In the title compound, {[Co(C
8H
4O
5)(C
10H
8N
2)]·2H
2O]}
n or {[Co(OH-BDC)(2,2′-bipy)]·2H
2O]}
n (where OH-H
2BDC is 5-hydroxyisophthalic acid and 2,2′-bipy is 2,2′-bipyridine), the Co atoms are chelated by two N atoms from the 2,2′-bipy ligand and by four O atoms from OH-BDC ligands in a highly distorted octahedral geometry. OH-BDC acts as a tetradentate ligand, with one carboxylate group chelating one Co atom and the other binding in a monodentate fashion to two other Co atoms to form a one-dimensional zigzag chain. In the crystal structure, one of the solvent water molecules lies on a crystallographic twofold axis. The one-dimensional molecular chains are assembled into a two-dimensional network
via O—H
O hydrogen-bonding interactions, while π–π stacking interactions generate a three-dimensional open framework between the two-dimensional networks.
Supporting information
CCDC reference: 613826
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.005 Å
- Disorder in solvent or counterion
- R factor = 0.054
- wR factor = 0.131
- Data-to-parameter ratio = 14.1
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.25 Ratio
PLAT128_ALERT_4_C Non-standard setting of Space group P2/c .... P2/n
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 17.00 Perc.
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
6 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 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
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2000); software used to prepare material for publication: SHELXTL.
Poly[[[(2,2'-bipyridine-
κ2N:
N')cobalt(II)]-µ
3-5-hydroxyisophthalato- k
4O,
O':
O'':
O'''] dihydrate]
top
Crystal data top
[Co(C8H4O5)(C10H8N2)]·2H2O] | F(000) = 884 |
Mr = 431.26 | Dx = 1.540 Mg m−3 |
Monoclinic, P2/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yac | Cell parameters from 994 reflections |
a = 10.917 (3) Å | θ = 2.1–26.0° |
b = 11.530 (3) Å | µ = 0.97 mm−1 |
c = 15.079 (5) Å | T = 298 K |
β = 101.473 (5)° | Block, red |
V = 1860 (1) Å3 | 0.32 × 0.28 × 0.26 mm |
Z = 4 | |
Data collection top
Bruker SMART APEX CCD area-detector diffractometer | 3643 independent reflections |
Radiation source: fine-focus sealed tube | 2931 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
