Buy article online - an online subscription or single-article purchase is required to access this article.
share
share
Issue contentsclose
Statistics
close
Download citation
closeDownload citation
Format BIBTeX
EndNote
RefMan
Refer
Medline
CIF
SGML
Text
Plain Text
Supporting information
Supporting informationclose
Download PDF of article
Download PDF of articleclose
Acta Cryst. (2007). E63, m2413
https://doi.org/10.1107/S1600536807040913
Download PDF of article
Download PDF of articleclose
Supporting information
Supporting informationclose
Download citation
closeDownload citation
Format BIBTeX
EndNote
RefMan
Refer
Medline
CIF
SGML
Text
Plain Text
Statistics
close
Issue contentsclose
share
link to html

Tetra­aqua­bis(4,4′-bipyridine)cobalt(II) 2-aminona­phthalene-1-sulfonate hexa­hydrate

M.-J. Wu, P.-X. Dai, X.-G. Wang, E.-C. Yang and X.-J. Zhao
The title compound, [Co(C10H8N2)2(H2O)4](C10H8NO3S)2·6H2O, contains a tetra­aqua­bis(4,4′-bipyridine)­cobalt(II) cation, two ANS− anions (HANS = 2-amino­naphthalene-1-sulfonic acid) and six solvent water mol­ecules. The CoII atom lies on an inversion centre and is coordinated octahedrally by two mutually trans 4,4′-bipyridine mol­ecules bound in a monodentate fashion and by four water mol­ecules in the equatorial plane. The cations and water mol­ecules are arranged into infinite two-dimensional layers by an extensive network of hydrogen bonds. The ANS− anions are trapped between these layers via N—H...O inter­actions between the amino groups and the solvent and coordinated water mol­ecules. Adjacent layers are stacked via weak π–π inter­actions between 4,4′-bipyridine mol­ecules [nearest centroid-to-centroid distance 3.662 (0) Å].
Read articleSimilar articles

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807040913/sj2334sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807040913/sj2334Isup2.hkl
Contains datablock I

CCDC reference: 660161

checkCIF report

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.039
  • wR factor = 0.109
  • Data-to-parameter ratio = 13.6

checkCIF/PLATON results

No syntax errors found




Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical .          ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         C1
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         C2
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         N1
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         N2
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         C5
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         C6
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         S1
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.84
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2B    ..  S1      ..       2.93 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H6B    ..  S1      ..       3.03 Ang.
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          5
            N1  -CO1 -N1  -C3      9.00  0.00   3.666   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         10
            N1  -CO1 -N1  -C2      8.00  0.00   3.666   1.555   1.555   1.555


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
PLAT794_ALERT_5_G Check Predicted Bond Valency for Co1         (2)       1.83


   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
  15 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   8 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
   4 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check
Comment top

The asymmetric unit of the title complex (Fig. 1) contains half of a CoII center, one monodentate 4,4'-bipyridine ligand, one free ANS- anion, two coordinated water (O1 and O2) and three lattice water molecules (O6, O7 and O8). The CoII atom, which lies on an inversion center, is six-coordinated to four oxygen atoms from four coordinated water molecules and two nitrogen atoms from two 4,4'-bipyridine ligands, exhibiting a nearly ideal octahedral coordination geometry. The isolated cations are connected to three lattice water molecules by extensive O—H···O hydrogen bonds interactions to generate a two-dimensional CoII–H2O layer (Fig. 2 and Table 1). And these adjacent two-dimensional layers are further stacked together by weak π–π interactions between interlayer 4,4'-bipy, exhibiting three-dimensional interdigitated supramoleuclar architectures. The nearest centroid-to-centroid distance is 3.662 (0) Å. Free ANS anions are tightly encapsulated in the channels of the three-dimensional packing structure via N—H···O interactions between amino groups and the lattice as well as coordinated water molecules (Fig. 3 and Table 2).

Related literature top

For details of the role of water molecules in self-assembly processes, see Tajkhorshid et al. (2002). For investigations of water-based clusters assembled by hydrogen bonds, see: Yoshizawa et al. (2005); Sreenivasulu & Vittal (2004).

