Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805025122/sj6130sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805025122/sj6130Isup2.hkl |
CCDC reference: 283991
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- R factor = 0.030
- wR factor = 0.082
- Data-to-parameter ratio = 11.5
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O1 PLAT420_ALERT_2_B D-H Without Acceptor O11 - H11A ... ?
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cd1 - O5 .. 8.34 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cd1 - O11 .. 5.93 su PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.27 PLAT432_ALERT_2_C Short Inter X...Y Contact O6 .. C1 .. 2.92 Ang.
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: APEX-II (Bruker, 2003); cell refinement: APEX-II and SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001) and DIAMOND (Brandenburg & Berndt, 1999); software used to prepare material for publication: SHELXTL.
[Cd(C5H3N2O4)2(H2O)3]·H2O | F(000) = 984 |
Mr = 494.66 | Dx = 1.989 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 6.8945 (9) Å | Cell parameters from 4160 reflections |
b = 17.432 (2) Å | θ = 2.3–28.0° |
c = 13.8726 (19) Å | µ = 1.40 mm−1 |
β = 97.771 (2)° | T = 293 K |
V = 1652.0 (4) Å3 | Block, pale yellow |
Z = 4 | 0.38 × 0.16 × 0.10 mm |
Bruker APEX-II CCD area-detector diffractometer | 2913 independent reflections |
Radiation source: fine-focus sealed tube | 2547 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
φ and ω scans | θmax = 25.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −8→8 |
Tmin = 0.602, Tmax = 0.870 | k = −20→20 |
9284 measured reflections | l = −16→15 |
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)] = 0.030 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.082 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.06P)2] where P = (Fo2 + 2Fc2)/3 |
2913 reflections | (Δ/σ)max = 0.002 |
254 parameters | Δρmax = 1.08 e Å−3 |
12 restraints | Δρmin = −0.63 e Å−3 |
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 | 0.20253 (3) | 0.766981 (11) | 0.181577 (15) | 0.03706 (12) | |
O1 | −0.1202 (4) | 0.68883 (14) | 0.0999 (2) | 0.0717 (8) | |
O2 | −0.2349 (3) | 0.57266 (12) | 0.06718 (17) | 0.0478 (5) | |
H2 | −0.1950 | 0.5286 | 0.0762 | 0.072* | |
O3 | −0.1122 (3) | 0.44096 (12) | 0.09420 (16) | 0.0454 (5) | |
