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In the title complex, [Co(C
4O
4)(C
12H
8N
2)(H
2O)
2]
n, the Co
II atom exhibits a slightly distorted octahedral coordination geometry involving two N atoms from 1,10-phenanthroline, two O atoms from two acetylenedicarboxylate (ace
2−) dianions and two water O atoms. The ace
2− ligand acts in a bis-monodentate mode to connect two adjacent Co
II atoms, forming chains along the
b axis. A three-dimensional supramolecular architecture is constructed
via O—H
O hydrogen bonds and π–π interactions.
Supporting information
CCDC reference: 628040
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.003 Å
- R factor = 0.026
- wR factor = 0.069
- Data-to-parameter ratio = 16.0
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT371_ALERT_2_C Long C(sp2)-C(sp1) Bond C13 - C14 ... 1.47 Ang.
PLAT371_ALERT_2_C Long C(sp2)-C(sp1) Bond C15 - C16 ... 1.47 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 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
0 ALERT type 5 Informative message, check
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
catena-Poly[[diaqua(1,10-phenanthroline-
κ2N,
N')cobalt(II)]- µ-acetylenedicarboxylato-
κ2O:
O']
top
Crystal data top
[Co(C4O4)(C12H8N2)(H2O)2] | F(000) = 1576 |
Mr = 387.21 | Dx = 1.550 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 22452 reflections |
a = 13.496 (3) Å | θ = 3.0–27.5° |
b = 9.5681 (19) Å | µ = 1.07 mm−1 |
c = 25.706 (5) Å | T = 295 K |
V = 3319.5 (11) Å3 | Prism, red |
Z = 8 | 0.25 × 0.20 × 0.15 mm |
Data collection top
Rigaku R-AXIS RAPID area-detector diffractometer | 3797 independent reflections |
Radiation source: fine-focus sealed tube | 3128 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
Detector resolution: 10.000 pixels mm-1 | θmax = 27.5°, θmin = 3.0° |
ω scans | h = −17→17 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −11→12 |
Tmin = 0.776, Tmax = 0.856 | l = −33→32 |
30566 measured reflections | |
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) = 0.070 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0344P)2 + 1.0761P] where P = (Fo2 + 2Fc2)/3 |
3797 reflections | (Δ/σ)max = 0.001 |
238 parameters | Δρmax = 0.24 e Å−3 |
6 restraints | Δρmin = −0.23 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 | |
Co1 | 0.467068 (14) | 0.22567 (2) | 0.637350 (7) | 0.02296 (7) | |
