The title complex, [Co(C
12H
8N
2)(H
2O)
4](C
10H
6O
6S
2)·2H
2O, was synthesized hydrothermally. The Co
2+ cation, which lies on a twofold rotation axis, is six-coordinate. The anion is located on a centre of inversion. An extensive network of O—H
O hydrogen bonds links the components into a three-dimensional network.
Supporting information
CCDC reference: 672731
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.002 Å
- R factor = 0.034
- wR factor = 0.097
- Data-to-parameter ratio = 14.6
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT230_ALERT_2_C Hirshfeld Test Diff for C8 - C9 .. 5.20 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - O4 .. 8.75 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - O5 .. 5.89 su
Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 6
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
A mixture of naphthalene-1,5-disulfonic acid (0.2810 g, 0.001 mol),
1,10-phenanthroline(0.1780 g, 0.001 mol) and CoNO3.6H2O (0.2310,0.001 mol)
was added to 20 ml water, The mixture was closed in a steel tomb and heated at
418 K for 4 days. Single crystals suitable for X-ray diffraction analysis
formed after it cooled down to room temperature.
All H atoms bonded to C atoms were set to calculated positions and refined as
riding on their parent C atoms with the C—H bond length fixed to 0.93Å
with Uiso(H) = 1.2 times Ueq(C). The H atoms of the water
molecules were taken from an electron density map and refined as riding on
their parent O atoms with the O—H bond length fixed to 0.82Å with
Uiso(H) = 1.5 times Ueq(O).
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1996); software used to prepare material for publication: SHELXTL (Siemens, 1996).
Tetraaqua(1,10-phenanthroline)cobalt(II) naphthalene-1,5-disulfonate dihydrate
top
Crystal data top
[Co(C12H8N2)(H2O)4](C10H6O6S2)·2H2O | F(000) = 1308 |
Mr = 633.52 | Dx = 1.590 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 7881 reflections |
a = 20.578 (4) Å | θ = 1.0–28.3° |
b = 12.431 (3) Å | µ = 0.87 mm−1 |
c = 12.462 (3) Å | T = 293 K |
β = 123.867 (2)° | Block, brown |
V = 2647.0 (10) Å3 | 0.40 × 0.35 × 0.32 mm |
Z = 4 | |
Data collection top
CCD area-detector diffractometer | 2353 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.018 |
Graphite monochromator | θmax = 26.0°, θmin = 2.0° |
ϕ and ω scans | h = −25→25 |
8365 measured reflections | k = −15→15 |
2590 independent reflections | l = −15→15 |
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) = 0.098 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0589P)2 + 2.5933P] where P = (Fo2 + 2Fc2)/3 |
2590 reflections | (Δ/σ)max = 0.004 |
177 parameters | Δρmax = 0.77 e Å−3 |
6 restraints | Δρmin = −0.42 e Å−3 |
Crystal data top
[Co(C12H8N2)(H2O)4](C10H6O6S2)·2H2O | V = 2647.0 (10) Å3 |
Mr = 633.52 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 20.578 (4) Å | µ = 0.87 mm−1 |