Experimental top

The title complex was synthesized by dissolving Co(CH3COO)24H2O (99.6 mg, 0.4 mmol), 4,4'-bipyridine (38.4 mg, 0.2 mmol), HANS (89.3 mg, 0.4 mmol), NaOH (24 mg, 0.6 mmol), and H2O (15 ml) in a 23 ml Teflon lined autoclave under autogenous pressure at 140°C for 2 days. The mixture was slowly cooled to room temperature at a rate of 5 K h-1, pale-red block-shaped crystals suitable for X-ray analysis were obtained in 33% yield. Analysis calculated for C40H52CoN6O16S2: C 48.24, H 5.26, N 8.44%; found: C 48.20, H 5.38, N 8.62%.

Refinement top

H atoms were initially located in difference maps, but were subsequently introduced in calculated positions and treated as riding, with C—H = 0.93, O—H = 0.85 and N—H = 0.86 Å. All H atoms were allocated displacement parameters related to those of their parent atoms [Uiso(H) = 1.2Ueq(C, N), or 1.5Ueq(O)].

Structure description top

The asymmetric unit of the title complex (Fig. 1) contains half of a CoII center, one monodentate 4,4'-bipyridine ligand, one free ANS- anion, two coordinated water (O1 and O2) and three lattice water molecules (O6, O7 and O8). The CoII atom, which lies on an inversion center, is six-coordinated to four oxygen atoms from four coordinated water molecules and two nitrogen atoms from two 4,4'-bipyridine ligands, exhibiting a nearly ideal octahedral coordination geometry. The isolated cations are connected to three lattice water molecules by extensive O—H···O hydrogen bonds interactions to generate a two-dimensional CoII–H2O layer (Fig. 2 and Table 1). And these adjacent two-dimensional layers are further stacked together by weak π–π interactions between interlayer 4,4'-bipy, exhibiting three-dimensional interdigitated supramoleuclar architectures. The nearest centroid-to-centroid distance is 3.662 (0) Å. Free ANS anions are tightly encapsulated in the channels of the three-dimensional packing structure via N—H···O interactions between amino groups and the lattice as well as coordinated water molecules (Fig. 3 and Table 2).

For details of the role of water molecules in self-assembly processes, see Tajkhorshid et al. (2002). For investigations of water-based clusters assembled by hydrogen bonds, see: Yoshizawa et al. (2005); Sreenivasulu & Vittal (2004).

Computing details top

Data collection: APEX2 (Bruker, 2003); cell refinement: APEX2; 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 (Bruker, 2003); software used to prepare material for publication: SHELXTL and DIAMOND (Brandenburg & Berndt, 1999).