O1W | 0.43620 (10) | 0.24640 (12) | 0.71676 (4) | 0.0357 (3) | |
H1W1 | 0.4551 (15) | 0.1698 (11) | 0.7298 (7) | 0.054* | |
H1W2 | 0.4628 (14) | 0.3148 (13) | 0.7318 (7) | 0.054* | |
O2W | 0.31968 (9) | 0.22338 (12) | 0.61176 (5) | 0.0365 (3) | |
H2W1 | 0.2849 (14) | 0.1579 (14) | 0.6245 (8) | 0.055* | |
H2W2 | 0.2958 (15) | 0.3021 (11) | 0.6198 (8) | 0.055* | |
O1 | 0.46593 (8) | 0.44249 (12) | 0.63445 (4) | 0.0328 (3) | |
O2 | 0.30514 (10) | 0.49898 (14) | 0.63282 (7) | 0.0589 (4) | |
O3 | 0.47544 (11) | 0.96246 (12) | 0.72848 (4) | 0.0470 (3) | |
O4 | 0.45049 (9) | 1.01074 (12) | 0.64412 (4) | 0.0343 (3) | |
N1 | 0.62239 (10) | 0.18997 (15) | 0.65123 (5) | 0.0339 (3) | |
N2 | 0.52484 (10) | 0.20115 (14) | 0.56077 (5) | 0.0306 (3) | |
C1 | 0.66868 (14) | 0.1810 (3) | 0.69653 (8) | 0.0531 (5) | |
H1 | 0.6374 | 0.2162 | 0.7260 | 0.064* | |
C2 | 0.76235 (17) | 0.1210 (3) | 0.70211 (9) | 0.0711 (7) | |
H2 | 0.7915 | 0.1146 | 0.7348 | 0.085* | |
C3 | 0.81076 (15) | 0.0720 (3) | 0.65950 (10) | 0.0637 (6) | |
H3 | 0.8736 | 0.0330 | 0.6627 | 0.076* | |
C4 | 0.76498 (13) | 0.0806 (2) | 0.61045 (8) | 0.0470 (5) | |
C5 | 0.80941 (16) | 0.0324 (2) | 0.56306 (9) | 0.0604 (6) | |
H5 | 0.8723 | −0.0073 | 0.5640 | 0.072* | |
C6 | 0.76210 (17) | 0.0435 (2) | 0.51723 (9) | 0.0601 (6) | |
H6 | 0.7929 | 0.0115 | 0.4872 | 0.072* | |
C7 | 0.66494 (15) | 0.1038 (2) | 0.51375 (7) | 0.0446 (4) | |
C8 | 0.61162 (18) | 0.1192 (2) | 0.46738 (7) | 0.0564 (6) | |
H8 | 0.6398 | 0.0922 | 0.4359 | 0.068* | |
C9 | 0.51913 (19) | 0.1733 (3) | 0.46842 (7) | 0.0578 (6) | |
H9 | 0.4837 | 0.1845 | 0.4377 | 0.069* | |
C10 | 0.47671 (15) | 0.2124 (2) | 0.51609 (7) | 0.0445 (4) | |
H10 | 0.4124 | 0.2475 | 0.5163 | 0.053* | |
C11 | 0.61817 (12) | 0.14956 (16) | 0.55971 (6) | 0.0319 (3) | |
C12 | 0.66996 (12) | 0.14017 (17) | 0.60844 (6) | 0.0333 (4) | |
C13 | 0.39424 (12) | 0.52396 (16) | 0.64031 (6) | 0.0311 (3) | |
C14 | 0.41926 (12) | 0.66609 (16) | 0.65760 (6) | 0.0318 (3) | |
C15 | 0.43759 (13) | 0.78293 (16) | 0.67008 (6) | 0.0326 (3) | |
C16 | 0.45650 (12) | 0.93090 (16) | 0.68240 (6) | 0.0303 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.02359 (11) | 0.01786 (11) | 0.02744 (11) | 0.00062 (7) | −0.00130 (8) | −0.00184 (7) |
O1W | 0.0493 (7) | 0.0273 (6) | 0.0304 (6) | −0.0022 (5) | 0.0023 (5) | −0.0041 (5) |
