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In the title compound, [Co(C
8H
6NO
4)
2(H
2O)
2]
n, the Co
II ion (site symmetry
) adopts a distorted octahedral coordination geometry. Neighboring metal ions are bridged by 1-(carboxylatomethyl)pyridinium-3-carboxylate ligands, forming a two-dimensional coordination network which is stabilized by O—H
O hydrogen bonds.
Supporting information
CCDC reference: 624707
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.003 Å
- R factor = 0.031
- wR factor = 0.072
- Data-to-parameter ratio = 13.5
checkCIF/PLATON results
No syntax errors found
Alert level C
CELLV02_ALERT_1_C The supplied cell volume s.u. differs from that
calculated from the cell parameter s.u.'s by > 2
Calculated cell volume su = 21.48
Cell volume su given = 19.00
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
2 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
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
1 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: XSCANS (Siemens, 1994); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.
Poly[diaquabis[µ-1-(carboxylatomethyl)pyridinium-4-carboxylato-
κ2O1:
O3]cobalt(II)]
top
Crystal data top
[Co(C8H6NO4)2(H2O)2] | F(000) = 466 |
Mr = 455.24 | Dx = 1.823 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 25 reflections |
a = 7.5954 (5) Å | θ = 3.0–20.0° |
b = 16.901 (4) Å | µ = 1.10 mm−1 |
c = 7.2755 (5) Å | T = 296 K |
β = 117.378 (5)° | Block, pink |
V = 829.32 (19) Å3 | 0.22 × 0.22 × 0.18 mm |
Z = 2 | |
Data collection top
Siemens P4 diffractometer | 1550 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.018 |
Graphite monochromator | θmax = 27.0°, θmin = 2.4° |
ω scans | h = −9→8 |
Absorption correction: ψ scan (North et al., 1968) | k = −21→1 |
Tmin = 0.794, Tmax = 0.826 | l = 0→9 |
2090 measured reflections | 3 standard reflections every 120 reflections |
1815 independent reflections | intensity decay: 3.3% |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difmap and geom |
R[F2 > 2σ(F2)] = 0.031 | H-atom parameters constrained |
wR(F2) = 0.072 | w = 1/[σ2(Fo2) + (0.03P)2 + 0.536P] where P = (Fo2 + 2Fc2)/3 |
S = 1.09 | (Δ/σ)max < 0.001 |
1815 reflections | Δρmax = 0.36 e Å−3 |
134 parameters | Δρmin = −0.36 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0153 (17) |
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 | 0.5000 | 0.5000 | 0.0000 | 0.01667 (13) | |
O1W | 0.2914 (2) | 0.56593 (8) | 0.0644 (2) | 0.0232 (3) | |
H1WB | 0.3050 | 0.5635 | 0.2008 | 0.035* | |
H1WA | 0.3342 | 0.6177 | 0.0531 | 0.035* | |
O1 | 0.3785 (2) | 0.39410 (8) | 0.0432 (2) | 0.0244 (3) | |
