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The title complex, [Co(C12H8N2)(H2O)4](C10H6O6S2)·2H2O, was synthesized hydro­thermally. The Co2+ 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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680705982X/bt2626sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680705982X/bt2626Isup2.hkl
Contains datablock I

CCDC reference: 672731

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](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

Comment top

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).

Related literature top

For a related copper(II) structure, see Liu & Zeng (2007).

Experimental top

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.

Refinement top

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).

Computing details top

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).

Figures top
[Figure 1] Fig. 1. Perspective view of the title compound showing 50% probability displacement ellipsoids.
[Figure 2] Fig. 2. The packing diagram, viewed along the b axis; hydrogen bonds are shown as dashed lines.
Tetraaqua(1,10-phenanthroline)cobalt(II) naphthalene-1,5-disulfonate dihydrate top
Crystal data top
[Co(C12H8N2)(H2O)4](C10H6O6S2)·2H2OF(000) = 1308
Mr = 633.52Dx = 1.590 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 7881 reflections
a = 20.578 (4) Åθ = 1.0–28.3°
b = 12.431 (3) ŵ = 0.87 mm1
c = 12.462 (3) ÅT = 293 K
β = 123.867 (2)°Block, brown
V = 2647.0 (10) Å30.40 × 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 tubeRint = 0.018
Graphite monochromatorθmax = 26.0°, θmin = 2.0°
ϕ and ω scansh = 2525
8365 measured reflectionsk = 1515
2590 independent reflectionsl = 1515
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.098H-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 parametersΔρmax = 0.77 e Å3
6 restraintsΔρmin = 0.42 e Å3
Crystal data top
[Co(C12H8N2)(H2O)4](C10H6O6S2)·2H2OV = 2647.0 (10) Å3
Mr = 633.52Z = 4
Monoclinic, C2/cMo Kα radiation
a = 20.578 (4) ŵ = 0.87 mm1
b = 12.431 (3) ÅT = 293 K
c = 12.462 (3) Å0.40 × 0.35 × 0.32 mm
β = 123.867 (2)°
Data collection top
CCD area-detector
diffractometer
2353 reflections with I > 2σ(I)
8365 measured reflectionsRint = 0.018
2590 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0346 restraints
wR(F2) = 0.098H-atom parameters constrained
S = 1.07Δρmax = 0.77 e Å3
2590 reflectionsΔρmin = 0.42 e Å3
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
xyzUiso*/Ueq
O60.92197 (10)0.91248 (19)0.91351 (19)0.1020 (7)
H6A0.90140.94610.94700.153*
H6B0.88620.91220.83320.153*
C10.74393 (8)0.18231 (13)0.36018 (14)0.0350 (4)
H10.75080.11430.33690.042*
C20.75484 (8)0.19727 (11)0.48239 (14)0.0296 (3)
C30.77564 (8)0.11167 (12)0.57272 (14)0.0315 (4)
C40.78621 (9)0.12984 (13)0.68961 (14)0.0369 (4)
