.073 (2) | 0.0073 (14) | 0.0055 (16) | −0.0013 (16) |
O2 | 0.053 (2) | 0.0289 (16) | 0.071 (3) | 0.0011 (14) | 0.0105 (18) | 0.0000 (16) |
O3 | 0.0528 (19) | 0.0358 (16) | 0.0282 (17) | 0.0025 (14) | 0.0024 (14) | −0.0035 (14) |
O4 | 0.063 (2) | 0.0323 (17) | 0.046 (2) | −0.0073 (15) | −0.0024 (16) | 0.0007 (15) |
O5 | 0.0328 (16) | 0.0400 (16) | 0.050 (2) | 0.0018 (13) | 0.0012 (14) | 0.0115 (15) |
O6 | 0.053 (2) | 0.0544 (19) | 0.0327 (19) | 0.0056 (16) | −0.0027 (15) | −0.0052 (15) |
O7 | 0.0449 (17) | 0.0385 (16) | 0.0348 (18) | −0.0021 (14) | 0.0061 (14) | 0.0048 (14) |
O8 | 0.0524 (19) | 0.0312 (16) | 0.049 (2) | −0.0008 (14) | 0.0080 (16) | −0.0058 (15) |
O9 | 0.0386 (16) | 0.0372 (16) | 0.0364 (18) | 0.0076 (13) | −0.0120 (14) | −0.0024 (14) |
O10 | 0.0518 (19) | 0.0351 (17) | 0.049 (2) | 0.0034 (14) | −0.0083 (16) | −0.0030 (15) |
O11 | 0.0346 (16) | 0.0401 (16) | 0.047 (2) | 0.0077 (13) | −0.0069 (14) | −0.0119 (15) |
O12 | 0.050 (2) | 0.065 (2) | 0.037 (2) | 0.0072 (17) | 0.0081 (16) | 0.0054 (17) |
O13 | 0.055 (2) | 0.0491 (19) | 0.044 (2) | 0.0048 (16) | 0.0049 (16) | 0.0056 (16) |
O14 | 0.063 (2) | 0.061 (2) | 0.045 (2) | 0.0034 (18) | −0.0025 (17) | −0.0042 (18) |
O15 | 0.061 (2) | 0.0407 (17) | 0.044 (2) | 0.0095 (15) | 0.0061 (16) | 0.0031 (15) |
O17 | 0.225 (11) | 0.413 (17) | 0.175 (9) | −0.078 (11) | 0.034 (8) | −0.037 (10) |
O18 | 0.086 (3) | 0.080 (3) | 0.057 (3) | 0.010 (2) | 0.027 (2) | 0.005 (2) |
Cd1—O5 | 2.245 (3) | C21—H21B | 0.9700 |
Cd1—O6 | 2.260 (3) | C22—N4 | 1.475 (5) |
Cd1—O1 | 2.262 (3) | C22—H22A | 0.9700 |
Cd1—O3 | 2.282 (3) | C22—H22B | 0.9700 |
Cd1—N2 | 2.392 (4) | C23—N3 | 1.493 (5) |
Cd1—N1 | 2.403 (3) | C23—C24 | 1.501 (6) |
Cd2—O11 | 2.235 (3) | C23—H23A | 0.9700 |
Cd2—O12 | 2.247 (3) | C23—H23B | 0.9700 |
Cd2—O7 | 2.277 (3) | C24—C29 | 1.374 (7) |
Cd2—O9 | 2.307 (3) | C24—C25 | 1.381 (6) |
Cd2—N4 | 2.374 (3) | C25—C26 | 1.396 (7) |
Cd2—N3 | 2.387 (3) | C25—H25 | 0.9300 |
C1—N1 | 1.490 (6) | C26—C27 | 1.354 (8) |
C1—C2 | 1.514 (6) | C26—H26 | 0.9300 |
C1—H1A | 0.9700 | C27—C28 | 1.363 (8) |
C1—H1B | 0.9700 | C27—H27 | 0.9300 |
C2—N2 | 1.482 (5) | C28—C29 | 1.379 (7) |
C2—H2A | 0.9700 | C28—H28 | 0.9300 |
C2—H2B | 0.9700 | C29—H29 | 0.9300 |
C3—N1 | 1.485 (5) | C30—N3 | 1.472 (5) |
C3—C4 | 1.514 (6) | C30—C31 | 1.535 (6) |
C3—H3A | 0.9700 | C30—H30A | 0.9700 |