O2W | 0.0269 (6) | 0.0253 (6) | 0.0572 (8) | −0.0027 (5) | −0.0045 (5) | −0.0014 (5) |
O1 | 0.0269 (6) | 0.0198 (5) | 0.0519 (7) | −0.0013 (4) | −0.0006 (5) | −0.0018 (5) |
O2 | 0.0301 (7) | 0.0251 (6) | 0.1215 (13) | 0.0029 (5) | −0.0109 (7) | −0.0117 (7) |
O3 | 0.0852 (10) | 0.0255 (6) | 0.0302 (6) | −0.0007 (6) | −0.0130 (6) | −0.0009 (5) |
O4 | 0.0536 (7) | 0.0187 (5) | 0.0307 (5) | −0.0013 (5) | −0.0077 (5) | 0.0008 (4) |
N1 | 0.0264 (7) | 0.0405 (8) | 0.0348 (7) | 0.0023 (6) | −0.0029 (5) | −0.0058 (6) |
N2 | 0.0359 (7) | 0.0286 (7) | 0.0273 (6) | −0.0007 (5) | −0.0003 (5) | 0.0012 (5) |
C1 | 0.0354 (10) | 0.0817 (15) | 0.0421 (10) | 0.0054 (10) | −0.0104 (8) | −0.0124 (10) |
C2 | 0.0405 (12) | 0.113 (2) | 0.0595 (13) | 0.0140 (13) | −0.0212 (10) | −0.0101 (13) |
C3 | 0.0281 (10) | 0.0805 (17) | 0.0824 (15) | 0.0125 (10) | −0.0110 (10) | −0.0006 (13) |
C4 | 0.0282 (9) | 0.0475 (11) | 0.0652 (12) | 0.0044 (8) | 0.0055 (8) | −0.0058 (9) |
C5 | 0.0364 (11) | 0.0623 (14) | 0.0824 (16) | 0.0112 (10) | 0.0189 (11) | −0.0114 (12) |
C6 | 0.0519 (13) | 0.0629 (14) | 0.0657 (13) | −0.0005 (10) | 0.0314 (11) | −0.0199 (11) |
C7 | 0.0497 (11) | 0.0426 (10) | 0.0415 (9) | −0.0093 (8) | 0.0144 (8) | −0.0083 (8) |
C8 | 0.0693 (15) | 0.0670 (14) | 0.0330 (9) | −0.0161 (12) | 0.0156 (9) | −0.0090 (9) |
C9 | 0.0750 (16) | 0.0723 (15) | 0.0261 (9) | −0.0142 (12) | −0.0017 (9) | 0.0026 (9) |
C10 | 0.0493 (11) | 0.0512 (12) | 0.0329 (9) | −0.0016 (9) | −0.0057 (8) | 0.0070 (8) |
C11 | 0.0342 (9) | 0.0268 (8) | 0.0347 (8) | −0.0028 (6) | 0.0080 (6) | −0.0030 (6) |
C12 | 0.0268 (8) | 0.0310 (8) | 0.0420 (9) | 0.0005 (6) | 0.0035 (6) | −0.0050 (7) |
C13 | 0.0318 (8) | 0.0196 (7) | 0.0419 (8) | −0.0005 (6) | −0.0021 (7) | 0.0010 (6) |
C14 | 0.0351 (9) | 0.0232 (8) | 0.0373 (8) | 0.0020 (6) | −0.0016 (7) | 0.0005 (6) |
C15 | 0.0475 (9) | 0.0217 (8) | 0.0287 (7) | 0.0004 (7) | −0.0022 (7) | 0.0017 (6) |
C16 | 0.0384 (9) | 0.0197 (7) | 0.0329 (8) | 0.0006 (6) | −0.0026 (6) | −0.0010 (6) |
Geometric parameters (Å, º) top
Co1—O4i | 2.0760 (12) | C2—C3 | 1.359 (3) |
Co1—O1 | 2.0760 (12) | C2—H2 | 0.9300 |
Co1—O1W | 2.0927 (12) | C3—C4 | 1.407 (3) |
Co1—O2W | 2.0952 (12) | C3—H3 | 0.9300 |
Co1—N2 | 2.1303 (14) | C4—C12 | 1.404 (2) |
Co1—N1 | 2.1537 (14) | C4—C5 | 1.434 (3) |
O1W—H1W1 | 0.845 (9) | C5—C6 | 1.344 (3) |
O1W—H1W2 | 0.841 (9) | C5—H5 | 0.9300 |