Figures top
[Figure 1] Fig. 1. The structure of the title compound with thermal ellipsoids drawn at the 30% probability level.
[Figure 2] Fig. 2. The two dimensional layer structure formed by O—H···O hydrogen bonds (dashed lines) between the complex molecules and the water solvates.
[Figure 3] Fig. 3. Packing diagram for the title complex.
Tetraaquabis(4,4'-bipyridine)cobalt(II) 2-aminonaphthalene-1-sulfonate hexahydrate top
Crystal data top
[Co(C10H8N2)2(H2O)4](C10H8NO3S)2·6H2OF(000) = 1042
Mr = 995.93Dx = 1.450 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3808 reflections
a = 12.4737 (14) Åθ = 2.3–25.1°
b = 18.358 (2) ŵ = 0.54 mm−1
c = 10.9196 (13) ÅT = 293 K
β = 114.148 (1)°Block, pale red
V = 2281.7 (5) Å30.32 × 0.28 × 0.22 mm
Z = 2
Data collection top
Bruker APEXII CCD area-detector
diffractometer		4021 independent reflections
Radiation source: fine-focus sealed tube3270 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
φ and ω scansθmax = 25.0°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −14→12
Tmin = 0.840, Tmax = 0.887k = −19→21
12190 measured reflectionsl = −12→13
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)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.109H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0583P)2 + 1.0964P]
where P = (Fo2 + 2Fc2)/3
4021 reflections(Δ/σ)max = 0.001
295 parametersΔρmax = 0.48 e Å−3
0 restraintsΔρmin = −0.29 e Å−3
Crystal data top
[Co(C10H8N2)2(H2O)4](C10H8NO3S)2·6H2OV = 2281.7 (5) Å3
Mr = 995.93Z = 2
Monoclinic, P21/cMo Kα radiation
a = 12.4737 (14) ŵ = 0.54 mm−1
b = 18.358 (2) ÅT = 293 K
c = 10.9196 (13) Å0.32 × 0.28 × 0.22 mm
β = 114.148 (1)°
Data collection top
Bruker APEXII CCD area-detector
diffractometer		4021 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		3270 reflections with I > 2σ(I)
Tmin = 0.840, Tmax = 0.887Rint = 0.019
12190 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0390 restraints
wR(F2) = 0.109H-atom parameters constrained
S = 1.05Δρmax = 0.48 e Å−3
4021 reflectionsΔρmin = −0.29 e Å−3
295 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
Co10.50000.50000.50000.03414 (14)
S10.68106 (5)0.61872 (4)−0.02091 (6)0.04513 (18)
O10.44371 (14)0.57897 (9)0.34621 (16)0.0459 (4)
H1A0.43930.56950.26810.069*
H1B0.44800.62390.36680.069*
O20.48301 (14)0.57884 (10)0.62652 (17)0.0498 (4)
H2A0.41840.58720.63260.075*
H2B0.54420.59390.69190.075*
O30.7056 (2)0.54311 (11)0.0094 (2)0.0897 (8)
O40.67303 (18)0.63600 (12)−0.15273 (18)0.0664 (6)
O50.57611 (19)0.64226 (16)−0.0080 (3)0.0948 (8)
N10.31765 (16)0.46586 (11)0.44211 (19)0.0387 (4)
N2−0.27372 (18)0.40516 (14)0.3473 (2)0.0551 (6)
N30.6869 (3)0.73128 (17)0.1974 (3)0.0915 (10)
H3A0.62340.70880.14810.110*
H3B0.68620.76290.25510.110*
C10.1718 (2)0.39321 (19)0.4720 (4)0.0805 (11)
H10.15580.35210.51150.097*