C3—H3B | 0.9700 | C30—H30B | 0.9700 |
C4—C9 | 1.394 (7) | C31—O8 | 1.237 (5) |
C4—C5 | 1.395 (7) | C31—O7 | 1.265 (5) |
C5—C6 | 1.425 (8) | C32—N4 | 1.488 (5) |
C5—H5 | 0.9300 | C32—C33 | 1.519 (6) |
C6—C7 | 1.376 (10) | C32—H32A | 0.9700 |
C6—H6 | 0.9300 | C32—H32B | 0.9700 |
C7—C8 | 1.343 (9) | C33—C38 | 1.382 (7) |
C7—H7 | 0.9300 | C33—C34 | 1.385 (7) |
C8—C9 | 1.373 (7) | C34—C35 | 1.383 (7) |
C8—H8 | 0.9300 | C34—H34 | 0.9300 |
C9—H9 | 0.9300 | C35—C36 | 1.354 (9) |
C10—N1 | 1.466 (5) | C35—H35 | 0.9300 |
C10—C11 | 1.535 (6) | C36—C37 | 1.365 (8) |
C10—H10A | 0.9700 | C36—H36 | 0.9300 |
C10—H10B | 0.9700 | C37—C38 | 1.392 (7) |
C11—O2 | 1.217 (5) | C37—H37 | 0.9300 |
C11—O1 | 1.265 (5) | C38—H38 | 0.9300 |
C12—N2 | 1.495 (5) | C39—N4 | 1.469 (5) |
C12—C13 | 1.514 (6) | C39—C40 | 1.539 (6) |
C12—H12A | 0.9700 | C39—H39A | 0.9700 |
C12—H12B | 0.9700 | C39—H39B | 0.9700 |
C13—C14 | 1.384 (7) | C40—O10 | 1.244 (5) |
C13—C18 | 1.388 (7) | C40—O9 | 1.259 (5) |
C14—C15 | 1.365 (7) | O5—H5A | 0.8190 |
C14—H14 | 0.9300 | O5—H5B | 0.8211 |
C15—C16 | 1.363 (9) | O6—H6A | 0.8236 |
C15—H15 | 0.9300 | O6—H6B | 0.8177 |
C16—C17 | 1.352 (10) | O11—H11A | 0.8264 |
C16—H16 | 0.9300 | O11—H11B | 0.8238 |
C17—C18 | 1.391 (8) | O12—H12C | 0.8201 |
C17—H17 | 0.9300 | O12—H12D | 0.8201 |
C18—H18 | 0.9300 | O13—H13A | 0.8224 |
C19—N2 | 1.466 (5) | O13—H13B | 0.8215 |
C19—C20 | 1.535 (6) | O14—H14A | 0.8201 |
C19—H19A | 0.9700 | O14—H14B | 0.8200 |
C19—H19B | 0.9700 | O15—H15A | 0.8200 |
C20—O4 | 1.233 (5) | O15—H15B | 0.8200 |
C20—O3 | 1.264 (5) | O17—H17A | 0.9840 |
C21—N3 | 1.476 (5) | O17—H17B | 0.9827 |
C21—C22 | 1.511 (6) | O18—H18A | 0.9835 |
C21—H21A | 0.9700 | O18—H18B | 0.9839 |
O5—Cd1—O6 | 91.93 (11) | C21—C22—H22A | 109.0 |
O5—Cd1—O1 | 95.67 (10) | N4—C22—H22B | 109.0 |
O6—Cd1—O1 | 93.92 (12) | C21—C22—H22B | 109.0 |
O5—Cd1—O3 | 94.41 (10) | H22A—C22—H22B | 107.8 |
O6—Cd1—O3 | 95.41 (11) | N3—C23—C24 | 116.7 (3) |
O1—Cd1—O3 | 166.02 (11) | N3—C23—H23A | 108.1 |
O5—Cd1—N2 | 89.43 (11) | C24—C23—H23A | 108.1 |
O6—Cd1—N2 | 168.10 (12) | N3—C23—H23B | 108.1 |
O1—Cd1—N2 | 97.71 (12) | C24—C23—H23B | 108.1 |
O3—Cd1—N2 | 72.70 (11) | H23A—C23—H23B | 107.3 |
O5—Cd1—N1 | 161.94 (12) | C29—C24—C25 | 117.4 (5) |
O6—Cd1—N1 | 102.62 (12) | C29—C24—C23 | 123.0 (4) |
O1—Cd1—N1 | 72.97 (11) | C25—C24—C23 | 119.6 (4) |