O4 | 0.1582 (3) | 0.38021 (12) | 0.16132 (15) | 0.0459 (5) | |
O5 | 0.3403 (3) | 0.91249 (12) | 0.21005 (16) | 0.0446 (5) | |
O6 | 0.2494 (3) | 1.03249 (13) | 0.18263 (17) | 0.0518 (6) | |
H6A | 0.1503 | 1.0556 | 0.1595 | 0.078* | |
O7 | −0.0415 (3) | 1.10409 (11) | 0.11224 (14) | 0.0409 (5) | |
O8 | −0.3400 (3) | 1.07928 (11) | 0.03779 (14) | 0.0406 (5) | |
O9 | 0.3702 (3) | 0.77932 (11) | 0.05186 (15) | 0.0447 (5) | |
H9A | 0.3913 | 0.7398 | 0.0189 | 0.054* | |
H9B | 0.3327 | 0.8194 | 0.0196 | 0.054* | |
O10 | 0.0879 (4) | 0.75886 (12) | 0.32848 (19) | 0.0516 (6) | |
H10A | 0.0724 | 0.7116 | 0.3406 | 0.062* | |
H10B | −0.0089 | 0.7884 | 0.3324 | 0.062* | |
O11 | 0.5103 (4) | 0.76518 (12) | 0.28174 (19) | 0.0523 (6) | |
H11A | 0.5956 | 0.7777 | 0.2457 | 0.063* | |
H11B | 0.4996 | 0.7948 | 0.3295 | 0.063* | |
N1 | 0.2411 (3) | 0.63827 (14) | 0.17727 (15) | 0.0360 (6) | |
N2 | 0.3485 (3) | 0.52061 (14) | 0.20013 (17) | 0.0370 (5) | |
H2A | 0.4262 | 0.4831 | 0.2178 | 0.044* | |
N3 | −0.0170 (3) | 0.85773 (12) | 0.12456 (16) | 0.0334 (5) | |
N4 | −0.2763 (3) | 0.92187 (13) | 0.06031 (18) | 0.0360 (5) | |
H4A | −0.3927 | 0.9311 | 0.0319 | 0.043* | |
C1 | 0.3918 (4) | 0.59493 (16) | 0.2106 (2) | 0.0385 (7) | |
H1 | 0.5131 | 0.6138 | 0.2380 | 0.046* | |
C2 | 0.0934 (4) | 0.58798 (16) | 0.14284 (18) | 0.0320 (6) | |
C3 | −0.0982 (4) | 0.62043 (17) | 0.1013 (2) | 0.0415 (7) | |
C4 | 0.1594 (4) | 0.51437 (16) | 0.15644 (19) | 0.0313 (6) | |
C5 | 0.0655 (4) | 0.43878 (15) | 0.13635 (19) | 0.0349 (6) | |
C6 | −0.1999 (4) | 0.85250 (16) | 0.0806 (2) | 0.0399 (7) | |
H6 | −0.2659 | 0.8066 | 0.0658 | 0.048* | |
C7 | 0.0214 (4) | 0.93416 (15) | 0.13238 (18) | 0.0291 (6) | |
C8 | 0.2168 (4) | 0.95985 (19) | 0.17800 (17) | 0.0349 (7) | |
C9 | −0.1390 (4) | 0.97568 (15) | 0.09228 (18) | 0.0294 (6) | |
C10 | −0.1784 (4) | 1.05914 (15) | 0.07972 (18) | 0.0322 (6) | |
O12 | 0.4462 (3) | 0.65402 (12) | 0.94844 (14) | 0.0509 (6) | |
H12B | 0.3466 | 0.6251 | 0.9366 | 0.061* | |
H12A | 0.5427 | 0.6358 | 0.9861 | 0.061* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.02870 (16) | 0.02807 (17) | 0.05135 (17) | 0.00434 (8) | −0.00573 (10) | 0.00527 (8) |
O1 | 0.0471 (14) | 0.0327 (13) | 0.122 (2) | 0.0075 (11) | −0.0355 (14) | 0.0020 (13) |