H40.79960.07310.74700.044*
C50.72373 (9)0.26630 (14)0.27639 (15)0.0392 (4)
H50.71620.25470.19650.047*
C60.52159 (13)0.21659 (15)0.8154 (2)0.0628 (6)
H60.53680.28170.85960.075*
C70.54443 (9)0.11799 (15)0.88668 (16)0.0437 (4)
C80.58766 (10)0.11283 (18)1.02151 (17)0.0522 (5)
H80.60360.17561.07040.063*
C90.60609 (10)0.01630 (19)1.08079 (16)0.0522 (5)
H90.63560.01231.17050.063*
C100.58099 (9)0.07835 (17)1.00709 (15)0.0429 (4)
H100.59360.14431.04940.052*
C110.52200 (8)0.01967 (12)0.81936 (13)0.0312 (4)
Co10.50000.21031 (2)0.75000.03305 (8)
N10.53944 (7)0.07706 (11)0.87848 (11)0.0322 (3)
O10.85225 (7)0.02251 (10)0.52277 (13)0.0548 (3)
O20.79931 (7)0.08974 (9)0.64024 (11)0.0466 (3)
O30.71259 (8)0.04810 (10)0.41253 (12)0.0523 (4)
O40.53359 (7)0.32180 (12)0.89771 (15)0.0656 (4)
H4A0.50490.35000.91590.098*
H4B0.56480.37130.91780.098*
O50.61506 (6)0.21906 (9)0.79332 (11)0.0394 (3)
H5A0.64460.16820.83080.059*
H5B0.64050.27500.81620.059*
S20.78554 (2)0.02258 (3)0.53385 (4)0.03427 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O60.0932 (9)0.1232 (16)0.1006 (10)0.0290 (11)0.0608 (8)0.0182 (10)
C10.0407 (6)0.0264 (7)0.0379 (6)0.0013 (6)0.0219 (5)0.0038 (5)
C20.0274 (5)0.0232 (7)0.0344 (6)0.0021 (5)0.0150 (5)0.0014 (5)
C30.0305 (5)0.0231 (7)0.0378 (6)0.0004 (5)0.0170 (5)0.0008 (5)
C40.0415 (6)0.0289 (7)0.0371 (6)0.0010 (6)0.0199 (5)0.0050 (6)
C50.0478 (7)0.0348 (8)0.0335 (6)0.0003 (7)0.0217 (5)0.0011 (6)
C60.0847 (11)0.0287 (9)0.0812 (11)0.0067 (8)0.0501 (9)0.0116 (8)
C70.0441 (6)0.0397 (9)0.0520 (7)0.0062 (7)0.0296 (5)0.0121 (7)
C80.0451 (7)0.0611 (11)0.0501 (8)0.0106 (8)0.0263 (6)0.0253 (8)
C90.0348 (7)0.0840 (14)0.0320 (7)0.0016 (8)0.0150 (5)0.0156 (8)
C100.0342 (6)0.0587 (11)0.0322 (6)0.0082 (7)0.0162 (5)0.0057 (7)
C110.0297 (5)0.0316 (8)0.0340 (6)0.0010 (5)0.0188 (4)0.0032 (5)
Co10.03179 (11)0.02513 (14)0.04219 (13)0.0000.02060 (9)0.000
N10.0302 (5)0.0354 (7)0.0302 (5)0.0037 (5)0.0163 (4)0.0014 (5)
O10.0607 (5)0.0418 (7)0.0830 (6)0.0173 (5)0.0530 (5)0.0175 (5)
O20.0643 (6)0.0266 (6)0.0546 (5)0.0084 (5)0.0368 (4)0.0107 (4)
O30.0597 (7)0.0294 (6)0.0514 (6)0.0095 (5)0.0208 (5)0.0068 (5)
O40.0556 (5)0.0521 (7)0.1043 (8)0.0211 (6)0.0539 (5)0.0404 (6)
O50.0339 (4)0.0262 (5)0.0552 (6)0.0003 (4)0.0230 (4)0.0014 (4)
S20.04075 (15)0.02087 (17)0.04330 (16)0.00339 (13)0.02474 (13)0.00308 (12)
Geometric parameters (Å, º) top
O6—H6A0.8504C9—C101.402 (3)
O6—H6B0.8501C9—H90.9301
C1—C51.367 (2)C10—N11.331 (2)
C1—C21.422 (2)C10—H100.9300
C1—H10.9300C11—N11.350 (2)
C2—C31.430 (2)C11—C11ii1.437 (3)
C2—C2i1.431 (3)Co1—O42.0902 (15)
C3—C41.366 (2)Co1—O4ii2.0902 (15)
C3—S21.7808 (16)Co1—O5ii2.1177 (13)
C4—C5i1.409 (2)Co1—O52.1177 (13)
C4—H40.9300Co1—N1ii2.1255 (14)
C5—C4i1.409 (2)Co1—N12.1255 (14)
C5—H50.9301O1—S21.4543 (15)
C6—C6ii1.354 (4)O2—S21.4548 (13)
C6—C71.431 (3)O3—S21.4528 (12)
C6—H60.9300O4—H4A0.8206