O3—Cd1—N1 | 94.80 (11) | C24—C25—C26 | 120.7 (5) |
N2—Cd1—N1 | 78.55 (12) | C24—C25—H25 | 119.6 |
O11—Cd2—O12 | 95.76 (12) | C26—C25—H25 | 119.6 |
O11—Cd2—O7 | 95.63 (11) | C27—C26—C25 | 119.7 (6) |
O12—Cd2—O7 | 96.35 (12) | C27—C26—H26 | 120.2 |
O11—Cd2—O9 | 96.09 (10) | C25—C26—H26 | 120.2 |
O12—Cd2—O9 | 93.47 (12) | C26—C27—C28 | 120.9 (5) |
O7—Cd2—O9 | 163.87 (10) | C26—C27—H27 | 119.5 |
O11—Cd2—N4 | 161.46 (12) | C28—C27—H27 | 119.5 |
O12—Cd2—N4 | 99.07 (12) | C27—C28—C29 | 118.9 (6) |
O7—Cd2—N4 | 93.74 (11) | C27—C28—H28 | 120.5 |
O9—Cd2—N4 | 72.03 (10) | C29—C28—H28 | 120.5 |
O11—Cd2—N3 | 89.20 (11) | C24—C29—C28 | 122.3 (5) |
O12—Cd2—N3 | 168.40 (12) | C24—C29—H29 | 118.9 |
O7—Cd2—N3 | 72.68 (11) | C28—C29—H29 | 118.9 |
O9—Cd2—N3 | 96.43 (11) | N3—C30—C31 | 113.4 (3) |
N4—Cd2—N3 | 78.37 (12) | N3—C30—H30A | 108.9 |
N1—C1—C2 | 112.6 (3) | C31—C30—H30A | 108.9 |
N1—C1—H1A | 109.1 | N3—C30—H30B | 108.9 |
C2—C1—H1A | 109.1 | C31—C30—H30B | 108.9 |
N1—C1—H1B | 109.1 | H30A—C30—H30B | 107.7 |
C2—C1—H1B | 109.1 | O8—C31—O7 | 125.0 (4) |
H1A—C1—H1B | 107.8 | O8—C31—C30 | 116.5 (4) |
N2—C2—C1 | 112.6 (4) | O7—C31—C30 | 118.5 (4) |
N2—C2—H2A | 109.1 | N4—C32—C33 | 116.3 (3) |
C1—C2—H2A | 109.1 | N4—C32—H32A | 108.2 |
N2—C2—H2B | 109.1 | C33—C32—H32A | 108.2 |
C1—C2—H2B | 109.1 | N4—C32—H32B | 108.2 |
H2A—C2—H2B | 107.8 | C33—C32—H32B | 108.2 |
N1—C3—C4 | 115.8 (4) | H32A—C32—H32B | 107.4 |
N1—C3—H3A | 108.3 | C38—C33—C34 | 118.5 (4) |
C4—C3—H3A | 108.3 | C38—C33—C32 | 121.5 (4) |
N1—C3—H3B | 108.3 | C34—C33—C32 | 120.0 (4) |
C4—C3—H3B | 108.3 | C35—C34—C33 | 120.1 (5) |
H3A—C3—H3B | 107.4 | C35—C34—H34 | 119.9 |
C9—C4—C5 | 118.0 (5) | C33—C34—H34 | 119.9 |
C9—C4—C3 | 121.0 (4) | C36—C35—C34 | 120.7 (6) |
C5—C4—C3 | 120.9 (5) | C36—C35—H35 | 119.7 |
C4—C5—C6 | 119.2 (6) | C34—C35—H35 | 119.7 |
C4—C5—H5 | 120.4 | C35—C36—C37 | 120.6 (5) |
C6—C5—H5 | 120.4 | C35—C36—H36 | 119.7 |
C7—C6—C5 | 120.5 (6) | C37—C36—H36 | 119.7 |
C7—C6—H6 | 119.8 | C36—C37—C38 | 119.4 (6) |
C5—C6—H6 | 119.8 | C36—C37—H37 | 120.3 |
C8—C7—C6 | 119.4 (6) | C38—C37—H37 | 120.3 |
C8—C7—H7 | 120.3 | C33—C38—C37 | 120.8 (5) |
C6—C7—H7 | 120.3 | C33—C38—H38 | 119.6 |
C7—C8—C9 | 121.9 (7) | C37—C38—H38 | 119.6 |
C7—C8—H8 | 119.0 | N4—C39—C40 | 112.6 (3) |
C9—C8—H8 | 119.0 | N4—C39—H39A | 109.1 |
C8—C9—C4 | 121.0 (6) | C40—C39—H39A | 109.1 |
