The title compound, (C10H10N2)[Co(H2O)6](SO4)2, consists of 4,4'-bipyridinium dications, hexaaquacobalt(II) cations and sulfate anions that are linked by hydrogen bonds into a network structure. Six water molecules are coordinated to the Co atom and the geometry is octahedral. The bipyridinium cation has site symmetry 2 and the Co atom lies on a position of site symmetry 2/m.
Supporting information
CCDC reference: 258644
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.005 Å
- R factor = 0.034
- wR factor = 0.090
- Data-to-parameter ratio = 11.0
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for Co1
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.37
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
1 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
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; 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.
4,4'-Bipyridinium hexaaquacobalt(II) disulfate
top
Crystal data top
(C10H10N2)[Co(H2O)6](SO4)2 | F(000) = 534 |
Mr = 517.35 | Dx = 1.787 Mg m−3 |
Monoclinic, C2/m | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C2y | Cell parameters from 937 reflections |
a = 11.9210 (11) Å | θ = 2.6–21.4° |
b = 6.6042 (6) Å | µ = 1.19 mm−1 |
c = 12.9122 (12) Å | T = 298 K |
β = 108.951 (1)° | Plate, pink |
V = 961.46 (15) Å3 | 0.26 × 0.22 × 0.05 mm |
Z = 2 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 937 independent reflections |
Radiation source: fine-focus sealed tube | 905 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.018 |
φ and ω scans | θmax = 25.1°, θmin = 1.7° |
Absorption correction: numerical (SADABS; Sheldrick, 1996) | h = −14→14 |
Tmin = 0.74, Tmax = 0.94 | k = −7→7 |
2551 measured reflections | l = −15→12 |
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)] = 0.034 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.090 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.19 | w = 1/[σ2(Fo2) + (0.0468P)2 + 1.0311P] where P = (Fo2 + 2Fc2)/3 |
937 reflections | (Δ/σ)max = 0.001 |
85 parameters | Δρmax = 0.30 e Å−3 |
1 restraint | Δρmin = −0.57 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co1 | 0.5000 | 0.0000 | 0.5000 | 0.0260 (2) | |
O1 | 0.39848 (14) | 0.2254 (3) | 0.40218 (16) | 0.0525 (6) | |
H1B | 0.3290 | 0.1892 | 0.3792 | 0.079* | |
H1A | 0.4398 | 0.2921 | 0.3750 | 0.079* | |
O2 | 0.3770 (3) | 0.0000 | 0.5830 (3) | 0.0472 (7) | |
H2A | 0.3794 | −0.1091 | 0.6140 | 0.071* | |
O3 | 0.16052 (14) | 0.1826 (3) | 0.29323 (15) | 0.0388 (4) | |
O4 | 0.0522 (2) | 0.0000 | 0.13059 (19) | 0.0410 (7) | |
O5 | −0.01800 (19) | 0.0000 | 0.28473 (19) | 0.0340 (6) | |
S1 | 0.08938 (6) | 0.0000 | 0.25187 (6) | 0.0265 (2) | |
N1 | 0.2318 (2) | 0.0000 | 0.0539 (2) | 0.0331 (7) | |
H1N | 0.1657 | 0.0000 | 0.0674 | 0.040* | |
C1 | 0.2303 (3) | 0.0000 | −0.0490 (3) | 0.0362 (8) | |
H1 | 0.1582 | 0.0000 | −0.1056 | 0.043* | |
C2 | 0.3349 (3) | 0.0000 | −0.0728 (3) | 0.0354 (8) | |
H2 | 0.3333 | 0.0000 | −0.1453 | 0.042* | |
C3 | 0.4428 (2) | 0.0000 | 0.0113 (3) | 0.0244 (7) | |
C4 | 0.4399 (3) | 0.0000 | 0.1180 (3) | 0.0431 (10) | |
H4 | 0.5103 | 0.0000 | 0.1766 | 0.052* | |
C5 | 0.3332 (3) | 0.0000 | 0.1369 (3) | 0.0486 (10) | |