O2 | 0.0333 (11) | 0.0364 (11) | 0.0673 (14) | −0.0001 (9) | −0.0165 (10) | 0.0049 (10) |
O3 | 0.0334 (11) | 0.0348 (11) | 0.0642 (13) | −0.0047 (9) | −0.0070 (10) | 0.0005 (10) |
O4 | 0.0405 (11) | 0.0275 (11) | 0.0686 (13) | 0.0013 (9) | 0.0033 (10) | 0.0031 (10) |
O5 | 0.0294 (11) | 0.0399 (12) | 0.0590 (12) | 0.0061 (9) | −0.0149 (9) | 0.0002 (10) |
O6 | 0.0351 (11) | 0.0337 (12) | 0.0778 (15) | −0.0033 (10) | −0.0240 (10) | −0.0031 (10) |
O7 | 0.0350 (11) | 0.0281 (10) | 0.0554 (11) | −0.0013 (9) | −0.0093 (9) | −0.0039 (9) |
O8 | 0.0269 (10) | 0.0309 (10) | 0.0602 (12) | 0.0058 (8) | −0.0081 (9) | 0.0073 (9) |
O9 | 0.0487 (14) | 0.0290 (10) | 0.0564 (13) | 0.0044 (9) | 0.0075 (10) | 0.0043 (9) |
O10 | 0.0564 (16) | 0.0310 (11) | 0.0688 (16) | 0.0071 (10) | 0.0140 (13) | 0.0086 (10) |
O11 | 0.0405 (14) | 0.0498 (15) | 0.0625 (15) | −0.0059 (10) | −0.0081 (11) | −0.0002 (10) |
N1 | 0.0268 (12) | 0.0316 (13) | 0.0465 (14) | −0.0008 (10) | −0.0064 (10) | 0.0038 (9) |
N2 | 0.0270 (12) | 0.0303 (12) | 0.0511 (14) | 0.0049 (10) | −0.0038 (10) | 0.0050 (11) |
N3 | 0.0229 (12) | 0.0259 (12) | 0.0490 (13) | −0.0014 (9) | −0.0034 (10) | 0.0047 (9) |
N4 | 0.0188 (11) | 0.0289 (12) | 0.0570 (14) | 0.0004 (9) | −0.0069 (10) | 0.0049 (10) |
C1 | 0.0263 (14) | 0.0329 (15) | 0.0522 (16) | −0.0019 (12) | −0.0094 (12) | 0.0013 (12) |
C2 | 0.0268 (14) | 0.0303 (15) | 0.0367 (14) | −0.0004 (11) | −0.0040 (11) | 0.0024 (11) |
C3 | 0.0293 (15) | 0.0338 (17) | 0.0566 (17) | 0.0020 (13) | −0.0118 (13) | 0.0024 (13) |
C4 | 0.0247 (13) | 0.0328 (15) | 0.0354 (13) | −0.0016 (11) | 0.0002 (10) | 0.0023 (11) |
C5 | 0.0334 (15) | 0.0303 (15) | 0.0408 (15) | −0.0017 (12) | 0.0051 (12) | −0.0010 (12) |
C6 | 0.0285 (15) | 0.0261 (14) | 0.0618 (18) | −0.0019 (12) | −0.0067 (13) | 0.0038 (13) |
C7 | 0.0227 (13) | 0.0279 (14) | 0.0350 (13) | 0.0000 (11) | −0.0023 (10) | 0.0005 (11) |
C8 | 0.0273 (15) | 0.0363 (17) | 0.0380 (15) | 0.0009 (12) | −0.0061 (12) | −0.0018 (11) |
C9 | 0.0243 (13) | 0.0297 (14) | 0.0331 (13) | 0.0016 (11) | −0.0003 (10) | 0.0019 (11) |
C10 | 0.0299 (15) | 0.0307 (14) | 0.0350 (13) | 0.0012 (12) | 0.0012 (11) | 0.0011 (11) |
O12 | 0.0342 (12) | 0.0438 (12) | 0.0691 (14) | 0.0030 (10) | −0.0141 (10) | −0.0021 (10) |
Cd1—N3 | 2.257 (2) | N1—C1 | 1.317 (4) |
Cd1—N1 | 2.261 (2) | N1—C2 | 1.379 (3) |