C20.2858 (2)0.40909 (18)0.4935 (4)0.0777 (11)
H20.34440.37770.54790.093*
C30.2301 (2)0.50586 (18)0.3617 (3)0.0679 (9)
H30.24790.54510.31930.081*
C40.1139 (2)0.49405 (18)0.3355 (3)0.0661 (9)
H40.05670.52510.27770.079*
C50.08187 (19)0.43739 (13)0.3932 (2)0.0378 (5)
C6−0.04222 (19)0.42505 (13)0.3733 (2)0.0388 (5)
C7−0.1325 (2)0.4684 (2)0.2911 (3)0.0686 (9)
H7−0.11810.50560.24210.082*
C8−0.2450 (2)0.4563 (2)0.2816 (3)0.0740 (10)
H8−0.30460.48650.22500.089*
C9−0.1865 (3)0.36315 (18)0.4241 (4)0.0726 (9)
H9−0.20350.32590.47110.087*
C10−0.0719 (2)0.37078 (16)0.4394 (4)0.0661 (9)
H10−0.01460.33890.49480.079*
C110.8024 (2)0.66754 (12)0.0958 (2)0.0384 (5)
C120.9161 (2)0.65456 (12)0.0952 (2)0.0389 (5)
C130.9385 (2)0.60407 (14)0.0116 (3)0.0482 (6)
H130.87730.5756−0.04680.058*
C141.0489 (3)0.59610 (18)0.0148 (3)0.0685 (9)
H141.06110.5625−0.04210.082*
C151.1428 (3)0.6372 (2)0.1010 (4)0.0785 (11)
H151.21720.63130.10200.094*
C161.1250 (3)0.6855 (2)0.1833 (4)0.0723 (10)
H161.18800.71300.24130.087*
C171.0133 (2)0.69561 (15)0.1836 (3)0.0525 (7)
C180.9945 (3)0.74661 (16)0.2700 (3)0.0676 (9)
H181.05750.77420.32770.081*
C190.8892 (3)0.75618 (16)0.2710 (3)0.0695 (9)
H190.88110.78970.33040.083*
C200.7885 (3)0.71681 (15)0.1840 (3)0.0544 (7)
O60.4298 (2)0.57428 (12)0.0930 (2)0.0804 (7)
H6A0.49920.56250.10420.121*
H6B0.37810.54190.05520.121*
O70.4464 (2)0.73225 (13)0.3298 (3)0.0924 (8)
H7A0.42820.73340.24580.139*
H7B0.50770.75540.37980.139*
O80.3637 (3)0.72911 (17)0.0418 (3)0.1175 (11)
H8A0.36430.68690.01000.176*
H8B0.40630.76110.02720.176*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0231 (2)0.0467 (3)0.0319 (2)−0.00243 (18)0.01052 (17)−0.00211 (18)
S10.0398 (3)0.0500 (4)0.0410 (3)−0.0111 (3)0.0118 (3)0.0024 (3)
O10.0433 (10)0.0538 (10)0.0381 (9)−0.0024 (8)0.0142 (8)0.0024 (7)
O20.0274 (8)0.0727 (12)0.0491 (10)−0.0074 (8)0.0156 (7)−0.0223 (9)
O30.0922 (17)0.0486 (12)0.0858 (16)−0.0270 (12)−0.0068 (13)0.0134 (11)
O40.0602 (12)0.0839 (14)0.0397 (10)−0.0284 (11)0.0045 (9)0.0050 (9)
O50.0512 (13)0.140 (2)0.0998 (18)−0.0185 (14)0.0372 (13)−0.0230 (17)
N10.0286 (10)0.0476 (12)0.0395 (10)−0.0019 (9)0.0137 (8)−0.0020 (9)
N20.0327 (12)0.0803 (16)0.0553 (13)−0.0074 (11)0.0210 (10)−0.0121 (12)
N30.088 (2)0.096 (2)0.108 (2)0.0034 (17)0.0578 (19)−0.0365 (19)
C10.0311 (14)0.081 (2)0.118 (3)0.0009 (14)0.0194 (16)0.052 (2)
C20.0289 (14)0.073 (2)0.119 (3)0.0047 (14)0.0177 (16)0.042 (2)
C30.0308 (14)0.094 (2)0.0695 (19)−0.0048 (14)0.0112 (13)0.0424 (17)
C40.0277 (13)0.088 (2)0.0715 (19)0.0032 (13)0.0088 (13)0.0391 (17)
C50.0274 (11)0.0475 (13)0.0384 (12)−0.0032 (10)0.0134 (10)−0.0062 (10)
C60.0286 (11)0.0496 (14)0.0386 (12)−0.0023 (10)0.0141 (10)−0.0088 (10)
C70.0346 (14)0.116 (3)0.0572 (17)0.0102 (16)0.0207 (13)0.0350 (18)
C80.0301 (14)0.134 (3)0.0538 (17)0.0148 (17)0.0131 (13)0.0266 (19)
C90.0471 (17)0.0645 (19)0.119 (3)−0.0043 (15)0.0465 (19)0.0164 (19)
