The title compound, {[Cd2(CH3COO)4(C10H8N2)2]·H2O}n, is a new metal-organic framework structure. The cadmium(II) ion has a distorted octahedral geometry. One of the acetate anions is coordinated to the metal atom in a bidentate chelating mode, whereas the other two anions act as bridges between adjacent CdII ions. The bipyridine ligands link the cadmium(II) ions, forming a ribbon structure. There is a centre of symmetry midway between the Cd atoms and a twofold rotation axis relating the pyridyl rings, and the water molecule also lies on a twofold rotation axis.
Supporting information
CCDC reference: 298390
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (C-C) = 0.004 Å
- R factor = 0.026
- wR factor = 0.066
- Data-to-parameter ratio = 16.2
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.54 Ratio
PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.05 Ratio
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O4
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C13
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.651 0.844
Tmin(prime) and Tmax expected: 0.727 0.844
RR(prime) = 0.895
Please check that your absorption correction is appropriate.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.88
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cd1
0 ALERT level A = In general: serious problem
4 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
5 ALERT type 2 Indicator that the structure model may be wrong or deficient
3 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); 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, 2000); software used to prepare material for publication: SHELXTL.
catena-poly[[[di-µ-acetato-1
κ2O:2
κ2O'-bis[(acetato-
κ2O,
O')cadmium(II)]]-di-µ-4,4'-bipyridine-1
κN:1'
κN';2
κN:2'
κN'] monohydrate]
top
Crystal data top
[Cd2(C2H3O2)4(C10H8N2)2]·H2O | F(000) = 1576 |
Mr = 791.36 | Dx = 1.680 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 4745 reflections |
a = 13.5069 (16) Å | θ = 2.3–26.3° |
b = 11.8393 (14) Å | µ = 1.42 mm−1 |
c = 19.570 (2) Å | T = 294 K |
β = 91.595 (2)° | Block, colourless |
V = 3128.3 (6) Å3 | 0.22 × 0.18 × 0.12 mm |
Z = 4 | |
Data collection top
Bruker SMART 1000 CCD area-detector diffractometer | 3179 independent reflections |
Radiation source: fine-focus sealed tube | 2644 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
