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In the crystal structure of the title complex, [Co(H
2O)
6](
L)
2 (
L = isonicotinate
N-oxide, C
6H
4NO
3), the Co
II center, on a special position with site symmetry 2/
m, is in an elongated octahedral environment composed of six coordinated water molecules. Each water ligand forms two strong O—H
O hydrogen bonds with the adjacent isonicotinate
N-oxide counter-ions, which lie on mirror planes, forming a three-dimensional hydrogen-bonding supramolecular architecture.
Supporting information
CCDC reference: 242045
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.036
- wR factor = 0.082
- Data-to-parameter ratio = 15.1
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT242_ALERT_2_A Check Low U(eq) as Compared to Neighbors .... Co1
Alert level B
PLAT213_ALERT_2_B Atom O2 has ADP max/min Ratio ............. 4.30 prolat
PLAT250_ALERT_2_B Large U3/U1 Ratio for Average U(i,j) Tensor .... 4.62
Alert level C
PLAT213_ALERT_2_C Atom O3 has ADP max/min Ratio ............. 3.10 prolat
PLAT213_ALERT_2_C Atom O4 has ADP max/min Ratio ............. 3.40 prolat
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.55 Ratio
PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C1
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... N1
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C3
PLAT480_ALERT_4_C Long H...A H-Bond Reported H4B .. N1 .. 2.67 Ang.
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.15 Ratio
Alert level G
REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values
From the CIF: _diffrn_reflns_theta_max 28.03
From the CIF: _reflns_number_total 1086
From the CIF: _diffrn_reflns_limit_ max hkl 13. 9. 9.
From the CIF: _diffrn_reflns_limit_ min hkl -8. -11. -9.
TEST1: Expected hkl limits for theta max
Calculated maximum hkl 15. 12. 10.
Calculated minimum hkl -15. -12. -10.
1 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
8 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
9 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, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Berndt, 1999); software used to prepare material for publication: SHELXL97.
Crystal data top
[Co(H2O)6](C6H4NO3)2 | F(000) = 458 |
Mr = 443.23 | Dx = 1.705 Mg m−3 |
Monoclinic, C2/m | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2y | Cell parameters from 756 reflections |
a = 11.425 (4) Å | θ = 2.7–28.0° |
b = 9.780 (4) Å | µ = 1.06 mm−1 |
c = 7.726 (3) Å | T = 293 K |
β = 90.967 (6)° | Block, pink |
V = 863.2 (6) Å3 | 0.28 × 0.20 × 0.12 mm |
Z = 2 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 1086 independent reflections |
Radiation source: fine-focus sealed tube | 1061 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
φ and ω scans | θmax = 28.0°, θmin = 2.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1997) | h = −8→13 |
Tmin = 0.688, Tmax = 0.880 | k = −11→9 |
2775 measured reflections | l = −9→9 |
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)] = 0.036 | H-atom parameters constrained |
wR(F2) = 0.082 | w = 1/[σ2(Fo2) + (0.0203P)2 + 2.5192P] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | (Δ/σ)max < 0.001 |
1086 reflections | Δρmax = 0.56 e Å−3 |
72 parameters | Δρmin = −0.41 e Å−3 |
2 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0032 (9) |
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 | 0.5000 | 0.02533 (18) | |
C1 | 0.8275 (3) | 0.6162 (4) | 0.1438 (5) | 0.0842 (12) | |
H1 | 0.7884 | 0.6982 | 0.1233 | 0.101* | |
C2 | 0.9402 (2) | 0.6183 (3) | 0.2079 (4) | 0.0681 (9) | |
H2 | 0.9770 | 0.7016 | 0.2292 | 0.082* | |