C7—C81.397 (3)O4—H4B0.8203
C7—C111.407 (2)O5—H5A0.8190
C8—C91.348 (3)O5—H5B0.8196
C8—H80.9300
H6A—O6—H6B103.9N1—C11—C11ii117.02 (8)
C5—C1—C2121.16 (15)C7—C11—C11ii119.67 (10)
C5—C1—H1119.4O4—Co1—O4ii96.93 (9)
C2—C1—H1119.5O4—Co1—O5ii87.97 (5)
C1—C2—C3123.01 (14)O4ii—Co1—O5ii88.13 (5)
C1—C2—C2i118.83 (17)O4—Co1—O588.13 (5)
C3—C2—C2i118.16 (18)O4ii—Co1—O587.97 (5)
C4—C3—C2121.07 (14)O5ii—Co1—O5174.11 (6)
C4—C3—S2118.07 (12)O4—Co1—N1ii168.58 (6)
C2—C3—S2120.84 (12)O4ii—Co1—N1ii93.06 (6)
C3—C4—C5i120.57 (15)O5ii—Co1—N1ii86.83 (5)
C3—C4—H4119.8O5—Co1—N1ii97.78 (5)
C5i—C4—H4119.6O4—Co1—N193.06 (6)
C1—C5—C4i120.22 (16)O4ii—Co1—N1168.58 (6)
C1—C5—H5119.8O5ii—Co1—N197.78 (5)
C4i—C5—H5119.9O5—Co1—N186.83 (5)
C6ii—C6—C7121.03 (11)N1ii—Co1—N177.60 (7)
C6ii—C6—H6119.4C10—N1—C11117.69 (14)
C7—C6—H6119.5C10—N1—Co1128.09 (12)
C8—C7—C11117.04 (17)C11—N1—Co1114.16 (9)
C8—C7—C6123.68 (18)Co1—O4—H4A126.2
C11—C7—C6119.28 (16)Co1—O4—H4B125.7
C9—C8—C7119.74 (18)H4A—O4—H4B99.0
C9—C8—H8119.9Co1—O5—H5A118.4
C7—C8—H8120.3Co1—O5—H5B122.6
C8—C9—C10119.96 (16)H5A—O5—H5B109.2
C8—C9—H9120.1O3—S2—O1112.58 (9)
C10—C9—H9119.9O3—S2—O2112.74 (8)
N1—C10—C9122.24 (18)O1—S2—O2111.85 (8)
N1—C10—H10118.8O3—S2—C3106.21 (7)
C9—C10—H10118.9O1—S2—C3106.41 (8)
N1—C11—C7123.32 (14)O2—S2—C3106.48 (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···AD—HH···AD···AD—H···A
O5—H5B···O2iii0.821.982.7953 (17)176
O5—H5A···O3iv0.821.912.7255 (17)178
O4—H4B···O1iii0.821.952.7660 (19)174
O4—H4A···O6v0.821.862.663 (3)166
O6—H6B···O2vi0.852.052.896 (2)179
O6—H6A···O1vii0.851.972.821 (3)179
Symmetry codes: (iii) x+3/2, y+1/2, z+3/2; (iv) x, y, z+1/2; (v) x1/2, y1/2, 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
Mr633.52
Crystal system, space groupMonoclinic, C2/c
Temperature (K)293
a, b, c (Å)20.578 (4), 12.431 (3), 12.462 (3)
β (°) 123.867 (2)
V3)2647.0 (10)
Z4
Radiation typeMo Kα
µ (mm1)0.87
Crystal size (mm)0.40 × 0.35 × 0.32
Data collection
DiffractometerCCD area-detector
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
8365, 2590, 2353
Rint0.018
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.098, 1.07
No. of reflections2590
No. of parameters177
No. of restraints6
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.77, 0.42

Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 2003), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Siemens, 1996).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5B···O2i0.821.982.7953 (17)176.1
O5—H5A···O3ii0.821.912.7255 (17)178.1
O4—H4B···O1i0.821.952.7660 (19)173.8
O4—H4A···O6iii0.821.862.663 (3)165.9
O6—H6B···O2iv0.852.052.896 (2)179.2
O6—H6A···O1v0.851.972.821 (3)179.0
Symmetry codes: (i) x+3/2, y+1/2, z+3/2; (ii) x, y, z+1/2; (iii) x1/2, y1/2, z; (iv) x, y+1, z; (v) x, y+1, z+1/2.
 

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