φ and ω scans | θmax = 26.3°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −16→15 |
Tmin = 0.651, Tmax = 0.844 | k = −14→14 |
8593 measured reflections | l = −24→16 |
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)] = 0.026 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.066 | H-atom parameters constrained |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0298P)2 + 1.454P] where P = (Fo2 + 2Fc2)/3 |
3179 reflections | (Δ/σ)max = 0.003 |
196 parameters | Δρmax = 0.39 e Å−3 |
7 restraints | Δρmin = −0.57 e Å−3 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cd1 | 0.361587 (14) | 0.261628 (16) | 0.436865 (9) | 0.03581 (8) | |
O1 | 0.46488 (19) | 0.12487 (19) | 0.38714 (13) | 0.0694 (7) | |
O2 | 0.50050 (17) | 0.30036 (19) | 0.36705 (12) | 0.0604 (6) | |
O3 | 0.33853 (17) | 0.45491 (17) | 0.44932 (11) | 0.0547 (6) | |
O4 | 0.24072 (19) | 0.3737 (3) | 0.51944 (15) | 0.0896 (10) | |
N1 | 0.25343 (17) | 0.26728 (19) | 0.34155 (12) | 0.0390 (5) | |
N2 | −0.04043 (18) | 0.25185 (19) | 0.03632 (12) | 0.0409 (6) | |
C1 | 0.2013 (2) | 0.1756 (2) | 0.32236 (14) | 0.0401 (6) | |
H1 | 0.2049 | 0.1119 | 0.3501 | 0.048* | |
C2 | 0.14278 (19) | 0.1710 (2) | 0.26392 (13) | 0.0370 (6) | |
H2 | 0.1079 | 0.1055 | 0.2529 | 0.044* | |
C3 | 0.1359 (2) | 0.2649 (2) | 0.22110 (14) | 0.0336 (6) | |
C4 | 0.1890 (2) | 0.3602 (2) | 0.24127 (14) | 0.0422 (7) | |
H4 | 0.1860 | 0.4254 | 0.2148 | 0.051* | |
C5 | 0.2463 (2) | 0.3579 (2) | 0.30093 (14) | 0.0449 (7) | |
H5 | 0.2817 | 0.4224 | 0.3134 | 0.054* | |
C6 | 0.0752 (2) | 0.2618 (2) | 0.15718 (14) | 0.0344 (6) | |
C7 | 0.0617 (2) | 0.1613 (3) | 0.12142 (15) | 0.0474 (8) | |
H7 | 0.0912 | 0.0951 | 0.1375 | 0.057* | |
C8 | 0.0046 (2) | 0.1604 (3) | 0.06229 (15) | 0.0498 (8) | |
H8 | −0.0032 | 0.0923 | 0.0391 | 0.060* | |
C9 | −0.0267 (2) | 0.3484 (3) | 0.07039 (15) | 0.0446 (7) | |
H9 | −0.0569 | 0.4134 | 0.0531 | 0.054* | |
C10 | 0.0298 (2) | 0.3570 (2) | 0.12989 (15) | 0.0424 (7) | |
H10 | 0.0373 | 0.4265 | 0.1516 | 0.051* | |
C11 | 0.5189 (3) | 0.1973 (3) | 0.36134 (17) | 0.0542 (8) | |
C12 | 0.6080 (3) | 0.1607 (4) | 0.3227 (2) | 0.0993 (16) | |
H12A | 0.6291 | 0.0875 | 0.3385 | 0.149* | |
H12B | 0.6606 | 0.2141 | 0.3302 | 0.149* | |
H12C | 0.5911 | 0.1570 | 0.2748 | 0.149* | |