φ and ω scans | θmax = 26.0°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2000) | h = −13→13 |
Tmin = 0.747, Tmax = 0.787 | k = −14→13 |
9780 measured reflections | l = −9→18 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.054 | H-atom parameters constrained |
wR(F2) = 0.131 | w = 1/[σ2(Fo2) + (0.0615P)2 + 2.1186P] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max < 0.001 |
3643 reflections | Δρmax = 0.26 e Å−3 |
258 parameters | Δρmin = −0.41 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997) |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.003 |
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 | Occ. (<1) |
C1 | 0.3308 (3) | 0.8366 (3) | 0.4921 (2) | 0.0387 (8) | |
H1 | 0.3238 | 0.7605 | 0.5109 | 0.046* | |
C2 | 0.3037 (4) | 0.9259 (4) | 0.5470 (3) | 0.0476 (9) | |
H2 | 0.2790 | 0.9102 | 0.6013 | 0.057* | |
C3 | 0.3144 (4) | 1.0375 (4) | 0.5187 (3) | 0.0489 (10) | |
H3 | 0.2986 | 1.0994 | 0.5544 | 0.059* | |
C4 | 0.3487 (4) | 1.0575 (3) | 0.4371 (3) | 0.0450 (9) | |
H4 | 0.3540 | 1.1329 | 0.4163 | 0.054* | |
C5 | 0.3753 (3) | 0.9644 (3) | 0.3861 (3) | 0.0391 (8) | |
C6 | 0.4143 (3) | 0.9743 (3) | 0.2981 (2) | 0.0351 (7) | |
C7 | 0.4454 (3) | 1.0775 (3) | 0.2625 (2) | 0.0376 (8) | |
H7 | 0.4418 | 1.1467 | 0.2935 | 0.045* | |
C8 | 0.4817 (3) | 1.0767 (3) | 0.1807 (3) | 0.0426 (9) | |
H8 | 0.5018 | 1.1457 | 0.1551 | 0.051* | |
C9 | 0.4881 (4) | 0.9743 (3) | 0.1373 (3) | 0.0487 (10) | |
H9 | 0.5126 | 0.9723 | 0.0817 | 0.058* | |
C10 | 0.4579 (4) | 0.8742 (4) | 0.1767 (3) | 0.0456 (9) | |
H10 | 0.4631 | 0.8042 | 0.1469 | 0.055* | |
C11 | 0.3454 (3) | 0.5831 (3) | 0.1752 (2) | 0.0394 (8) | |
C12 | 0.3467 (3) | 0.4890 (3) | 0.1082 (2) | 0.0357 (7) | |
C13 | 0.2379 (3) | 0.4599 (3) | 0.0492 (2) | 0.0378 (8) | |
H13 | 0.1644 | 0.4995 | 0.0516 | 0.045* | |
C14 | 0.2370 (4) | 0.3725 (3) | −0.0132 (3) | 0.0434 (9) | |
C15 | 0.1178 (3) | 0.3354 (3) | −0.0729 (2) | 0.0326 (7) | |
C16 | 0.3484 (3) | 0.3163 (3) | −0.0195 (2) | 0.0349 (7) | |
H16 | 0.3488 | 0.2597 | −0.0634 | 0.042* | |
C17 | 0.4597 (3) | 0.3453 (3) | 0.0403 (2) | 0.0392 (8) | |
C18 | 0.4589 (3) | 0.4304 (3) | 0.1052 (2) | 0.0336 (7) | |
H18 | 0.5318 | 0.4486 | 0.1463 | 0.040* | |
Co1 | 0.40672 (5) | 0.72064 (4) | 0.33049 (3) | 0.04107 (17) | |
N1 | 0.3659 (3) | 0.8548 (3) | 0.41472 (19) | 0.0386 (7) | |
N2 | 0.4213 (3) | 0.8727 (2) | 0.2563 (2) | 0.0375 (7) | |