C8—C9—H9 | 119.5 | N4—C39—H39B | 109.1 |
C4—C9—H9 | 119.5 | C40—C39—H39B | 109.1 |
N1—C10—C11 | 114.7 (3) | H39A—C39—H39B | 107.8 |
N1—C10—H10A | 108.6 | O10—C40—O9 | 125.6 (4) |
C11—C10—H10A | 108.6 | O10—C40—C39 | 116.7 (4) |
N1—C10—H10B | 108.6 | O9—C40—C39 | 117.7 (4) |
C11—C10—H10B | 108.6 | C10—N1—C3 | 111.7 (3) |
H10A—C10—H10B | 107.6 | C10—N1—C1 | 110.0 (3) |
O2—C11—O1 | 126.4 (4) | C3—N1—C1 | 112.6 (3) |
O2—C11—C10 | 116.9 (4) | C10—N1—Cd1 | 104.5 (2) |
O1—C11—C10 | 116.7 (4) | C3—N1—Cd1 | 113.9 (2) |
N2—C12—C13 | 115.4 (4) | C1—N1—Cd1 | 103.6 (2) |
N2—C12—H12A | 108.4 | C19—N2—C2 | 111.5 (3) |
C13—C12—H12A | 108.4 | C19—N2—C12 | 111.6 (3) |
N2—C12—H12B | 108.4 | C2—N2—C12 | 113.0 (3) |
C13—C12—H12B | 108.4 | C19—N2—Cd1 | 103.2 (3) |
H12A—C12—H12B | 107.5 | C2—N2—Cd1 | 104.0 (3) |
C14—C13—C18 | 118.1 (5) | C12—N2—Cd1 | 112.8 (3) |
C14—C13—C12 | 122.3 (4) | C30—N3—C21 | 111.7 (3) |
C18—C13—C12 | 119.6 (5) | C30—N3—C23 | 112.9 (3) |
C15—C14—C13 | 121.3 (6) | C21—N3—C23 | 113.3 (3) |
C15—C14—H14 | 119.3 | C30—N3—Cd2 | 104.8 (2) |
C13—C14—H14 | 119.3 | C21—N3—Cd2 | 105.1 (2) |
C16—C15—C14 | 120.0 (6) | C23—N3—Cd2 | 108.3 (2) |
C16—C15—H15 | 120.0 | C39—N4—C22 | 111.5 (3) |
C14—C15—H15 | 120.0 | C39—N4—C32 | 112.8 (3) |
C17—C16—C15 | 120.3 (6) | C22—N4—C32 | 113.4 (3) |
C17—C16—H16 | 119.9 | C39—N4—Cd2 | 104.4 (2) |
C15—C16—H16 | 119.9 | C22—N4—Cd2 | 104.1 (2) |
C16—C17—C18 | 120.6 (6) | C32—N4—Cd2 | 109.9 (2) |
C16—C17—H17 | 119.7 | C11—O1—Cd1 | 119.0 (3) |
C18—C17—H17 | 119.7 | C20—O3—Cd1 | 115.9 (3) |
C13—C18—C17 | 119.6 (6) | Cd1—O5—H5A | 116.8 |
C13—C18—H18 | 120.2 | Cd1—O5—H5B | 127.1 |
C17—C18—H18 | 120.2 | H5A—O5—H5B | 110.3 |
N2—C19—C20 | 114.6 (4) | Cd1—O6—H6A | 107.1 |
N2—C19—H19A | 108.6 | Cd1—O6—H6B | 141.7 |
C20—C19—H19A | 108.6 | H6A—O6—H6B | 110.7 |
N2—C19—H19B | 108.6 | C31—O7—Cd2 | 116.5 (3) |
C20—C19—H19B | 108.6 | C40—O9—Cd2 | 116.3 (3) |
H19A—C19—H19B | 107.6 | Cd2—O11—H11A | 117.1 |
O4—C20—O3 | 126.0 (4) | Cd2—O11—H11B | 115.0 |
O4—C20—C19 | 116.4 (4) | H11A—O11—H11B | 109.6 |
O3—C20—C19 | 117.6 (4) | Cd2—O12—H12C | 106.3 |
N3—C21—C22 | 113.0 (3) | Cd2—O12—H12D | 123.3 |
N3—C21—H21A | 109.0 | H12C—O12—H12D | 107.7 |
C22—C21—H21A | 109.0 | H13A—O13—H13B | 110.2 |
N3—C21—H21B | 109.0 | H14A—O14—H14B | 107.7 |
C22—C21—H21B | 109.0 | H15A—O15—H15B | 107.7 |