O2W—H2W1 | 0.848 (9) | C6—C7 | 1.435 (3) |
O2W—H2W2 | 0.845 (9) | C6—H6 | 0.9300 |
O1—C13 | 1.2515 (19) | C7—C8 | 1.400 (3) |
O2—C13 | 1.241 (2) | C7—C11 | 1.409 (2) |
O3—C16 | 1.2490 (19) | C8—C9 | 1.352 (3) |
O4—C16 | 1.2483 (18) | C8—H8 | 0.9300 |
O4—Co1ii | 2.0760 (12) | C9—C10 | 1.403 (3) |
N1—C1 | 1.324 (2) | C9—H9 | 0.9300 |
N1—C12 | 1.360 (2) | C10—H10 | 0.9300 |
N2—C10 | 1.324 (2) | C11—C12 | 1.437 (2) |
N2—C11 | 1.353 (2) | C13—C14 | 1.470 (2) |
C1—C2 | 1.396 (3) | C14—C15 | 1.189 (2) |
C1—H1 | 0.9300 | C15—C16 | 1.473 (2) |
| | | |
O4i—Co1—O1 | 172.83 (5) | C4—C3—H3 | 120.3 |
O4i—Co1—O1W | 89.46 (4) | C12—C4—C3 | 117.25 (18) |
O1—Co1—O1W | 86.49 (5) | C12—C4—C5 | 118.77 (18) |
O4i—Co1—O2W | 85.05 (5) | C3—C4—C5 | 123.98 (19) |
O1—Co1—O2W | 89.55 (4) | C6—C5—C4 | 121.37 (19) |
O1W—Co1—O2W | 96.79 (5) | C6—C5—H5 | 119.3 |
O4i—Co1—N2 | 90.45 (5) | C4—C5—H5 | 119.3 |
O1—Co1—N2 | 94.56 (5) | C5—C6—C7 | 121.35 (18) |
O1W—Co1—N2 | 169.94 (5) | C5—C6—H6 | 119.3 |
O2W—Co1—N2 | 93.23 (5) | C7—C6—H6 | 119.3 |
O4i—Co1—N1 | 86.21 (5) | C8—C7—C11 | 116.80 (19) |
O1—Co1—N1 | 99.89 (5) | C8—C7—C6 | 124.39 (18) |
O1W—Co1—N1 | 92.71 (5) | C11—C7—C6 | 118.80 (18) |
O2W—Co1—N1 | 167.01 (5) | C9—C8—C7 | 119.87 (18) |
N2—Co1—N1 | 77.25 (5) | C9—C8—H8 | 120.1 |
Co1—O1W—H1W1 | 104.2 (14) | C7—C8—H8 | 120.1 |
Co1—O1W—H1W2 | 115.9 (14) | C8—C9—C10 | 119.75 (19) |
H1W1—O1W—H1W2 | 111.4 (14) | C8—C9—H9 | 120.1 |
Co1—O2W—H2W1 | 114.3 (15) | C10—C9—H9 | 120.1 |
Co1—O2W—H2W2 | 106.0 (15) | N2—C10—C9 | 122.39 (19) |
H2W1—O2W—H2W2 | 110.8 (14) | N2—C10—H10 | 118.8 |
C13—O1—Co1 | 128.60 (10) | C9—C10—H10 | 118.8 |
C16—O4—Co1ii | 131.70 (10) | N2—C11—C7 | 123.18 (16) |
C1—N1—C12 | 117.76 (15) | N2—C11—C12 | 117.24 (14) |
C1—N1—Co1 | 127.96 (13) | C7—C11—C12 | 119.57 (16) |
C12—N1—Co1 | 112.40 (10) | N1—C12—C4 | 122.94 (16) |
C10—N2—C11 | 117.96 (15) | N1—C12—C11 | 116.97 (14) |
C10—N2—Co1 | 127.81 (13) | C4—C12—C11 | 120.09 (15) |
C11—N2—Co1 | 113.55 (10) | O2—C13—O1 | 127.61 (15) |
N1—C1—C2 | 122.98 (19) | O2—C13—C14 | 116.60 (15) |
N1—C1—H1 | 118.5 | O1—C13—C14 | 115.79 (14) |
C2—C1—H1 | 118.5 | C15—C14—C13 | 177.60 (18) |
C3—C2—C1 | 119.6 (2) | C14—C15—C16 | 176.09 (17) |
C3—C2—H2 | 120.2 | O4—C16—O3 | 127.81 (15) |
C1—C2—H2 | 120.2 | O4—C16—C15 | 114.04 (13) |
C2—C3—C4 | 119.41 (19) | O3—C16—C15 | 118.15 (14) |
C2—C3—H3 | 120.3 | | |