O1 | 0.2651 (2) | 0.6611 (2) | 0.15602 (16) | 0.0383 (6) | |
O2 | 0.4277 (2) | 0.5842 (2) | 0.24745 (15) | 0.0340 (5) | |
O3 | 0.0155 (2) | 0.3618 (2) | −0.05048 (16) | 0.0387 (6) | |
O4 | 0.1178 (2) | 0.27619 (19) | −0.14217 (15) | 0.0340 (5) | |
O5 | 0.5646 (2) | 0.2872 (2) | 0.03121 (18) | 0.0461 (6) | |
H5 | 0.6176 | 0.2935 | 0.0779 | 0.055* | |
O6 | 0.2500 | 0.4179 (3) | 0.7500 | 0.0443 (9) | |
H6A | 0.2013 | 0.3829 | 0.7786 | 0.053* | |
O7 | 0.5012 (3) | 0.3685 (3) | 0.3576 (2) | 0.0601 (8) | |
H7A | 0.5007 | 0.3850 | 0.4125 | 0.072* | |
H7B | 0.4683 | 0.4237 | 0.3237 | 0.072* | |
O8 | 0.7394 (4) | 0.3391 (5) | 0.3372 (3) | 0.0430 (12) | 0.50 |
H8A | 0.6561 | 0.3121 | 0.3346 | 0.052* | 0.50 |
H8B | 0.7581 | 0.3780 | 0.2852 | 0.052* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0404 (19) | 0.0362 (18) | 0.042 (2) | −0.0046 (15) | 0.0134 (16) | −0.0054 (15) |
C2 | 0.044 (2) | 0.054 (2) | 0.049 (2) | −0.0047 (18) | 0.0165 (18) | −0.0177 (19) |
C3 | 0.048 (2) | 0.048 (2) | 0.053 (2) | 0.0027 (18) | 0.0168 (19) | −0.0144 (19) |
C4 | 0.057 (2) | 0.0313 (18) | 0.044 (2) | 0.0017 (17) | 0.0031 (18) | −0.0113 (16) |
C5 | 0.0269 (16) | 0.0406 (19) | 0.047 (2) | −0.0012 (14) | 0.0007 (15) | −0.0051 (16) |
C6 | 0.0342 (17) | 0.0261 (16) | 0.0409 (18) | −0.0042 (13) | −0.0027 (14) | 0.0051 (14) |
C7 | 0.0415 (19) | 0.0283 (16) | 0.0392 (19) | −0.0092 (14) | −0.0012 (15) | 0.0137 (14) |
C8 | 0.0398 (19) | 0.045 (2) | 0.045 (2) | −0.0200 (16) | 0.0129 (16) | 0.0159 (17) |
C9 | 0.047 (2) | 0.050 (2) | 0.051 (2) | −0.0123 (18) | 0.0139 (18) | 0.0230 (19) |
C10 | 0.048 (2) | 0.051 (2) | 0.039 (2) | −0.0047 (18) | 0.0128 (17) | 0.0093 (17) |
C11 | 0.0409 (19) | 0.045 (2) | 0.0332 (18) | −0.0052 (16) | 0.0085 (16) | −0.0006 (15) |
C12 | 0.0414 (19) | 0.0387 (18) | 0.0265 (16) | −0.0004 (15) | 0.0058 (14) | 0.0030 (14) |
C13 | 0.0419 (19) | 0.0419 (19) | 0.0301 (17) | 0.0023 (15) | 0.0084 (15) | 0.0029 (15) |
C14 | 0.041 (2) | 0.046 (2) | 0.042 (2) | 0.0010 (16) | 0.0039 (16) | 0.0046 (17) |
C15 | 0.0278 (16) | 0.0439 (19) | 0.0255 (16) | −0.0005 (14) | 0.0035 (13) | 0.0031 (14) |
C16 | 0.0348 (17) | 0.0418 (18) | 0.0284 (16) | 0.0045 (14) | 0.0071 (14) | −0.0025 (14) |
C17 | 0.0417 (19) | 0.044 (2) | 0.0320 (17) | 0.0031 (16) | 0.0084 (15) | 0.0011 (15) |