H5 | 0.3316 | 0.0000 | 0.2085 | 0.058* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0208 (3) | 0.0315 (4) | 0.0261 (4) | 0.000 | 0.0081 (2) | 0.000 |
O1 | 0.0252 (8) | 0.0580 (12) | 0.0687 (13) | −0.0003 (9) | 0.0076 (9) | 0.0306 (11) |
O2 | 0.0580 (17) | 0.0396 (15) | 0.0596 (18) | 0.000 | 0.0406 (15) | 0.000 |
O3 | 0.0276 (8) | 0.0378 (10) | 0.0496 (10) | −0.0046 (7) | 0.0104 (7) | −0.0032 (8) |
O4 | 0.0234 (11) | 0.0726 (19) | 0.0288 (12) | 0.000 | 0.0109 (10) | 0.000 |
O5 | 0.0247 (11) | 0.0471 (15) | 0.0355 (13) | 0.000 | 0.0171 (10) | 0.000 |
S1 | 0.0171 (4) | 0.0360 (5) | 0.0275 (4) | 0.000 | 0.0088 (3) | 0.000 |
N1 | 0.0229 (13) | 0.0353 (16) | 0.0465 (17) | 0.000 | 0.0188 (12) | 0.000 |
C1 | 0.0193 (15) | 0.043 (2) | 0.044 (2) | 0.000 | 0.0066 (14) | 0.000 |
C2 | 0.0220 (15) | 0.053 (2) | 0.0307 (17) | 0.000 | 0.0082 (13) | 0.000 |
C3 | 0.0203 (15) | 0.0247 (16) | 0.0297 (16) | 0.000 | 0.0102 (12) | 0.000 |
C4 | 0.0229 (16) | 0.078 (3) | 0.0285 (17) | 0.000 | 0.0091 (13) | 0.000 |
C5 | 0.038 (2) | 0.081 (3) | 0.0339 (19) | 0.000 | 0.0218 (16) | 0.000 |
Geometric parameters (Å, º) top
Co1—O1i | 2.0695 (18) | N1—C1 | 1.323 (5) |
Co1—O1ii | 2.0695 (18) | N1—C5 | 1.330 (5) |
Co1—O1 | 2.0695 (18) | N1—H1N | 0.8600 |
Co1—O1iii | 2.0695 (17) | C1—C2 | 1.378 (5) |
Co1—O2 | 2.078 (2) | C1—H1 | 0.9300 |
Co1—O2iii | 2.078 (2) | C2—C3 | 1.387 (4) |
O1—H1B | 0.8200 | C2—H2 | 0.9300 |
O1—H1A | 0.8201 | C3—C4 | 1.390 (5) |
O2—H2A | 0.8200 | C3—C3iv | 1.485 (6) |
O3—S1 | 1.4712 (17) | C4—C5 | 1.371 (5) |
O4—S1 | 1.483 (2) | C4—H4 | 0.9300 |
O5—S1 | 1.474 (2) | C5—H5 | 0.9300 |
S1—O3i | 1.4712 (17) | | |
| | | |
O1i—Co1—O1ii | 180.00 (8) | O3—S1—O4 | 108.83 (9) |
O1i—Co1—O1 | 91.99 (12) | O3i—S1—O4 | 108.83 (9) |
O1ii—Co1—O1 | 88.01 (12) | O5—S1—O4 | 108.33 (13) |
O1i—Co1—O1iii | 88.01 (12) | C1—N1—C5 | 121.4 (3) |
O1ii—Co1—O1iii | 91.99 (12) | C1—N1—H1N | 119.3 |
O1—Co1—O1iii | 180.00 (10) | C5—N1—H1N | 119.3 |
O1i—Co1—O2 | 86.80 (8) | N1—C1—C2 | 120.4 (3) |
O1ii—Co1—O2 | 93.20 (8) | N1—C1—H1 | 119.8 |
O1—Co1—O2 | 86.80 (8) | C2—C1—H1 | 119.8 |
O1iii—Co1—O2 | 93.20 (8) | C1—C2—C3 | 120.1 (3) |
O1i—Co1—O2iii | 93.20 (8) | C1—C2—H2 | 120.0 |
O1ii—Co1—O2iii | 86.80 (8) | C3—C2—H2 | 120.0 |
O1—Co1—O2iii | 93.20 (8) | C2—C3—C4 | 117.5 (3) |
O1iii—Co1—O2iii | 86.80 (8) | C2—C3—C3iv | 121.5 (4) |
O2—Co1—O2iii | 180.0 | C4—C3—C3iv | 121.0 (3) |
Co1—O1—H1B | 109.5 | C5—C4—C3 | 120.0 (3) |
Co1—O1—H1A | 109.5 | C5—C4—H4 | 120.0 |
H1B—O1—H1A | 132.7 | C3—C4—H4 | 120.0 |
Co1—O2—H2A | 109.5 | N1—C5—C4 | 120.6 (3) |
O3—S1—O3i | 110.11 (14) | N1—C5—H5 | 119.7 |
O3—S1—O5 | 110.34 (9) | C4—C5—H5 | 119.7 |
O3i—S1—O5 | 110.34 (9) | | |
| | | |
C5—N1—C1—C2 | 0.0 | C2—C3—C4—C5 | 0.0 |
N1—C1—C2—C3 | 0.0 | C3iv—C3—C4—C5 | 180.0 |
C1—C2—C3—C4 | 0.0 | C1—N1—C5—C4 | 0.0 |
C1—C2—C3—C3iv | 180.0 | C3—C4—C5—N1 | 0.0 |
Symmetry codes: (i) x, −y, z; (ii) −x+1, y, −z+1; (iii) −x+1, −y, −z+1; (iv) −x+1, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1N···O4 | 0.86 | 1.79 | 2.634 (3) | 166 |
N1—H1N···O4 | 0.86 | 1.79 | 2.634 (3) | 166 |
O2—H2A···O3v | 0.82 | 1.98 | 2.759 (2) | 158 |
O1—H1A···O5vi | 0.82 | 1.97 | 2.750 (2) | 159 |
O1—H1B···O3 | 0.82 | 1.95 | 2.741 (2) | 161 |
N1—H1N···O4 | 0.86 | 1.79 | 2.634 (3) | 166 |
Symmetry codes: (v) −x+1/2, y−1/2, −z+1; (vi) x+1/2, y+1/2, z. |