C13 | 0.2759 (2) | 0.4611 (3) | 0.49422 (15) | 0.0487 (8) | |
C14 | 0.2465 (4) | 0.5740 (5) | 0.5199 (3) | 0.119 (2) | |
H14A | 0.3039 | 0.6128 | 0.5378 | 0.178* | |
H14B | 0.1994 | 0.5650 | 0.5553 | 0.178* | |
H14C | 0.2171 | 0.6171 | 0.4830 | 0.178* | |
O5 | 1.0000 | 0.9433 (2) | 0.2500 | 0.0665 (9) | |
H5A | 1.0020 | 0.9066 | 0.2866 | 0.080* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.03397 (12) | 0.04627 (14) | 0.02703 (12) | −0.00666 (9) | −0.00193 (8) | 0.00197 (8) |
O1 | 0.0805 (17) | 0.0471 (13) | 0.0823 (18) | −0.0007 (12) | 0.0340 (14) | 0.0027 (12) |
O2 | 0.0668 (15) | 0.0477 (13) | 0.0680 (15) | −0.0009 (11) | 0.0241 (12) | 0.0035 (11) |
O3 | 0.0701 (15) | 0.0462 (12) | 0.0484 (13) | −0.0091 (10) | 0.0161 (11) | 0.0008 (9) |
O4 | 0.0653 (17) | 0.121 (3) | 0.0812 (19) | −0.0443 (16) | −0.0118 (14) | 0.0499 (18) |
N1 | 0.0398 (13) | 0.0460 (13) | 0.0307 (12) | −0.0061 (10) | −0.0065 (10) | −0.0019 (10) |
N2 | 0.0375 (13) | 0.0517 (15) | 0.0333 (13) | 0.0067 (10) | −0.0058 (10) | −0.0044 (10) |
C1 | 0.0421 (16) | 0.0423 (16) | 0.0358 (15) | −0.0044 (12) | −0.0035 (12) | 0.0024 (12) |
C2 | 0.0364 (15) | 0.0381 (15) | 0.0364 (15) | −0.0060 (11) | −0.0034 (12) | −0.0021 (11) |
C3 | 0.0319 (13) | 0.0394 (14) | 0.0294 (14) | 0.0022 (11) | 0.0004 (11) | −0.0049 (11) |
C4 | 0.0477 (17) | 0.0424 (16) | 0.0361 (16) | −0.0094 (13) | −0.0059 (13) | 0.0033 (12) |
C5 | 0.0498 (17) | 0.0451 (17) | 0.0393 (16) | −0.0167 (13) | −0.0088 (13) | −0.0003 (13) |
C6 | 0.0301 (13) | 0.0425 (15) | 0.0305 (14) | 0.0015 (11) | 0.0002 (11) | −0.0026 (11) |
C7 | 0.0510 (18) | 0.0465 (17) | 0.0438 (17) | 0.0198 (14) | −0.0161 (14) | −0.0144 (13) |
C8 | 0.0545 (19) | 0.0518 (18) | 0.0421 (17) | 0.0167 (15) | −0.0167 (14) | −0.0177 (14) |
C9 | 0.0454 (17) | 0.0438 (17) | 0.0440 (17) | 0.0028 (13) | −0.0095 (13) | 0.0041 (13) |
C10 | 0.0472 (17) | 0.0381 (15) | 0.0414 (16) | −0.0002 (12) | −0.0077 (13) | −0.0028 (12) |
C11 | 0.0542 (19) | 0.059 (2) | 0.0502 (19) | 0.0099 (16) | 0.0101 (15) | 0.0037 (16) |
C12 | 0.092 (3) | 0.094 (3) | 0.116 (4) | 0.025 (3) | 0.058 (3) | 0.015 (3) |
C13 | 0.0464 (18) | 0.059 (2) | 0.0400 (18) | −0.0105 (15) | −0.0061 (15) | 0.0095 (14) |
C14 | 0.135 (5) | 0.113 (4) | 0.110 (4) | 0.038 (3) | 0.034 (3) | −0.032 (3) |
O5 | 0.102 (3) | 0.0365 (17) | 0.061 (2) | 0.000 | 0.0001 (19) | 0.000 |