b = 12.431 (3) Å | T = 293 K |
c = 12.462 (3) Å | 0.40 × 0.35 × 0.32 mm |
β = 123.867 (2)° | |
Data collection top
CCD area-detector diffractometer | 2353 reflections with I > 2σ(I) |
8365 measured reflections | Rint = 0.018 |
2590 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.034 | 6 restraints |
wR(F2) = 0.098 | H-atom parameters constrained |
S = 1.07 | Δρmax = 0.77 e Å−3 |
2590 reflections | Δρmin = −0.42 e Å−3 |
177 parameters | |
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 | |
O6 | 0.92197 (10) | 0.91248 (19) | 0.91351 (19) | 0.1020 (7) | |
H6A | 0.9014 | 0.9461 | 0.9470 | 0.153* | |
H6B | 0.8862 | 0.9122 | 0.8332 | 0.153* | |
C1 | 0.74393 (8) | 0.18231 (13) | 0.36018 (14) | 0.0350 (4) | |
H1 | 0.7508 | 0.1143 | 0.3369 | 0.042* | |
C2 | 0.75484 (8) | 0.19727 (11) | 0.48239 (14) | 0.0296 (3) | |
C3 | 0.77564 (8) | 0.11167 (12) | 0.57272 (14) | 0.0315 (4) | |
C4 | 0.78621 (9) | 0.12984 (13) | 0.68961 (14) | 0.0369 (4) | |
H4 | 0.7996 | 0.0731 | 0.7470 | 0.044* | |
C5 | 0.72373 (9) | 0.26630 (14) | 0.27639 (15) | 0.0392 (4) | |
H5 | 0.7162 | 0.2547 | 0.1965 | 0.047* | |
C6 | 0.52159 (13) | −0.21659 (15) | 0.8154 (2) | 0.0628 (6) | |
H6 | 0.5368 | −0.2817 | 0.8596 | 0.075* | |
C7 | 0.54443 (9) | −0.11799 (15) | 0.88668 (16) | 0.0437 (4) | |
C8 | 0.58766 (10) | −0.11283 (18) | 1.02151 (17) | 0.0522 (5) | |
H8 | 0.6036 | −0.1756 | 1.0704 | 0.063* | |
C9 | 0.60609 (10) | −0.01630 (19) | 1.08079 (16) | 0.0522 (5) | |
H9 | 0.6356 | −0.0123 | 1.1705 | 0.063* | |
C10 | 0.58099 (9) | 0.07835 (17) | 1.00709 (15) | 0.0429 (4) | |
H10 | 0.5936 | 0.1443 | 1.0494 | 0.052* | |
C11 | 0.52200 (8) | −0.01967 (12) | 0.81936 (13) | 0.0312 (4) | |
Co1 | 0.5000 | 0.21031 (2) | 0.7500 | 0.03305 (8) | |
N1 | 0.53944 (7) | 0.07706 (11) | 0.87848 (11) | 0.0322 (3) | |
O1 | 0.85225 (7) | −0.02251 (10) | 0.52277 (13) | 0.0548 (3) | |
O2 | 0.79931 (7) | −0.08974 (9) | 0.64024 (11) | 0.0466 (3) | |
O3 | 0.71259 (8) | −0.04810 (10) | 0.41253 (12) | 0.0523 (4) | |
O4 | 0.53359 (7) | 0.32180 (12) | 0.89771 (15) | 0.0656 (4) | |
H4A | 0.5049 | 0.3500 | 0.9159 | 0.098* | |
H4B | 0.5648 | 0.3713 | 0.9178 | 0.098* | |
O5 | 0.61506 (6) | 0.21906 (9) | 0.79332 (11) | 0.0394 (3) | |
H5A | 0.6446 | 0.1682 | 0.8308 | 0.059* | |
H5B | 0.6405 | 0.2750 | 0.8162 | 0.059* | |
S2 | 0.78554 (2) | −0.02258 (3) | 0.53385 (4) | 0.03427 (10) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
O6 | 0.0932 (9) | 0.1232 (16) | 0.1006 (10) | 0.0290 (11) | 0.0608 (8) | −0.0182 (10) |
C1 | 0.0407 (6) | 0.0264 (7) | 0.0379 (6) | −0.0013 (6) | 0.0219 (5) | −0.0038 (5) |
C2 | 0.0274 (5) | 0.0232 (7) | 0.0344 (6) | −0.0021 (5) | 0.0150 (5) | −0.0014 (5) |
C3 | 0.0305 (5) | 0.0231 (7) | 0.0378 (6) | 0.0004 (5) | 0.0170 (5) | 0.0008 (5) |
C4 | 0.0415 (6) | 0.0289 (7) | 0.0371 (6) | 0.0010 (6) | 0.0199 (5) | 0.0050 (6) |