Cd1—O9 | 2.276 (2) | N2—C1 | 1.333 (4) |
Cd1—O10 | 2.288 (3) | N2—C4 | 1.366 (3) |
Cd1—O11 | 2.374 (2) | N2—H2A | 0.8600 |
O1—C3 | 1.202 (4) | N3—C6 | 1.327 (3) |
O2—C3 | 1.298 (4) | N3—C7 | 1.360 (3) |
O2—H2 | 0.8200 | N4—C6 | 1.334 (4) |
O3—C5 | 1.285 (3) | N4—C9 | 1.364 (3) |
O4—C5 | 1.230 (4) | N4—H4A | 0.8600 |
O5—C8 | 1.226 (4) | C1—H1 | 0.9300 |
O6—C8 | 1.286 (4) | C2—C4 | 1.366 (4) |
O6—H6A | 0.8200 | C2—C3 | 1.480 (4) |
O7—C10 | 1.262 (3) | C4—C5 | 1.478 (4) |
O8—C10 | 1.236 (3) | C6—H6 | 0.9300 |
O9—H9A | 0.8501 | C7—C9 | 1.375 (4) |
O9—H9B | 0.8500 | C7—C8 | 1.478 (3) |
O10—H10A | 0.8499 | C9—C10 | 1.486 (4) |
O10—H10B | 0.8500 | O12—H12B | 0.8500 |
O11—H11A | 0.8505 | O12—H12A | 0.8500 |
O11—H11B | 0.8501 | ||
N3—Cd1—N1 | 139.63 (8) | C9—N4—H4A | 125.7 |
N3—Cd1—O9 | 92.57 (8) | N1—C1—N2 | 111.4 (2) |
N1—Cd1—O9 | 89.93 (8) | N1—C1—H1 | 124.3 |
N3—Cd1—O10 | 93.41 (8) | N2—C1—H1 | 124.3 |
N1—Cd1—O10 | 91.04 (8) | C4—C2—N1 | 109.4 (2) |
O9—Cd1—O10 | 169.57 (9) | C4—C2—C3 | 132.5 (3) |
N3—Cd1—O11 | 135.91 (7) | N1—C2—C3 | 118.1 (2) |
N1—Cd1—O11 | 84.45 (7) | O1—C3—O2 | 123.1 (3) |
O9—Cd1—O11 | 87.41 (9) | O1—C3—C2 | 119.3 (3) |
O10—Cd1—O11 | 82.35 (10) | O2—C3—C2 | 117.5 (3) |
C3—O2—H2 | 109.5 | C2—C4—N2 | 105.5 (2) |
C8—O6—H6A | 109.5 | C2—C4—C5 | 133.0 (3) |
Cd1—O9—H9A | 119.4 | N2—C4—C5 | 121.5 (2) |
Cd1—O9—H9B | 110.1 | O4—C5—O3 | 125.5 (3) |
H9A—O9—H9B | 116.4 | O4—C5—C4 | 119.3 (3) |
Cd1—O10—H10A | 107.7 | O3—C5—C4 | 115.2 (2) |
Cd1—O10—H10B | 112.9 | N3—C6—N4 | 111.0 (2) |
H10A—O10—H10B | 116.9 | N3—C6—H6 | 124.5 |
Cd1—O11—H11A | 106.6 | N4—C6—H6 | 124.5 |
Cd1—O11—H11B | 106.4 | N3—C7—C9 | 110.3 (2) |
H11A—O11—H11B | 116.2 | N3—C7—C8 | 119.2 (2) |
C1—N1—C2 | 105.5 (2) | C9—C7—C8 | 130.6 (3) |
C1—N1—Cd1 | 130.54 (19) | O5—C8—O6 | 122.5 (2) |
C2—N1—Cd1 | 123.76 (17) | O5—C8—C7 | 120.0 (3) |
C1—N2—C4 | 108.2 (2) | O6—C8—C7 | 117.6 (2) |
C1—N2—H2A | 125.9 | N4—C9—C7 | 104.8 (2) |
C4—N2—H2A | 125.9 | N4—C9—C10 | 121.8 (2) |
C6—N3—C7 | 105.5 (2) | C7—C9—C10 | 133.4 (2) |
C6—N3—Cd1 | 131.54 (18) | O8—C10—O7 | 125.1 (3) |
C7—N3—Cd1 | 123.00 (17) | O8—C10—C9 | 118.2 (2) |
C6—N4—C9 | 108.5 (2) | O7—C10—C9 | 116.7 (2) |
C6—N4—H4A | 125.7 | H12B—O12—H12A | 116.2 |
N3—Cd1—N1—C1 | 174.2 (2) | N1—C2—C4—C5 | 178.2 (3) |
O9—Cd1—N1—C1 | 80.3 (3) | C3—C2—C4—C5 | −0.9 (5) |