O2 | 0.5445 (2) | 0.30181 (9) | −0.0367 (3) | 0.0338 (4) | |
C1 | 0.4039 (3) | 0.32543 (12) | −0.0069 (3) | 0.0198 (4) | |
C2 | 0.2446 (3) | 0.26546 (11) | −0.0403 (3) | 0.0185 (4) | |
C3 | 0.0615 (3) | 0.28745 (12) | −0.0571 (3) | 0.0222 (4) | |
H3A | 0.0354 | 0.3403 | −0.0432 | 0.027* | |
C4 | −0.0815 (3) | 0.23052 (13) | −0.0945 (3) | 0.0256 (5) | |
H4A | −0.2026 | 0.2443 | −0.1003 | 0.031* | |
C5 | −0.0426 (3) | 0.15315 (12) | −0.1232 (3) | 0.0229 (4) | |
H5A | −0.1384 | 0.1145 | −0.1494 | 0.027* | |
C6 | 0.2770 (3) | 0.18703 (11) | −0.0687 (3) | 0.0188 (4) | |
H1A | 0.3993 | 0.1714 | −0.0568 | 0.023* | |
N1 | 0.1329 (3) | 0.13312 (9) | −0.1134 (3) | 0.0187 (3) | |
C7 | 0.1639 (3) | 0.05182 (11) | −0.1694 (3) | 0.0215 (4) | |
H7A | 0.2351 | 0.0553 | −0.2507 | 0.026* | |
H7B | 0.0353 | 0.0286 | −0.2568 | 0.026* | |
C8 | 0.2773 (3) | −0.00384 (12) | 0.0126 (3) | 0.0191 (4) | |
O3 | 0.2943 (2) | 0.01652 (9) | 0.1861 (2) | 0.0257 (3) | |
O4 | 0.3343 (2) | −0.06625 (9) | −0.0338 (2) | 0.0291 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0199 (2) | 0.01335 (19) | 0.0173 (2) | −0.00245 (15) | 0.00900 (15) | −0.00178 (15) |
O1W | 0.0273 (8) | 0.0194 (7) | 0.0256 (8) | −0.0031 (6) | 0.0146 (7) | −0.0007 (6) |
O1 | 0.0350 (9) | 0.0161 (7) | 0.0276 (8) | −0.0070 (6) | 0.0191 (7) | −0.0051 (6) |
O2 | 0.0287 (8) | 0.0207 (7) | 0.0602 (12) | −0.0021 (7) | 0.0274 (8) | −0.0012 (7) |
C1 | 0.0230 (10) | 0.0170 (9) | 0.0175 (10) | −0.0036 (8) | 0.0078 (8) | 0.0002 (8) |
C2 | 0.0222 (10) | 0.0168 (9) | 0.0153 (9) | −0.0022 (8) | 0.0076 (8) | −0.0006 (7) |
C3 | 0.0252 (10) | 0.0184 (9) | 0.0238 (11) | 0.0009 (8) | 0.0118 (9) | −0.0049 (8) |
C4 | 0.0198 (10) | 0.0306 (11) | 0.0273 (11) | −0.0013 (9) | 0.0118 (9) | −0.0049 (9) |
C5 | 0.0227 (10) | 0.0241 (10) | 0.0237 (11) | −0.0064 (8) | 0.0122 (9) | −0.0025 (8) |
C6 | 0.0185 (9) | 0.0185 (9) | 0.0193 (10) | −0.0005 (8) | 0.0085 (8) | 0.0011 (8) |
N1 | 0.0244 (8) | 0.0146 (8) | 0.0167 (8) | −0.0012 (7) | 0.0091 (7) | 0.0014 (6) |
C7 | 0.0294 (11) | 0.0140 (9) | 0.0197 (10) | −0.0003 (8) | 0.0101 (9) | −0.0014 (8) |
C8 | 0.0186 (9) | 0.0172 (9) | 0.0217 (9) | −0.0031 (8) | 0.0093 (8) | 0.0015 (8) |
O3 | 0.0293 (8) | 0.0270 (8) | 0.0192 (7) | 0.0048 (6) | 0.0098 (6) | 0.0027 (6) |
O4 | 0.0389 (9) | 0.0200 (7) | 0.0312 (9) | 0.0073 (7) | 0.0185 (8) | 0.0030 (7) |
Geometric parameters (Å, º) top
Co1—O1i | 2.1025 (14) | C3—H3A | 0.9300 |
Co1—O1 | 2.1025 (14) | C4—C5 | 1.378 (3) |
Co1—O3ii | 2.1101 (15) | C4—H4A | 0.9300 |
Co1—O3iii | 2.1101 (15) | C5—N1 | 1.345 (3) |
Co1—O1Wi | 2.1573 (14) | C5—H5A | 0.9300 |
Co1—O1W | 2.1573 (14) | C6—N1 | 1.344 (3) |