C18 | 0.0415 (18) | 0.0277 (16) | 0.0305 (17) | 0.0030 (14) | 0.0044 (14) | 0.0023 (13) |
Co1 | 0.0413 (3) | 0.0372 (3) | 0.0431 (3) | −0.0003 (2) | 0.0045 (2) | −0.0002 (2) |
N1 | 0.0420 (17) | 0.0430 (17) | 0.0304 (15) | −0.0035 (13) | 0.0059 (13) | −0.0028 (13) |
N2 | 0.0431 (16) | 0.0300 (14) | 0.0367 (16) | −0.0002 (12) | 0.0015 (13) | 0.0052 (12) |
O1 | 0.0309 (12) | 0.0459 (14) | 0.0389 (13) | 0.0096 (11) | 0.0090 (10) | −0.0003 (11) |
O2 | 0.0310 (12) | 0.0345 (12) | 0.0322 (12) | 0.0056 (9) | −0.0039 (10) | −0.0109 (10) |
O3 | 0.0399 (14) | 0.0326 (12) | 0.0411 (14) | 0.0022 (10) | 0.0021 (11) | −0.0055 (10) |
O4 | 0.0347 (12) | 0.0345 (12) | 0.0318 (12) | −0.0015 (10) | 0.0042 (10) | −0.0106 (10) |
O5 | 0.0419 (14) | 0.0470 (15) | 0.0490 (15) | 0.0117 (12) | 0.0078 (12) | −0.0133 (12) |
O6 | 0.045 (2) | 0.049 (2) | 0.044 (2) | 0.000 | 0.0230 (17) | 0.000 |
O7 | 0.0657 (19) | 0.0593 (18) | 0.0564 (18) | 0.0191 (15) | 0.0151 (15) | −0.0039 (14) |
O8 | 0.034 (2) | 0.060 (3) | 0.038 (3) | 0.007 (2) | 0.013 (2) | 0.009 (2) |
Geometric parameters (Å, º) top
C1—N1 | 1.315 (4) | C13—C14 | 1.378 (5) |
C1—C2 | 1.389 (5) | C13—H13 | 0.9300 |
C1—H1 | 0.9300 | C14—C16 | 1.398 (5) |
C2—C3 | 1.368 (6) | C14—C15 | 1.490 (5) |
C2—H2 | 0.9300 | C15—O4 | 1.248 (4) |
C3—C4 | 1.375 (6) | C15—O3 | 1.267 (4) |
C3—H3 | 0.9300 | C16—C17 | 1.403 (5) |
C4—C5 | 1.385 (5) | C16—H16 | 0.9300 |
C4—H4 | 0.9300 | C17—O5 | 1.358 (4) |
C5—N1 | 1.345 (5) | C17—C18 | 1.386 (5) |
C5—C6 | 1.476 (5) | C18—H18 | 0.9300 |
C6—N2 | 1.340 (4) | Co1—O1i | 2.045 (2) |
C6—C7 | 1.375 (4) | Co1—O2 | 2.052 (2) |
C7—C8 | 1.368 (5) | Co1—N2 | 2.102 (3) |
C7—H7 | 0.9300 | Co1—N1 | 2.105 (3) |
C8—C9 | 1.358 (6) | Co1—O3ii | 2.165 (2) |
C8—H8 | 0.9300 | Co1—O4ii | 2.259 (2) |
C9—C10 | 1.368 (5) | O1—Co1i | 2.045 (2) |
C9—H9 | 0.9300 | O3—Co1iii | 2.165 (2) |
C10—N2 | 1.339 (5) | O4—Co1iii | 2.259 (2) |
C10—H10 | 0.9300 | O5—H5 | 0.8200 |
C11—O1 | 1.249 (4) | O6—H6A | 0.8500 |
C11—O2 | 1.267 (4) | O7—H7A | 0.8501 |
C11—C12 | 1.485 (5) | O7—H7B | 0.8499 |
C12—C13 | 1.376 (5) | O8—H8A | 0.9543 |
C12—C18 | 1.407 (5) | O8—H8B | 0.9600 |
| | | |
N1—C1—C2 | 123.0 (4) | C16—C14—C15 | 119.6 (3) |
N1—C1—H1 | 118.5 | O4—C15—O3 | 120.1 (3) |
C2—C1—H1 | 118.5 | O4—C15—C14 | 121.1 (3) |
C3—C2—C1 | 118.0 (4) | O3—C15—C14 | 118.7 (3) |