C3 | 0.9983 (2) | 0.5000 | 0.2403 (4) | 0.0336 (6) | |
C4 | 1.1224 (2) | 0.5000 | 0.3097 (4) | 0.0330 (6) | |
N1 | 0.7740 (2) | 0.5000 | 0.1112 (4) | 0.0649 (12) | |
O1 | 1.16996 (14) | 0.38743 (18) | 0.3336 (3) | 0.0533 (5) | |
O2 | 0.6669 (2) | 0.5000 | 0.0443 (3) | 0.1031 (16) | |
O3 | 0.63001 (15) | 0.6422 (2) | 0.4881 (3) | 0.0761 (8) | |
H3A | 0.6927 | 0.6311 | 0.5465 | 0.114* | |
H3B | 0.6330 | 0.7173 | 0.4352 | 0.114* | |
O4 | 0.5190 (2) | 0.5000 | 0.7654 (3) | 0.0975 (15) | |
H4A | 0.5770 | 0.5000 | 0.8359 | 0.146* | |
H4B | 0.4545 | 0.5000 | 0.8187 | 0.146* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0175 (3) | 0.0266 (3) | 0.0317 (3) | 0.000 | −0.00609 (18) | 0.000 |
C1 | 0.0472 (16) | 0.105 (3) | 0.099 (3) | 0.0381 (18) | −0.0328 (17) | −0.022 (2) |
C2 | 0.0453 (15) | 0.0605 (18) | 0.097 (2) | 0.0203 (13) | −0.0331 (15) | −0.0225 (17) |
C3 | 0.0239 (13) | 0.0481 (18) | 0.0287 (14) | 0.000 | −0.0049 (10) | 0.000 |
C4 | 0.0245 (13) | 0.0407 (16) | 0.0336 (14) | 0.000 | −0.0079 (11) | 0.000 |
N1 | 0.0203 (13) | 0.146 (4) | 0.0279 (14) | 0.000 | −0.0060 (10) | 0.000 |
O1 | 0.0354 (8) | 0.0388 (9) | 0.0850 (13) | −0.0024 (7) | −0.0247 (8) | 0.0169 (9) |
O2 | 0.0191 (11) | 0.254 (5) | 0.0356 (14) | 0.000 | −0.0108 (10) | 0.000 |
O3 | 0.0404 (10) | 0.0561 (12) | 0.1302 (19) | −0.0250 (9) | −0.0475 (11) | 0.0491 (13) |
O4 | 0.0277 (13) | 0.233 (5) | 0.0313 (13) | 0.000 | −0.0084 (10) | 0.000 |
Geometric parameters (Å, º) top
Co1—O3i | 2.0378 (18) | C3—C2ii | 1.356 (3) |
Co1—O3 | 2.0378 (18) | C3—C4 | 1.507 (4) |
Co1—O3ii | 2.0378 (18) | C4—O1ii | 1.240 (2) |
Co1—O3iii | 2.0378 (18) | C4—O1 | 1.240 (2) |
Co1—O4i | 2.059 (3) | N1—C1ii | 1.313 (4) |
Co1—O4 | 2.059 (3) | N1—O2 | 1.320 (3) |
C1—N1 | 1.313 (4) | O3—H3A | 0.8470 |
C1—C2 | 1.372 (4) | O3—H3B | 0.8413 |
C1—H1 | 0.9300 | O4—H4A | 0.8500 |
C2—C3 | 1.356 (3) | O4—H4B | 0.8500 |
C2—H2 | 0.9300 | | |
| | | |
O3i—Co1—O3 | 180.00 (8) | C3—C2—C1 | 120.5 (3) |
O3i—Co1—O3ii | 93.95 (13) | C3—C2—H2 | 119.8 |
O3—Co1—O3ii | 86.05 (13) | C1—C2—H2 | 119.8 |
O3i—Co1—O3iii | 86.05 (13) | C2ii—C3—C2 | 117.2 (3) |
O3—Co1—O3iii | 93.95 (13) | C2ii—C3—C4 | 121.39 (16) |
O3ii—Co1—O3iii | 180.0 | C2—C3—C4 | 121.39 (16) |
O3i—Co1—O4i | 88.87 (9) | O1ii—C4—O1 | 125.2 (3) |
O3—Co1—O4i | 91.13 (9) | O1ii—C4—C3 | 117.40 (13) |
O3ii—Co1—O4i | 91.13 (9) | O1—C4—C3 | 117.40 (13) |
O3iii—Co1—O4i | 88.87 (9) | C1—N1—C1ii | 119.9 (3) |
O3i—Co1—O4 | 91.13 (9) | C1—N1—O2 | 120.06 (16) |
O3—Co1—O4 | 88.87 (9) | C1ii—N1—O2 | 120.06 (16) |
O3ii—Co1—O4 | 88.87 (9) | Co1—O3—H3A | 119.9 |
O3iii—Co1—O4 | 91.13 (9) | Co1—O3—H3B | 130.7 |
O4i—Co1—O4 | 180.0 | H3A—O3—H3B | 109.3 |
N1—C1—C2 | 120.9 (3) | Co1—O4—H4A | 134.9 |
N1—C1—H1 | 119.5 | Co1—O4—H4B | 113.9 |
C2—C1—H1 | 119.5 | H4A—O4—H4B | 111.2 |
| | | |
N1—C1—C2—C3 | −0.6 (6) | C2ii—C3—C4—O1 | 1.1 (5) |
C1—C2—C3—C2ii | −0.4 (6) | C2—C3—C4—O1 | −179.0 (3) |
C1—C2—C3—C4 | 179.7 (3) | C2—C1—N1—C1ii | 1.7 (7) |
C2ii—C3—C4—O1ii | 179.0 (3) | C2—C1—N1—O2 | −177.8 (3) |
C2—C3—C4—O1ii | −1.1 (5) | | |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, −y+1, z; (iii) −x+1, y, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H4B···N1i | 0.85 | 2.67 | 3.495 (4) | 163 |
O4—H4B···O2i | 0.85 | 1.76 | 2.603 (4) | 172 |
O4—H4A···O2iv | 0.85 | 1.90 | 2.715 (4) | 161 |
O3—H3B···O1v | 0.84 | 1.89 | 2.721 (3) | 169 |
O3—H3A···O1vi | 0.85 | 1.82 | 2.664 (2) | 178 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (iv) x, y, z+1; (v) x−1/2, y+1/2, z; (vi) −x+2, −y+1, −z+1. |
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