O1W—H1WB | 0.9501 | C6—H1A | 0.9300 |
O1W—H1WA | 0.9500 | N1—C7 | 1.482 (2) |
C1—O1 | 1.258 (2) | C7—C8 | 1.526 (3) |
C1—O2 | 1.249 (3) | C7—H7A | 0.9700 |
C1—C2 | 1.510 (3) | C7—H7B | 0.9700 |
C2—C6 | 1.381 (3) | C8—O4 | 1.244 (2) |
C2—C3 | 1.390 (3) | C8—O3 | 1.257 (2) |
C3—C4 | 1.381 (3) | O3—Co1iv | 2.1101 (15) |
| | | |
O1i—Co1—O1 | 180.0 | C4—C3—C2 | 119.73 (19) |
O1i—Co1—O3ii | 96.23 (6) | C4—C3—H3A | 120.1 |
O1—Co1—O3ii | 83.77 (6) | C2—C3—H3A | 120.1 |
O1i—Co1—O3iii | 83.77 (6) | C5—C4—C3 | 119.14 (19) |
O1—Co1—O3iii | 96.23 (6) | C5—C4—H4A | 120.4 |
O3ii—Co1—O3iii | 180.000 (1) | C3—C4—H4A | 120.4 |
O1i—Co1—O1Wi | 89.46 (5) | N1—C5—C4 | 120.48 (19) |
O1—Co1—O1Wi | 90.54 (5) | N1—C5—H5A | 119.8 |
O3ii—Co1—O1Wi | 87.08 (6) | C4—C5—H5A | 119.8 |
O3iii—Co1—O1Wi | 92.92 (6) | N1—C6—C2 | 120.36 (18) |
O1i—Co1—O1W | 90.54 (5) | N1—C6—H1A | 119.8 |
O1—Co1—O1W | 89.46 (5) | C2—C6—H1A | 119.8 |
O3ii—Co1—O1W | 92.92 (6) | C6—N1—C5 | 121.28 (17) |
O3iii—Co1—O1W | 87.08 (6) | C6—N1—C7 | 118.69 (17) |
O1Wi—Co1—O1W | 180.000 (1) | C5—N1—C7 | 119.85 (17) |
Co1—O1W—H1WB | 117.8 | N1—C7—C8 | 115.51 (16) |
Co1—O1W—H1WA | 98.2 | N1—C7—H7A | 108.4 |
H1WB—O1W—H1WA | 104.6 | C8—C7—H7A | 108.4 |
C1—O1—Co1 | 127.29 (13) | N1—C7—H7B | 108.4 |
O2—C1—O1 | 127.07 (19) | C8—C7—H7B | 108.4 |
O2—C1—C2 | 116.34 (17) | H7A—C7—H7B | 107.5 |
O1—C1—C2 | 116.58 (18) | O4—C8—O3 | 128.08 (19) |
C6—C2—C3 | 118.92 (18) | O4—C8—C7 | 114.53 (17) |
C6—C2—C1 | 118.92 (18) | O3—C8—C7 | 117.31 (17) |
C3—C2—C1 | 122.02 (18) | C8—O3—Co1iv | 137.20 (14) |
| | | |
O3ii—Co1—O1—C1 | 72.80 (17) | C3—C4—C5—N1 | 0.5 (3) |
O3iii—Co1—O1—C1 | −107.20 (17) | C3—C2—C6—N1 | 0.5 (3) |
O1Wi—Co1—O1—C1 | −14.20 (17) | C1—C2—C6—N1 | −175.22 (17) |
O1W—Co1—O1—C1 | 165.80 (17) | C2—C6—N1—C5 | −2.8 (3) |
Co1—O1—C1—O2 | 22.1 (3) | C2—C6—N1—C7 | 172.20 (18) |
Co1—O1—C1—C2 | −156.14 (13) | C4—C5—N1—C6 | 2.3 (3) |
O2—C1—C2—C6 | 9.9 (3) | C4—C5—N1—C7 | −172.63 (19) |
O1—C1—C2—C6 | −171.61 (18) | C6—N1—C7—C8 | 84.9 (2) |
O2—C1—C2—C3 | −165.7 (2) | C5—N1—C7—C8 | −100.1 (2) |
O1—C1—C2—C3 | 12.8 (3) | N1—C7—C8—O4 | −167.17 (17) |
C6—C2—C3—C4 | 2.2 (3) | N1—C7—C8—O3 | 15.9 (3) |
C1—C2—C3—C4 | 177.8 (2) | O4—C8—O3—Co1iv | 33.1 (3) |
C2—C3—C4—C5 | −2.7 (3) | C7—C8—O3—Co1iv | −150.42 (15) |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) x, −y+1/2, z−1/2; (iii) −x+1, y+1/2, −z+1/2; (iv) −x+1, y−1/2, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O2i | 0.95 | 1.68 | 2.612 (2) | 167 |
O1W—H1WB···O4v | 0.95 | 1.84 | 2.788 (2) | 176 |
Symmetry codes: (i) −x+1, −y+1, −z; (v) x, −y+1/2, z+1/2. |
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