C100.0398 (15)0.0577 (17)0.106 (2)0.0045 (13)0.0355 (16)0.0215 (17)
C110.0403 (13)0.0358 (12)0.0348 (12)−0.0024 (10)0.0110 (10)0.0018 (10)
C120.0398 (13)0.0364 (12)0.0350 (12)−0.0005 (10)0.0095 (10)0.0108 (10)
C130.0502 (15)0.0450 (14)0.0478 (14)0.0072 (12)0.0186 (12)0.0082 (11)
C140.072 (2)0.072 (2)0.073 (2)0.0298 (18)0.0413 (18)0.0262 (17)
C150.0443 (18)0.097 (3)0.096 (3)0.0162 (18)0.0308 (19)0.047 (2)
C160.0393 (16)0.081 (2)0.079 (2)−0.0086 (15)0.0064 (15)0.0287 (19)
C170.0467 (16)0.0482 (15)0.0477 (14)−0.0069 (12)0.0043 (12)0.0140 (12)
C180.073 (2)0.0526 (18)0.0506 (16)−0.0213 (15)−0.0014 (15)−0.0064 (14)
C190.093 (3)0.0526 (18)0.0548 (17)−0.0071 (17)0.0224 (17)−0.0175 (14)
C200.0661 (18)0.0461 (15)0.0519 (15)0.0029 (13)0.0252 (14)−0.0023 (12)
O60.1082 (18)0.0777 (15)0.0730 (14)−0.0410 (13)0.0551 (14)−0.0252 (12)
O70.1018 (19)0.0765 (16)0.1005 (19)−0.0156 (14)0.0430 (16)−0.0103 (14)
O80.127 (3)0.102 (2)0.161 (3)0.0241 (18)0.098 (2)0.018 (2)
Geometric parameters (Å, º) top
Co1—O2i2.0708 (16)C6—C71.371 (4)
Co1—O22.0708 (16)C7—C81.382 (4)
Co1—O1i2.1096 (16)C7—H70.9300
Co1—O12.1096 (16)C8—H80.9300
Co1—N1i2.1885 (18)C9—C101.377 (4)
Co1—N12.1885 (18)C9—H90.9300
S1—O31.431 (2)C10—H100.9300
S1—O41.4369 (19)C11—C201.383 (3)
S1—O51.439 (2)C11—C121.441 (3)
S1—C111.772 (2)C12—C131.406 (4)
O1—H1A0.8499C12—C171.419 (3)
O1—H1B0.8500C13—C141.372 (4)
O2—H2A0.8501C13—H130.9300
O2—H2B0.8500C14—C151.387 (5)
N1—C31.311 (3)C14—H140.9300
N1—C21.320 (3)C15—C161.345 (5)
N2—C91.317 (4)C15—H150.9300
N2—C81.318 (4)C16—C171.406 (4)
N3—C201.360 (4)C16—H160.9300
N3—H3A0.8600C17—C181.416 (4)
N3—H3B0.8600C18—C191.329 (5)
C1—C51.367 (4)C18—H180.9300
C1—C21.374 (4)C19—C201.424 (4)
C1—H10.9300C19—H190.9300
C2—H20.9300O6—H6A0.8505
C3—C41.375 (4)O6—H6B0.8502
C3—H30.9300O7—H7A0.8501
C4—C51.358 (4)O7—H7B0.8500
C4—H40.9300O8—H8A0.8501
C5—C61.490 (3)O8—H8B0.8501
C6—C101.368 (4)
O2i—Co1—O2180.0C10—C6—C7116.2 (2)
O2i—Co1—O1i87.66 (7)C10—C6—C5121.6 (2)
O2—Co1—O1i92.34 (7)C7—C6—C5122.2 (2)
O2i—Co1—O192.34 (7)C6—C7—C8119.6 (3)
O2—Co1—O187.66 (7)C6—C7—H7120.2
O1i—Co1—O1180.0C8—C7—H7120.2
O2i—Co1—N1i90.85 (7)N2—C8—C7124.6 (3)
O2—Co1—N1i89.15 (7)N2—C8—H8117.7
O1i—Co1—N1i89.93 (7)C7—C8—H8117.7
O1—Co1—N1i90.07 (7)N2—C9—C10124.3 (3)
O2i—Co1—N189.15 (7)N2—C9—H9117.9
O2—Co1—N190.85 (7)C10—C9—H9117.9
O1i—Co1—N190.07 (7)C6—C10—C9120.2 (3)
O1—Co1—N189.93 (7)C6—C10—H10119.9
N1i—Co1—N1180.00 (11)C9—C10—H10119.9
O3—S1—O4111.52 (15)C20—C11—C12121.0 (2)
O3—S1—O5112.69 (17)C20—C11—S1121.2 (2)
O4—S1—O5109.78 (15)C12—C11—S1117.77 (17)
O3—S1—C11106.57 (12)C13—C12—C17116.8 (2)
O4—S1—C11107.32 (11)C13—C12—C11124.6 (2)
O5—S1—C11108.73 (13)C17—C12—C11118.6 (2)
Co1—O1—H1A121.5C14—C13—C12121.2 (3)
Co1—O1—H1B119.4C14—C13—H13119.4
H1A—O1—H1B115.7C12—C13—H13119.4
Co1—O2—H2A122.6C13—C14—C15121.3 (3)