H21A—C21—H21B | 107.8 | H17A—O17—H17B | 109.4 |
N4—C22—C21 | 112.9 (3) | H18A—O18—H18B | 109.5 |
N4—C22—H22A | 109.0 | ||
N1—C1—C2—N2 | −64.9 (5) | N1—Cd1—N2—C19 | −131.6 (3) |
N1—C3—C4—C9 | −88.1 (5) | O5—Cd1—N2—C2 | 178.6 (2) |
N1—C3—C4—C5 | 93.0 (5) | O6—Cd1—N2—C2 | 81.9 (6) |
C9—C4—C5—C6 | 1.1 (7) | O1—Cd1—N2—C2 | −85.8 (2) |
C3—C4—C5—C6 | −180.0 (4) | O3—Cd1—N2—C2 | 83.8 (2) |
C4—C5—C6—C7 | −0.2 (8) | N1—Cd1—N2—C2 | −15.0 (2) |
C5—C6—C7—C8 | −0.8 (9) | O5—Cd1—N2—C12 | −58.6 (3) |
C6—C7—C8—C9 | 1.0 (9) | O6—Cd1—N2—C12 | −155.3 (5) |
C7—C8—C9—C4 | −0.1 (9) | O1—Cd1—N2—C12 | 37.0 (3) |
C5—C4—C9—C8 | −1.0 (7) | O3—Cd1—N2—C12 | −153.4 (3) |
C3—C4—C9—C8 | −179.9 (5) | N1—Cd1—N2—C12 | 107.8 (3) |
N1—C10—C11—O2 | 156.5 (4) | C31—C30—N3—C21 | −76.4 (4) |
N1—C10—C11—O1 | −25.4 (6) | C31—C30—N3—C23 | 154.5 (3) |
N2—C12—C13—C14 | 74.1 (6) | C31—C30—N3—Cd2 | 36.9 (4) |
N2—C12—C13—C18 | −102.7 (5) | C22—C21—N3—C30 | 152.5 (3) |
C18—C13—C14—C15 | 1.2 (8) | C22—C21—N3—C23 | −78.6 (4) |
C12—C13—C14—C15 | −175.7 (5) | C22—C21—N3—Cd2 | 39.4 (4) |
C13—C14—C15—C16 | −0.1 (9) | C24—C23—N3—C30 | 69.2 (5) |
C14—C15—C16—C17 | −0.6 (10) | C24—C23—N3—C21 | −59.0 (5) |
C15—C16—C17—C18 | 0.1 (10) | C24—C23—N3—Cd2 | −175.2 (3) |
C14—C13—C18—C17 | −1.7 (8) | O11—Cd2—N3—C30 | 64.9 (2) |
C12—C13—C18—C17 | 175.3 (5) | O12—Cd2—N3—C30 | −50.7 (7) |
C16—C17—C18—C13 | 1.1 (10) | O7—Cd2—N3—C30 | −31.3 (2) |
N2—C19—C20—O4 | 161.2 (4) | O9—Cd2—N3—C30 | 160.9 (2) |
N2—C19—C20—O3 | −20.1 (5) | N4—Cd2—N3—C30 | −129.0 (3) |
N3—C21—C22—N4 | −62.1 (5) | O11—Cd2—N3—C21 | −177.2 (2) |
N3—C23—C24—C29 | −79.8 (6) | O12—Cd2—N3—C21 | 67.2 (7) |
N3—C23—C24—C25 | 102.3 (5) | O7—Cd2—N3—C21 | 86.6 (2) |
C29—C24—C25—C26 | −0.3 (8) | O9—Cd2—N3—C21 | −81.2 (2) |
C23—C24—C25—C26 | 177.7 (5) | N4—Cd2—N3—C21 | −11.1 (2) |
C24—C25—C26—C27 | 1.0 (9) | O11—Cd2—N3—C23 | −55.9 (3) |
C25—C26—C27—C28 | −0.9 (9) | O12—Cd2—N3—C23 | −171.4 (5) |
C26—C27—C28—C29 | 0.2 (9) | O7—Cd2—N3—C23 | −152.0 (3) |
C25—C24—C29—C28 | −0.4 (7) | O9—Cd2—N3—C23 | 40.2 (3) |
C23—C24—C29—C28 | −178.3 (5) | N4—Cd2—N3—C23 | 110.3 (3) |
C27—C28—C29—C24 | 0.4 (8) | C40—C39—N4—C22 | −69.7 (4) |
N3—C30—C31—O8 | 162.4 (4) | C40—C39—N4—C32 | 161.4 (3) |
N3—C30—C31—O7 | −19.6 (5) | C40—C39—N4—Cd2 | 42.1 (4) |
N4—C32—C33—C38 | −84.9 (5) | C21—C22—N4—C39 | 157.3 (3) |
N4—C32—C33—C34 | 97.4 (5) | C21—C22—N4—C32 | −74.0 (4) |