C3—C2—H2 | 121.0 | C14—C16—C17 | 120.0 (3) |
C1—C2—H2 | 121.0 | C14—C16—H16 | 120.0 |
C2—C3—C4 | 119.4 (4) | C17—C16—H16 | 120.0 |
C2—C3—H3 | 120.3 | O5—C17—C18 | 123.0 (3) |
C4—C3—H3 | 120.3 | O5—C17—C16 | 117.2 (3) |
C3—C4—C5 | 119.5 (4) | C18—C17—C16 | 119.8 (3) |
C3—C4—H4 | 120.3 | C17—C18—C12 | 119.3 (3) |
C5—C4—H4 | 120.3 | C17—C18—H18 | 120.3 |
N1—C5—C4 | 120.8 (4) | C12—C18—H18 | 120.3 |
N1—C5—C6 | 114.6 (3) | O1i—Co1—O2 | 91.12 (10) |
C4—C5—C6 | 124.7 (3) | O1i—Co1—N2 | 120.04 (11) |
N2—C6—C7 | 122.1 (3) | O2—Co1—N2 | 106.59 (11) |
N2—C6—C5 | 114.1 (3) | O1i—Co1—N1 | 83.01 (11) |
C7—C6—C5 | 123.8 (3) | O2—Co1—N1 | 174.06 (11) |
C8—C7—C6 | 119.0 (4) | N2—Co1—N1 | 75.85 (12) |
C8—C7—H7 | 120.5 | O1i—Co1—O3ii | 97.63 (10) |
C6—C7—H7 | 120.5 | O2—Co1—O3ii | 93.44 (9) |
C9—C8—C7 | 119.4 (3) | N2—Co1—O3ii | 136.06 (10) |
C9—C8—H8 | 120.3 | N1—Co1—O3ii | 88.24 (11) |
C7—C8—H8 | 120.3 | O1i—Co1—O4ii | 155.47 (9) |
C8—C9—C10 | 119.0 (4) | O2—Co1—O4ii | 83.68 (9) |
C8—C9—H9 | 120.5 | N2—Co1—O4ii | 84.33 (10) |
C10—C9—H9 | 120.5 | N1—Co1—O4ii | 102.04 (10) |
N2—C10—C9 | 122.7 (4) | O3ii—Co1—O4ii | 58.97 (9) |
N2—C10—H10 | 118.6 | C1—N1—C5 | 119.3 (3) |
C9—C10—H10 | 118.6 | C1—N1—Co1 | 123.5 (2) |
O1—C11—O2 | 122.5 (3) | C5—N1—Co1 | 117.2 (2) |
O1—C11—C12 | 118.0 (3) | C10—N2—C6 | 117.7 (3) |
O2—C11—C12 | 119.4 (3) | C10—N2—Co1 | 123.7 (3) |
C13—C12—C18 | 120.5 (3) | C6—N2—Co1 | 117.5 (2) |
C13—C12—C11 | 119.6 (3) | C11—O1—Co1i | 146.5 (2) |
C18—C12—C11 | 119.9 (3) | C11—O2—Co1 | 112.7 (2) |
C12—C13—C14 | 120.5 (3) | C15—O3—Co1iii | 92.3 (2) |
C12—C13—H13 | 119.8 | C15—O4—Co1iii | 88.49 (19) |
C14—C13—H13 | 119.8 | C17—O5—H5 | 109.5 |
C13—C14—C16 | 119.8 (3) | H7A—O7—H7B | 109.5 |
C13—C14—C15 | 120.6 (3) | H8A—O8—H8B | 118.2 |
Symmetry codes: (i) −x+1/2, y, −z+1/2; (ii) x+1/2, −y+1, z+1/2; (iii) x−1/2, −y+1, z−1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O8—H8B···O6iv | 0.96 | 2.41 | 3.107 (6) | 129 |
O8—H8A···O7 | 0.95 | 1.91 | 2.701 (5) | 139 |
O7—H7B···O2 | 0.85 | 2.18 | 3.009 (4) | 166 |
O7—H7A···O3i | 0.85 | 2.14 | 2.951 (4) | 159 |
O6—H6A···O4v | 0.85 | 2.05 | 2.886 (3) | 167 |
O8—H8B···O8vi | 0.96 | 1.91 | 2.686 (10) | 137 |
O5—H5···O8vi | 0.82 | 1.89 | 2.680 (6) | 163 |
Symmetry codes: (i) −x+1/2, y, −z+1/2; (iv) −x+1, −y+1, −z+1; (v) x, y, z+1; (vi) −x+3/2, y, −z+1/2. |