Co1—O2—H2B119.1C13—C14—H14119.4
H2A—O2—H2B115.5C15—C14—H14119.4
C3—N1—C2114.4 (2)C16—C15—C14119.2 (3)
C3—N1—Co1121.05 (17)C16—C15—H15120.4
C2—N1—Co1124.17 (17)C14—C15—H15120.4
C9—N2—C8115.3 (2)C15—C16—C17121.5 (3)
C20—N3—H3A120.0C15—C16—H16119.2
C20—N3—H3B120.0C17—C16—H16119.2
H3A—N3—H3B120.0C16—C17—C18121.5 (3)
C5—C1—C2120.5 (3)C16—C17—C12120.0 (3)
C5—C1—H1119.8C18—C17—C12118.4 (3)
C2—C1—H1119.8C19—C18—C17121.8 (3)
N1—C2—C1124.4 (3)C19—C18—H18119.1
N1—C2—H2117.8C17—C18—H18119.1
C1—C2—H2117.8C18—C19—C20122.2 (3)
N1—C3—C4124.7 (2)C18—C19—H19118.9
N1—C3—H3117.6C20—C19—H19118.9
C4—C3—H3117.6N3—C20—C11126.2 (3)
C5—C4—C3120.6 (2)N3—C20—C19115.8 (3)
C5—C4—H4119.7C11—C20—C19118.0 (3)
C3—C4—H4119.7H6A—O6—H6B114.7
C4—C5—C1115.2 (2)H7A—O7—H7B116.9
C4—C5—C6122.3 (2)H8A—O8—H8B116.3
C1—C5—C6122.5 (2)
O2i—Co1—N1—C3−106.1 (2)N2—C9—C10—C60.5 (6)
O2—Co1—N1—C373.9 (2)O3—S1—C11—C20−119.3 (2)
O1i—Co1—N1—C3166.3 (2)O4—S1—C11—C20121.1 (2)
O1—Co1—N1—C3−13.7 (2)O5—S1—C11—C202.4 (3)
N1i—Co1—N1—C394 (100)O3—S1—C11—C1261.1 (2)
O2i—Co1—N1—C281.0 (3)O4—S1—C11—C12−58.5 (2)
O2—Co1—N1—C2−99.0 (3)O5—S1—C11—C12−177.19 (19)
O1i—Co1—N1—C2−6.7 (3)C20—C11—C12—C13178.2 (2)
O1—Co1—N1—C2173.3 (3)S1—C11—C12—C13−2.2 (3)
N1i—Co1—N1—C2−79 (100)C20—C11—C12—C17−2.5 (3)
C3—N1—C2—C1−2.9 (5)S1—C11—C12—C17177.12 (17)
Co1—N1—C2—C1170.4 (3)C17—C12—C13—C14−1.0 (3)
C5—C1—C2—N1−0.1 (6)C11—C12—C13—C14178.4 (2)
C2—N1—C3—C43.3 (5)C12—C13—C14—C150.4 (4)
Co1—N1—C3—C4−170.3 (3)C13—C14—C15—C160.2 (5)
N1—C3—C4—C5−0.6 (6)C14—C15—C16—C17−0.2 (5)
C3—C4—C5—C1−2.5 (5)C15—C16—C17—C18−179.9 (3)
C3—C4—C5—C6176.6 (3)C15—C16—C17—C12−0.4 (4)
C2—C1—C5—C42.8 (5)C13—C12—C17—C160.9 (3)
C2—C1—C5—C6−176.3 (3)C11—C12—C17—C16−178.5 (2)
C4—C5—C6—C10−175.4 (3)C13—C12—C17—C18−179.5 (2)
C1—C5—C6—C103.7 (4)C11—C12—C17—C181.1 (3)
C4—C5—C6—C72.7 (4)C16—C17—C18—C19−179.8 (3)
C1—C5—C6—C7−178.2 (3)C12—C17—C18—C190.7 (4)
C10—C6—C7—C81.3 (5)C17—C18—C19—C20−1.0 (5)
C5—C6—C7—C8−176.9 (3)C12—C11—C20—N3−177.1 (3)
C9—N2—C8—C7−1.3 (5)S1—C11—C20—N33.3 (4)
C6—C7—C8—N20.2 (6)C12—C11—C20—C192.1 (4)
C8—N2—C9—C100.9 (5)S1—C11—C20—C19−177.4 (2)
C7—C6—C10—C9−1.6 (5)C18—C19—C20—N3179.0 (3)
C5—C6—C10—C9176.6 (3)C18—C19—C20—C11−0.4 (4)
Symmetry code: (i) −x+1, −y+1, −z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O60.851.872.700 (3)166
O1—H1B···O70.852.032.821 (3)155
O2—H2A···N2ii0.851.912.756 (3)174
O2—H2B···O4iii0.851.962.803 (2)173
O2—H2B···S1iii0.852.933.6985 (18)152
N3—H3A···O50.861.982.660 (4)135
N3—H3B···O4iv0.862.152.980 (3)162
O6—H6A···O50.852.352.784 (3)112
O6—H6B···O3v0.851.852.684 (3)167
O6—H6B···S1v0.853.033.768 (2)147
O7—H7A···O80.852.042.881 (5)172
O7—H7B···O5iv0.852.212.953 (4)145
O8—H8A···O60.852.272.949 (4)137
O8—H8B···O7vi0.852.412.980 (4)125
Symmetry codes: (ii) −x, −y+1, −z+1; (iii) x, y, z+1; (iv) x, −y+3/2, z+1/2; (v) −x+1, −y+1, −z; (vi) x, −y+3/2, z−1/2.