C5 | 0.0478 (7) | 0.0348 (8) | 0.0335 (6) | −0.0003 (7) | 0.0217 (5) | −0.0011 (6) |
C6 | 0.0847 (11) | 0.0287 (9) | 0.0812 (11) | 0.0067 (8) | 0.0501 (9) | 0.0116 (8) |
C7 | 0.0441 (6) | 0.0397 (9) | 0.0520 (7) | 0.0062 (7) | 0.0296 (5) | 0.0121 (7) |
C8 | 0.0451 (7) | 0.0611 (11) | 0.0501 (8) | 0.0106 (8) | 0.0263 (6) | 0.0253 (8) |
C9 | 0.0348 (7) | 0.0840 (14) | 0.0320 (7) | 0.0016 (8) | 0.0150 (5) | 0.0156 (8) |
C10 | 0.0342 (6) | 0.0587 (11) | 0.0322 (6) | −0.0082 (7) | 0.0162 (5) | −0.0057 (7) |
C11 | 0.0297 (5) | 0.0316 (8) | 0.0340 (6) | 0.0010 (5) | 0.0188 (4) | 0.0032 (5) |
Co1 | 0.03179 (11) | 0.02513 (14) | 0.04219 (13) | 0.000 | 0.02060 (9) | 0.000 |
N1 | 0.0302 (5) | 0.0354 (7) | 0.0302 (5) | −0.0037 (5) | 0.0163 (4) | −0.0014 (5) |
O1 | 0.0607 (5) | 0.0418 (7) | 0.0830 (6) | 0.0173 (5) | 0.0530 (5) | 0.0175 (5) |
O2 | 0.0643 (6) | 0.0266 (6) | 0.0546 (5) | 0.0084 (5) | 0.0368 (4) | 0.0107 (4) |
O3 | 0.0597 (7) | 0.0294 (6) | 0.0514 (6) | −0.0095 (5) | 0.0208 (5) | −0.0068 (5) |
O4 | 0.0556 (5) | 0.0521 (7) | 0.1043 (8) | −0.0211 (6) | 0.0539 (5) | −0.0404 (6) |
O5 | 0.0339 (4) | 0.0262 (5) | 0.0552 (6) | 0.0003 (4) | 0.0230 (4) | 0.0014 (4) |
S2 | 0.04075 (15) | 0.02087 (17) | 0.04330 (16) | 0.00339 (13) | 0.02474 (13) | 0.00308 (12) |
Geometric parameters (Å, º) top
O6—H6A | 0.8504 | C9—C10 | 1.402 (3) |
O6—H6B | 0.8501 | C9—H9 | 0.9301 |
C1—C5 | 1.367 (2) | C10—N1 | 1.331 (2) |
C1—C2 | 1.422 (2) | C10—H10 | 0.9300 |
C1—H1 | 0.9300 | C11—N1 | 1.350 (2) |
C2—C3 | 1.430 (2) | C11—C11ii | 1.437 (3) |
C2—C2i | 1.431 (3) | Co1—O4 | 2.0902 (15) |
C3—C4 | 1.366 (2) | Co1—O4ii | 2.0902 (15) |
C3—S2 | 1.7808 (16) | Co1—O5ii | 2.1177 (13) |
C4—C5i | 1.409 (2) | Co1—O5 | 2.1177 (13) |
C4—H4 | 0.9300 | Co1—N1ii | 2.1255 (14) |
C5—C4i | 1.409 (2) | Co1—N1 | 2.1255 (14) |
C5—H5 | 0.9301 | O1—S2 | 1.4543 (15) |
C6—C6ii | 1.354 (4) | O2—S2 | 1.4548 (13) |
C6—C7 | 1.431 (3) | O3—S2 | 1.4528 (12) |
C6—H6 | 0.9300 | O4—H4A | 0.8206 |
C7—C8 | 1.397 (3) | O4—H4B | 0.8203 |
C7—C11 | 1.407 (2) | O5—H5A | 0.8190 |
C8—C9 | 1.348 (3) | O5—H5B | 0.8196 |
C8—H8 | 0.9300 | | |
| | | |
H6A—O6—H6B | 103.9 | N1—C11—C11ii | 117.02 (8) |
C5—C1—C2 | 121.16 (15) | C7—C11—C11ii | 119.67 (10) |
C5—C1—H1 | 119.4 | O4—Co1—O4ii | 96.93 (9) |
C2—C1—H1 | 119.5 | O4—Co1—O5ii | 87.97 (5) |
C1—C2—C3 | 123.01 (14) | O4ii—Co1—O5ii | 88.13 (5) |
C1—C2—C2i | 118.83 (17) | O4—Co1—O5 | 88.13 (5) |
C3—C2—C2i | 118.16 (18) | O4ii—Co1—O5 | 87.97 (5) |
C4—C3—C2 | 121.07 (14) | O5ii—Co1—O5 | 174.11 (6) |
C4—C3—S2 | 118.07 (12) | O4—Co1—N1ii | 168.58 (6) |
C2—C3—S2 | 120.84 (12) | O4ii—Co1—N1ii | 93.06 (6) |
C3—C4—C5i | 120.57 (15) | O5ii—Co1—N1ii | 86.83 (5) |
C3—C4—H4 | 119.8 | O5—Co1—N1ii | 97.78 (5) |
C5i—C4—H4 | 119.6 | O4—Co1—N1 | 93.06 (6) |
C1—C5—C4i | 120.22 (16) | O4ii—Co1—N1 | 168.58 (6) |
C1—C5—H5 | 119.8 | O5ii—Co1—N1 | 97.78 (5) |