Geometric parameters (Å, º) top
Cd1—O4i | 2.296 (2) | C3—C6 | 1.476 (4) |
Cd1—O3 | 2.323 (2) | C4—C5 | 1.384 (4) |
Cd1—N2ii | 2.329 (2) | C4—H4 | 0.93 |
Cd1—N1 | 2.338 (2) | C5—H5 | 0.93 |
Cd1—O1 | 2.364 (2) | C6—C10 | 1.383 (4) |
Cd1—O2 | 2.396 (2) | C6—C7 | 1.390 (4) |
Cd1—C11 | 2.731 (3) | C7—C8 | 1.373 (4) |
O1—C11 | 1.242 (4) | C7—H7 | 0.93 |
O2—C11 | 1.251 (4) | C8—H8 | 0.93 |
O3—C13 | 1.238 (4) | C9—C10 | 1.378 (4) |
O4—C13 | 1.246 (4) | C9—H9 | 0.93 |
O4—Cd1i | 2.296 (2) | C10—H10 | 0.93 |
N1—C5 | 1.337 (4) | C11—C12 | 1.502 (5) |
N1—C1 | 1.342 (3) | C12—H12A | 0.96 |
N2—C9 | 1.333 (4) | C12—H12B | 0.96 |
N2—C8 | 1.336 (4) | C12—H12C | 0.96 |
N2—Cd1iii | 2.328 (2) | C13—C14 | 1.486 (6) |
C1—C2 | 1.373 (4) | C14—H14A | 0.96 |
C1—H1 | 0.93 | C14—H14B | 0.96 |
C2—C3 | 1.394 (4) | C14—H14C | 0.96 |
C2—H2 | 0.93 | O5—H5A | 0.84 |
C3—C4 | 1.388 (4) | | |
| | | |
O4i—Cd1—O3 | 124.35 (10) | C5—C4—H4 | 120.1 |
O4i—Cd1—N2ii | 88.56 (8) | C3—C4—H4 | 120.1 |
O3—Cd1—N2ii | 93.13 (8) | N1—C5—C4 | 123.1 (3) |
O4i—Cd1—N1 | 87.01 (8) | N1—C5—H5 | 118.4 |
O3—Cd1—N1 | 88.45 (8) | C4—C5—H5 | 118.4 |
N2ii—Cd1—N1 | 175.43 (8) | C10—C6—C7 | 116.9 (3) |
O4i—Cd1—O1 | 92.50 (12) | C10—C6—C3 | 122.5 (2) |
O3—Cd1—O1 | 143.14 (8) | C7—C6—C3 | 120.6 (2) |
N2ii—Cd1—O1 | 88.22 (9) | C8—C7—C6 | 119.6 (3) |
N1—Cd1—O1 | 93.10 (9) | C8—C7—H7 | 120.2 |
O4i—Cd1—O2 | 146.60 (11) | C6—C7—H7 | 120.2 |
O3—Cd1—O2 | 88.90 (8) | N2—C8—C7 | 123.6 (3) |
N2ii—Cd1—O2 | 93.09 (9) | N2—C8—H8 | 118.2 |
N1—Cd1—O2 | 91.23 (9) | C7—C8—H8 | 118.2 |
O1—Cd1—O2 | 54.26 (7) | N2—C9—C10 | 123.5 (3) |
O4i—Cd1—C11 | 119.50 (12) | N2—C9—H9 | 118.3 |
O3—Cd1—C11 | 116.12 (9) | C10—C9—H9 | 118.3 |
N2ii—Cd1—C11 | 90.03 (10) | C9—C10—C6 | 119.7 (3) |
N1—Cd1—C11 | 93.13 (9) | C9—C10—H10 | 120.1 |
O1—Cd1—C11 | 27.02 (9) | C6—C10—H10 | 120.1 |
O2—Cd1—C11 | 27.26 (9) | O1—C11—O2 | 121.1 (3) |
C11—O1—Cd1 | 93.15 (19) | O1—C11—C12 | 119.6 (3) |
C11—O2—Cd1 | 91.45 (18) | O2—C11—C12 | 119.4 (3) |
C13—O3—Cd1 | 103.2 (2) | O1—C11—Cd1 | 59.83 (17) |
C13—O4—Cd1i | 165.2 (3) | O2—C11—Cd1 | 61.29 (15) |
C5—N1—C1 | 117.0 (2) | C12—C11—Cd1 | 177.5 (3) |
C5—N1—Cd1 | 122.01 (18) | C11—C12—H12A | 109.5 |
C1—N1—Cd1 | 120.77 (18) | C11—C12—H12B | 109.5 |
C9—N2—C8 | 116.7 (3) | H12A—C12—H12B | 109.5 |
C9—N2—Cd1iii | 122.99 (19) | C11—C12—H12C | 109.5 |