| | | |
O1W—Co1—O1—C13 | −68.00 (13) | C5—C6—C7—C8 | 179.7 (2) |
O2W—Co1—O1—C13 | 28.83 (13) | C5—C6—C7—C11 | −1.2 (3) |
N2—Co1—O1—C13 | 122.03 (13) | C11—C7—C8—C9 | −1.3 (3) |
N1—Co1—O1—C13 | −160.14 (13) | C6—C7—C8—C9 | 177.9 (2) |
O4i—Co1—N1—C1 | −86.59 (18) | C7—C8—C9—C10 | −0.6 (3) |
O1—Co1—N1—C1 | 89.60 (18) | C11—N2—C10—C9 | −0.2 (3) |
O1W—Co1—N1—C1 | 2.69 (18) | Co1—N2—C10—C9 | −170.09 (15) |
O2W—Co1—N1—C1 | −134.3 (2) | C8—C9—C10—N2 | 1.4 (3) |
N2—Co1—N1—C1 | −177.92 (18) | C10—N2—C11—C7 | −1.9 (2) |
O4i—Co1—N1—C12 | 77.27 (12) | Co1—N2—C11—C7 | 169.41 (13) |
O1—Co1—N1—C12 | −106.54 (12) | C10—N2—C11—C12 | 179.02 (16) |
O1W—Co1—N1—C12 | 166.55 (12) | Co1—N2—C11—C12 | −9.65 (18) |
O2W—Co1—N1—C12 | 29.5 (3) | C8—C7—C11—N2 | 2.6 (3) |
N2—Co1—N1—C12 | −14.05 (12) | C6—C7—C11—N2 | −176.55 (17) |
O4i—Co1—N2—C10 | 96.94 (15) | C8—C7—C11—C12 | −178.33 (17) |
O1—Co1—N2—C10 | −77.93 (15) | C6—C7—C11—C12 | 2.5 (3) |
O1W—Co1—N2—C10 | −173.6 (2) | C1—N1—C12—C4 | −0.1 (3) |
O2W—Co1—N2—C10 | 11.88 (15) | Co1—N1—C12—C4 | −165.76 (15) |
N1—Co1—N2—C10 | −177.05 (16) | C1—N1—C12—C11 | 179.39 (17) |
O4i—Co1—N2—C11 | −73.36 (11) | Co1—N1—C12—C11 | 13.73 (19) |
O1—Co1—N2—C11 | 111.78 (11) | C3—C4—C12—N1 | 0.8 (3) |
O1W—Co1—N2—C11 | 16.1 (4) | C5—C4—C12—N1 | −179.32 (18) |
O2W—Co1—N2—C11 | −158.42 (11) | C3—C4—C12—C11 | −178.72 (18) |
N1—Co1—N2—C11 | 12.65 (11) | C5—C4—C12—C11 | 1.2 (3) |
C12—N1—C1—C2 | −1.1 (3) | N2—C11—C12—N1 | −2.9 (2) |
Co1—N1—C1—C2 | 162.0 (2) | C7—C11—C12—N1 | 177.97 (15) |
N1—C1—C2—C3 | 1.7 (4) | N2—C11—C12—C4 | 176.57 (16) |
C1—C2—C3—C4 | −0.9 (4) | C7—C11—C12—C4 | −2.5 (2) |
C2—C3—C4—C12 | −0.2 (3) | Co1—O1—C13—O2 | −25.1 (3) |
C2—C3—C4—C5 | 179.9 (2) | Co1—O1—C13—C14 | 155.53 (11) |
C12—C4—C5—C6 | 0.1 (3) | Co1ii—O4—C16—O3 | −0.4 (3) |
C3—C4—C5—C6 | −180.0 (2) | Co1ii—O4—C16—C15 | 179.03 (11) |
C4—C5—C6—C7 | −0.1 (4) | | |
Symmetry codes: (i) x, y−1, z; (ii) x, y+1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···O3i | 0.85 (1) | 2.00 (1) | 2.7843 (18) | 153 (2) |
O1W—H1W2···O3iii | 0.84 (1) | 1.93 (1) | 2.7708 (17) | 175 (2) |
O2W—H2W1···O2iv | 0.85 (1) | 1.96 (1) | 2.7822 (18) | 164 (2) |
O2W—H2W2···O2 | 0.85 (1) | 1.92 (1) | 2.6991 (18) | 153 (2) |
Symmetry codes: (i) x, y−1, z; (iii) −x+1, y−1/2, −z+3/2; (iv) −x+1/2, y−1/2, z. |
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