C38—C33—C34—C35 | −0.6 (7) | C21—C22—N4—Cd2 | 45.4 (4) |
C32—C33—C34—C35 | 177.1 (5) | C33—C32—N4—C39 | 67.5 (5) |
C33—C34—C35—C36 | 1.3 (9) | C33—C32—N4—C22 | −60.4 (5) |
C34—C35—C36—C37 | −0.9 (9) | C33—C32—N4—Cd2 | −176.5 (3) |
C35—C36—C37—C38 | 0.0 (8) | O11—Cd2—N4—C39 | −85.7 (4) |
C34—C33—C38—C37 | −0.3 (7) | O12—Cd2—N4—C39 | 57.0 (3) |
C32—C33—C38—C37 | −178.0 (4) | O7—Cd2—N4—C39 | 154.1 (2) |
C36—C37—C38—C33 | 0.6 (8) | O9—Cd2—N4—C39 | −33.7 (2) |
N4—C39—C40—O10 | 156.5 (4) | N3—Cd2—N4—C39 | −134.5 (3) |
N4—C39—C40—O9 | −25.5 (5) | O11—Cd2—N4—C22 | 31.3 (5) |
C11—C10—N1—C3 | 160.3 (4) | O12—Cd2—N4—C22 | 174.1 (2) |
C11—C10—N1—C1 | −73.9 (5) | O7—Cd2—N4—C22 | −88.9 (2) |
C11—C10—N1—Cd1 | 36.7 (4) | O9—Cd2—N4—C22 | 83.3 (2) |
C4—C3—N1—C10 | 54.9 (5) | N3—Cd2—N4—C22 | −17.5 (2) |
C4—C3—N1—C1 | −69.5 (5) | O11—Cd2—N4—C32 | 153.1 (3) |
C4—C3—N1—Cd1 | 173.0 (3) | O12—Cd2—N4—C32 | −64.2 (3) |
C2—C1—N1—C10 | 154.9 (3) | O7—Cd2—N4—C32 | 32.8 (3) |
C2—C1—N1—C3 | −79.8 (4) | O9—Cd2—N4—C32 | −155.0 (3) |
C2—C1—N1—Cd1 | 43.7 (4) | N3—Cd2—N4—C32 | 104.3 (3) |
O5—Cd1—N1—C10 | −80.5 (5) | O2—C11—O1—Cd1 | 174.4 (4) |
O6—Cd1—N1—C10 | 62.5 (3) | C10—C11—O1—Cd1 | −3.4 (5) |
O1—Cd1—N1—C10 | −27.8 (3) | O5—Cd1—O1—C11 | −176.2 (3) |
O3—Cd1—N1—C10 | 159.1 (3) | O6—Cd1—O1—C11 | −83.8 (3) |
N2—Cd1—N1—C10 | −129.6 (3) | O3—Cd1—O1—C11 | 47.9 (6) |
O5—Cd1—N1—C3 | 157.4 (3) | N2—Cd1—O1—C11 | 93.6 (3) |
O6—Cd1—N1—C3 | −59.7 (3) | N1—Cd1—O1—C11 | 18.2 (3) |
O1—Cd1—N1—C3 | −149.9 (3) | O4—C20—O3—Cd1 | 165.0 (3) |
O3—Cd1—N1—C3 | 37.0 (3) | C19—C20—O3—Cd1 | −13.5 (5) |
N2—Cd1—N1—C3 | 108.2 (3) | O5—Cd1—O3—C20 | −61.3 (3) |
O5—Cd1—N1—C1 | 34.7 (5) | O6—Cd1—O3—C20 | −153.7 (3) |
O6—Cd1—N1—C1 | 177.6 (2) | O1—Cd1—O3—C20 | 74.7 (5) |
O1—Cd1—N1—C1 | 87.4 (2) | N2—Cd1—O3—C20 | 26.7 (3) |
O3—Cd1—N1—C1 | −85.7 (2) | N1—Cd1—O3—C20 | 103.1 (3) |
N2—Cd1—N1—C1 | −14.5 (2) | O8—C31—O7—Cd2 | 166.0 (3) |
C20—C19—N2—C2 | −72.4 (5) | C30—C31—O7—Cd2 | −11.8 (5) |
C20—C19—N2—C12 | 160.1 (4) | O11—Cd2—O7—C31 | −62.8 (3) |
C20—C19—N2—Cd1 | 38.7 (4) | O12—Cd2—O7—C31 | −159.3 (3) |
C1—C2—N2—C19 | 154.9 (4) | O9—Cd2—O7—C31 | 73.6 (5) |
C1—C2—N2—C12 | −78.3 (5) | N4—Cd2—O7—C31 | 101.2 (3) |
C1—C2—N2—Cd1 | 44.3 (4) | N3—Cd2—O7—C31 | 24.6 (3) |
C13—C12—N2—C19 | 41.0 (5) | O10—C40—O9—Cd2 | 169.7 (3) |
C13—C12—N2—C2 | −85.7 (5) | C39—C40—O9—Cd2 | −8.1 (5) |