O10—Cd1—N1—C1 | −89.3 (3) | C1—N2—C4—C2 | −0.6 (3) |
O11—Cd1—N1—C1 | −7.1 (3) | C1—N2—C4—C5 | −178.8 (2) |
N3—Cd1—N1—C2 | −11.3 (3) | C2—C4—C5—O4 | −176.0 (3) |
O9—Cd1—N1—C2 | −105.1 (2) | N2—C4—C5—O4 | 1.5 (4) |
O10—Cd1—N1—C2 | 85.2 (2) | C2—C4—C5—O3 | 3.1 (4) |
O11—Cd1—N1—C2 | 167.5 (2) | N2—C4—C5—O3 | −179.4 (2) |
N1—Cd1—N3—C6 | 9.9 (3) | C7—N3—C6—N4 | 0.3 (3) |
O9—Cd1—N3—C6 | 102.8 (3) | Cd1—N3—C6—N4 | 179.25 (19) |
O10—Cd1—N3—C6 | −85.8 (3) | C9—N4—C6—N3 | −0.1 (4) |
O11—Cd1—N3—C6 | −168.3 (2) | C6—N3—C7—C9 | −0.4 (3) |
N1—Cd1—N3—C7 | −171.34 (18) | Cd1—N3—C7—C9 | −179.43 (17) |
O9—Cd1—N3—C7 | −78.4 (2) | C6—N3—C7—C8 | −179.4 (2) |
O10—Cd1—N3—C7 | 93.0 (2) | Cd1—N3—C7—C8 | 1.5 (3) |
O11—Cd1—N3—C7 | 10.5 (3) | N3—C7—C8—O5 | −1.6 (4) |
C2—N1—C1—N2 | −0.4 (3) | C9—C7—C8—O5 | 179.6 (3) |
Cd1—N1—C1—N2 | 174.87 (18) | N3—C7—C8—O6 | 178.8 (2) |
C4—N2—C1—N1 | 0.7 (3) | C9—C7—C8—O6 | −0.1 (4) |
C1—N1—C2—C4 | 0.0 (3) | C6—N4—C9—C7 | −0.1 (3) |
Cd1—N1—C2—C4 | −175.70 (17) | C6—N4—C9—C10 | 179.4 (2) |
C1—N1—C2—C3 | 179.2 (3) | N3—C7—C9—N4 | 0.3 (3) |
Cd1—N1—C2—C3 | 3.5 (3) | C8—C7—C9—N4 | 179.2 (3) |
C4—C2—C3—O1 | 178.1 (3) | N3—C7—C9—C10 | −179.2 (3) |
N1—C2—C3—O1 | −0.9 (5) | C8—C7—C9—C10 | −0.3 (5) |
C4—C2—C3—O2 | −2.5 (5) | N4—C9—C10—O8 | −1.0 (4) |
N1—C2—C3—O2 | 178.5 (3) | C7—C9—C10—O8 | 178.4 (3) |
N1—C2—C4—N2 | 0.4 (3) | N4—C9—C10—O7 | 179.8 (2) |
C3—C2—C4—N2 | −178.7 (3) | C7—C9—C10—O7 | −0.8 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H2···O3 | 0.82 | 1.64 | 2.458 (3) | 179 |
O6—H6A···O7 | 0.82 | 1.63 | 2.450 (3) | 178 |
N2—H2A···O5i | 0.86 | 2.16 | 2.998 (3) | 164 |
N4—H4A···O8ii | 0.86 | 1.97 | 2.807 (3) | 164 |
O9—H9A···O12iii | 0.85 | 1.85 | 2.703 (3) | 178 |
O9—H9B···O8iv | 0.85 | 1.94 | 2.756 (3) | 160 |
O10—H10A···O7v | 0.85 | 2.00 | 2.851 (3) | 172 |
O10—H10B···O4vi | 0.85 | 1.91 | 2.727 (3) | 160 |
O11—H11B···O12vii | 0.85 | 1.95 | 2.793 (3) | 169 |
O12—H12A···O2viii | 0.85 | 2.09 | 2.929 (3) | 170 |
O12—H12B···O3ix | 0.85 | 1.98 | 2.833 (3) | 179 |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x−1, −y+2, −z; (iii) x, y, z−1; (iv) −x, −y+2, −z; (v) −x, y−1/2, −z+1/2; (vi) −x, y+1/2, −z+1/2; (vii) x, −y+3/2, z−1/2; (viii) x+1, y, z+1; (ix) −x, −y+1, −z+1. |
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