C4i—C5—H5 | 119.9 | O5—Co1—N1 | 86.83 (5) |
C6ii—C6—C7 | 121.03 (11) | N1ii—Co1—N1 | 77.60 (7) |
C6ii—C6—H6 | 119.4 | C10—N1—C11 | 117.69 (14) |
C7—C6—H6 | 119.5 | C10—N1—Co1 | 128.09 (12) |
C8—C7—C11 | 117.04 (17) | C11—N1—Co1 | 114.16 (9) |
C8—C7—C6 | 123.68 (18) | Co1—O4—H4A | 126.2 |
C11—C7—C6 | 119.28 (16) | Co1—O4—H4B | 125.7 |
C9—C8—C7 | 119.74 (18) | H4A—O4—H4B | 99.0 |
C9—C8—H8 | 119.9 | Co1—O5—H5A | 118.4 |
C7—C8—H8 | 120.3 | Co1—O5—H5B | 122.6 |
C8—C9—C10 | 119.96 (16) | H5A—O5—H5B | 109.2 |
C8—C9—H9 | 120.1 | O3—S2—O1 | 112.58 (9) |
C10—C9—H9 | 119.9 | O3—S2—O2 | 112.74 (8) |
N1—C10—C9 | 122.24 (18) | O1—S2—O2 | 111.85 (8) |
N1—C10—H10 | 118.8 | O3—S2—C3 | 106.21 (7) |
C9—C10—H10 | 118.9 | O1—S2—C3 | 106.41 (8) |
N1—C11—C7 | 123.32 (14) | O2—S2—C3 | 106.48 (8) |
Symmetry codes: (i) −x+3/2, −y+1/2, −z+1; (ii) −x+1, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5B···O2iii | 0.82 | 1.98 | 2.7953 (17) | 176 |
O5—H5A···O3iv | 0.82 | 1.91 | 2.7255 (17) | 178 |
O4—H4B···O1iii | 0.82 | 1.95 | 2.7660 (19) | 174 |
O4—H4A···O6v | 0.82 | 1.86 | 2.663 (3) | 166 |
O6—H6B···O2vi | 0.85 | 2.05 | 2.896 (2) | 179 |
O6—H6A···O1vii | 0.85 | 1.97 | 2.821 (3) | 179 |
Symmetry codes: (iii) −x+3/2, y+1/2, −z+3/2; (iv) x, −y, z+1/2; (v) x−1/2, y−1/2, z; (vi) x, y+1, z; (vii) x, −y+1, z+1/2. |
Experimental details
Crystal data |
Chemical formula | [Co(C12H8N2)(H2O)4](C10H6O6S2)·2H2O |
Mr | 633.52 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 293 |
a, b, c (Å) | 20.578 (4), 12.431 (3), 12.462 (3) |
β (°) | 123.867 (2) |
V (Å3) | 2647.0 (10) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.87 |
Crystal size (mm) | 0.40 × 0.35 × 0.32 |
|
Data collection |
Diffractometer | CCD area-detector diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8365, 2590, 2353 |
Rint | 0.018 |
(sin θ/λ)max (Å−1) | 0.617 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.098, 1.07 |
No. of reflections | 2590 |
No. of parameters | 177 |
No. of restraints | 6 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.77, −0.42 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5B···O2i | 0.82 | 1.98 | 2.7953 (17) | 176.1 |
O5—H5A···O3ii | 0.82 | 1.91 | 2.7255 (17) | 178.1 |
O4—H4B···O1i | 0.82 | 1.95 | 2.7660 (19) | 173.8 |
O4—H4A···O6iii | 0.82 | 1.86 | 2.663 (3) | 165.9 |
O6—H6B···O2iv | 0.85 | 2.05 | 2.896 (2) | 179.2 |
O6—H6A···O1v | 0.85 | 1.97 | 2.821 (3) | 179.0 |
Symmetry codes: (i) −x+3/2, y+1/2, −z+3/2; (ii) x, −y, z+1/2; (iii) x−1/2, y−1/2, z; (iv) x, y+1, z; (v) x, −y+1, z+1/2. |
The title compound is consisted of Cobalt(II) coordination cations, naphthalene-1,5-disulfonic acid anions and latice water molecules. In the complex there exists an extensive network of O—H···O hydrogen bonds which form among the coordinated water molecules, the sulfonate groups of the anions and the latice water molecules (Fig. 2).