C13—C12—N2—Cd1 | 156.7 (3) | O11—Cd2—O9—C40 | −170.6 (3) |
O5—Cd1—N2—C19 | 62.0 (3) | O12—Cd2—O9—C40 | −74.4 (3) |
O6—Cd1—N2—C19 | −34.7 (7) | O7—Cd2—O9—C40 | 53.1 (5) |
O1—Cd1—N2—C19 | 157.6 (2) | N4—Cd2—O9—C40 | 24.0 (3) |
O3—Cd1—N2—C19 | −32.8 (2) | N3—Cd2—O9—C40 | 99.6 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5A···O9i | 0.82 | 1.90 | 2.717 (4) | 173 |
O5—H5B···O8ii | 0.82 | 1.86 | 2.670 (4) | 167 |
O6—H6A···O14iii | 0.82 | 1.87 | 2.668 (4) | 162 |
O6—H6B···O13ii | 0.82 | 2.19 | 2.680 (4) | 119 |
O6—H6B···O18 | 0.82 | 2.51 | 2.938 (5) | 114 |
O11—H11A···O1iv | 0.83 | 1.83 | 2.654 (4) | 178 |
O11—H11B···O4v | 0.82 | 1.84 | 2.651 (4) | 165 |
O12—H12C···O18vi | 0.82 | 2.31 | 3.117 (5) | 168 |
O12—H12D···O18iv | 0.82 | 2.00 | 2.769 (5) | 155 |
O13—H13A···O10vii | 0.82 | 1.99 | 2.799 (4) | 169 |
O13—H13B···O7 | 0.82 | 1.97 | 2.784 (4) | 169 |
O14—H14A···O15 | 0.82 | 2.18 | 2.829 (5) | 136 |
O14—H14B···O10vi | 0.82 | 2.01 | 2.774 (5) | 155 |
O15—H15A···O2 | 0.82 | 1.90 | 2.704 (4) | 165 |
O15—H15B···O3vii | 0.82 | 2.03 | 2.786 (4) | 153 |
O17—H17B···O4viii | 0.98 | 2.00 | 2.778 (12) | 134 |
O18—H18B···O9i | 0.98 | 2.48 | 3.323 (5) | 144 |
C32—H32A···O18vi | 0.97 | 2.51 | 3.477 (6) | 178 |
Symmetry codes: (i) x−1, y, z; (ii) x−1, y−1, z; (iii) x, y−1, z; (iv) x+1, y, z; (v) x+1, y+1, z; (vi) −x+1, −y+1, −z; (vii) x, y+1, z; (viii) −x+1/2, y+1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Cd(C20H22N2O4)(H2O)2]·2.5H2O |
Mr | 547.87 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 294 |
a, b, c (Å) | 13.9704 (16), 9.4600 (11), 36.471 (3) |
β (°) | 92.273 (2) |
V (Å3) | 4816.2 (9) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 0.95 |
Crystal size (mm) | 0.30 × 0.20 × 0.20 |
Data collection | |
Diffractometer | Bruker SMART-CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2001) |
Tmin, Tmax | 0.763, 0.832 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 49413, 9436, 7654 |
Rint | 0.075 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.050, 0.123, 1.06 |
No. of reflections | 9436 |
No. of parameters | 568 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.70, −0.85 |
Computer programs: SMART (Bruker, 2000), SAINT-Plus (Bruker, 2000), SAINT-Plus, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), WinGX2003 (Farrugia, 1999), PLATON (Spek, 2003), PLATON.