C8—N2—Cd1iii | 120.31 (19) | H12A—C12—H12C | 109.5 |
N1—C1—C2 | 123.4 (3) | H12B—C12—H12C | 109.5 |
N1—C1—H1 | 118.3 | O3—C13—O4 | 120.5 (4) |
C2—C1—H1 | 118.3 | O3—C13—C14 | 119.1 (3) |
C1—C2—C3 | 119.8 (3) | O4—C13—C14 | 120.3 (4) |
C1—C2—H2 | 120.1 | C13—C14—H14A | 109.5 |
C3—C2—H2 | 120.1 | C13—C14—H14B | 109.5 |
C4—C3—C2 | 116.9 (3) | H14A—C14—H14B | 109.5 |
C4—C3—C6 | 122.1 (2) | C13—C14—H14C | 109.5 |
C2—C3—C6 | 121.0 (2) | H14A—C14—H14C | 109.5 |
C5—C4—C3 | 119.8 (3) | H14B—C14—H14C | 109.5 |
| | | |
O4i—Cd1—O1—C11 | 178.0 (2) | C1—C2—C3—C4 | −0.8 (4) |
O3—Cd1—O1—C11 | −0.7 (3) | C1—C2—C3—C6 | 178.7 (3) |
N2ii—Cd1—O1—C11 | −93.6 (2) | C2—C3—C4—C5 | 1.0 (4) |
N1—Cd1—O1—C11 | 90.8 (2) | C6—C3—C4—C5 | −178.6 (3) |
O2—Cd1—O1—C11 | 1.53 (19) | C1—N1—C5—C4 | −0.3 (4) |
O4i—Cd1—O2—C11 | −8.0 (3) | Cd1—N1—C5—C4 | 174.7 (2) |
O3—Cd1—O2—C11 | 177.13 (19) | C3—C4—C5—N1 | −0.4 (5) |
N2ii—Cd1—O2—C11 | 84.05 (19) | C4—C3—C6—C10 | −30.3 (4) |
N1—Cd1—O2—C11 | −94.45 (19) | C2—C3—C6—C10 | 150.1 (3) |
O1—Cd1—O2—C11 | −1.52 (19) | C4—C3—C6—C7 | 149.4 (3) |
O4i—Cd1—O3—C13 | 13.4 (2) | C2—C3—C6—C7 | −30.1 (4) |
N2ii—Cd1—O3—C13 | −77.0 (2) | C10—C6—C7—C8 | −0.6 (5) |
N1—Cd1—O3—C13 | 98.68 (19) | C3—C6—C7—C8 | 179.7 (3) |
O1—Cd1—O3—C13 | −168.22 (18) | C9—N2—C8—C7 | 0.8 (5) |
O2—Cd1—O3—C13 | −170.06 (19) | Cd1iii—N2—C8—C7 | −178.6 (2) |
C11—Cd1—O3—C13 | −168.59 (19) | C6—C7—C8—N2 | −0.3 (5) |
O4i—Cd1—N1—C5 | 156.2 (2) | C8—N2—C9—C10 | −0.5 (5) |
O3—Cd1—N1—C5 | 31.7 (2) | Cd1iii—N2—C9—C10 | 178.9 (2) |
O1—Cd1—N1—C5 | −111.4 (2) | N2—C9—C10—C6 | −0.3 (5) |
O2—Cd1—N1—C5 | −57.2 (2) | C7—C6—C10—C9 | 0.9 (4) |
C11—Cd1—N1—C5 | −84.4 (2) | C3—C6—C10—C9 | −179.4 (3) |
O4i—Cd1—N1—C1 | −29.0 (2) | Cd1—O1—C11—O2 | −2.8 (4) |
O3—Cd1—N1—C1 | −153.6 (2) | Cd1—O1—C11—C12 | 177.1 (3) |
O1—Cd1—N1—C1 | 63.3 (2) | Cd1—O2—C11—O1 | 2.7 (3) |
O2—Cd1—N1—C1 | 117.6 (2) | Cd1—O2—C11—C12 | −177.2 (3) |
C11—Cd1—N1—C1 | 90.4 (2) | Cd1—O3—C13—O4 | −1.4 (3) |
C5—N1—C1—C2 | 0.4 (4) | Cd1—O3—C13—C14 | 176.0 (3) |
Cd1—N1—C1—C2 | −174.6 (2) | Cd1i—O4—C13—O3 | −137.5 (10) |
N1—C1—C2—C3 | 0.2 (4) | Cd1i—O4—C13—C14 | 45.2 (12) |
Symmetry codes: (i) −x+1/2, −y+1/2, −z+1; (ii) x+1/2, −y+1/2, z+1/2; (iii) x−1/2, −y+1/2, z−1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5A···O2iv | 0.84 | 2.02 | 2.848 (3) | 172 |
Symmetry code: (iv) x+1/2, y+1/2, z. |