Cd1—O5 | 2.245 (3) | Cd2—O11 | 2.235 (3) |
Cd1—O6 | 2.260 (3) | Cd2—O12 | 2.247 (3) |
Cd1—O1 | 2.262 (3) | Cd2—O7 | 2.277 (3) |
Cd1—O3 | 2.282 (3) | Cd2—O9 | 2.307 (3) |
Cd1—N2 | 2.392 (4) | Cd2—N4 | 2.374 (3) |
Cd1—N1 | 2.403 (3) | Cd2—N3 | 2.387 (3) |
O5—Cd1—O6 | 91.93 (11) | O11—Cd2—O12 | 95.76 (12) |
O5—Cd1—O1 | 95.67 (10) | O11—Cd2—O7 | 95.63 (11) |
O6—Cd1—O1 | 93.92 (12) | O12—Cd2—O7 | 96.35 (12) |
O5—Cd1—O3 | 94.41 (10) | O11—Cd2—O9 | 96.09 (10) |
O6—Cd1—O3 | 95.41 (11) | O12—Cd2—O9 | 93.47 (12) |
O1—Cd1—O3 | 166.02 (11) | O7—Cd2—O9 | 163.87 (10) |
O5—Cd1—N2 | 89.43 (11) | O11—Cd2—N4 | 161.46 (12) |
O6—Cd1—N2 | 168.10 (12) | O12—Cd2—N4 | 99.07 (12) |
O1—Cd1—N2 | 97.71 (12) | O7—Cd2—N4 | 93.74 (11) |
O3—Cd1—N2 | 72.70 (11) | O9—Cd2—N4 | 72.03 (10) |
O5—Cd1—N1 | 161.94 (12) | O11—Cd2—N3 | 89.20 (11) |
O6—Cd1—N1 | 102.62 (12) | O12—Cd2—N3 | 168.40 (12) |
O1—Cd1—N1 | 72.97 (11) | O7—Cd2—N3 | 72.68 (11) |
O3—Cd1—N1 | 94.80 (11) | O9—Cd2—N3 | 96.43 (11) |
N2—Cd1—N1 | 78.55 (12) | N4—Cd2—N3 | 78.37 (12) |
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5A···O9i | 0.8200 | 1.9000 | 2.717 (4) | 173.00 |
O5—H5B···O8ii | 0.8200 | 1.8600 | 2.670 (4) | 167.00 |
O6—H6A···O14iii | 0.8200 | 1.8700 | 2.668 (4) | 162.00 |
O6—H6B···O13ii | 0.8200 | 2.1900 | 2.680 (4) | 119.00 |
O6—H6B···O18 | 0.8200 | 2.5100 | 2.938 (5) | 114.00 |
O11—H11A···O1iv | 0.8300 | 1.8300 | 2.654 (4) | 178.00 |
O11—H11B···O4v | 0.8200 | 1.8400 | 2.651 (4) | 165.00 |
O12—H12C···O18vi | 0.8200 | 2.3100 | 3.117 (5) | 168.00 |
O12—H12D···O18iv | 0.8200 | 2.0000 | 2.769 (5) | 155.00 |
O13—H13A···O10vii | 0.8200 | 1.9900 | 2.799 (4) | 169.00 |
O13—H13B···O7 | 0.8200 | 1.9700 | 2.784 (4) | 169.00 |
O14—H14A···O15 | 0.8200 | 2.1800 | 2.829 (5) | 136.00 |
O14—H14B···O10vi | 0.8200 | 2.0100 | 2.774 (5) | 155.00 |
O15—H15A···O2 | 0.8200 | 1.9000 | 2.704 (4) | 165.00 |
O15—H15B···O3vii | 0.8200 | 2.0300 | 2.786 (4) | 153.00 |
O17—H17B···O4viii | 0.9800 | 2.0000 | 2.778 (12) | 134.00 |
O18—H18B···O9i | 0.9800 | 2.4800 | 3.323 (5) | 144.00 |
C32—H32A···O18vi | 0.9700 | 2.5100 | 3.477 (6) | 178.00 |
Symmetry codes: (i) x−1, y, z; (ii) x−1, y−1, z; (iii) x, y−1, z; (iv) x+1, y, z; (v) x+1, y+1, z; (vi) −x+1, −y+1, −z; (vii) x, y+1, z; (viii) −x+1/2, y+1/2, −z+1/2. |
Previously we have synthesized the Cu(II) complex of (H2L=[N,N'-bis(benzyl)ethane-1,2-diyldiimino]diacetate) (Xu et al., 2004). Herein, we report the structure of the Cd(II) complex (1) with this ligand. In (1)(Fig 1) the asymmetric unit consists of two independent complex molecules and and five molecules of solvent water. The coordination geometry around atoms Cd1 and Cd2 is distorted octahedral defined by a N2O4 donor set, from two amine N atoms, two carboxyl O atoms, and two water O atoms (selected bond lengths and angles are given in Table 1). In the crystal structure (Fig. 2), extensive O—H···O hydrogen bonds (Table 2) form one-dimensional chains along the b axis.