Experimental details

Crystal data
Chemical formula[Co(C10H8N2)2(H2O)4](C10H8NO3S)2·6H2O
Mr995.93
Crystal system, space groupMonoclinic, P21/c
Temperature (K)293
a, b, c (Å)12.4737 (14), 18.358 (2), 10.9196 (13)
β (°) 114.148 (1)
V (Å3)2281.7 (5)
Z2
Radiation typeMo Kα
µ (mm−1)0.54
Crystal size (mm)0.32 × 0.28 × 0.22
Data collection
DiffractometerBruker APEXII CCD area-detector
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.840, 0.887
No. of measured, independent and
observed [I > 2σ(I)] reflections		12190, 4021, 3270
Rint0.019
(sin θ/λ)max (Å−1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.039, 0.109, 1.05
No. of reflections4021
No. of parameters295
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.48, −0.29

Computer programs: APEX2 (Bruker, 2003), APEX2, SAINT (Bruker, 2003), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2003), SHELXTL and DIAMOND (Brandenburg & Berndt, 1999).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O60.851.872.700 (3)165.6
O1—H1B···O70.852.032.821 (3)154.6
O2—H2A···N2i0.851.912.756 (3)173.5
O2—H2B···O4ii0.851.962.803 (2)173.4
O2—H2B···S1ii0.852.933.6985 (18)151.6
N3—H3A···O50.861.982.660 (4)135.1
N3—H3B···O4iii0.862.152.980 (3)162.3
O6—H6A···O50.852.352.784 (3)112.0
O6—H6B···O3iv0.851.852.684 (3)166.8
O6—H6B···S1iv0.853.033.768 (2)147.1
O7—H7A···O80.852.042.881 (5)172.0
O7—H7B···O5iii0.852.212.953 (4)145.2
O8—H8A···O60.852.272.949 (4)136.7
O8—H8B···O7v0.852.412.980 (4)125.3
Symmetry codes: (i) −x, −y+1, −z+1; (ii) x, y, z+1; (iii) x, −y+3/2, z+1/2; (iv) −x+1, −y+1, −z; (v) x, −y+3/2, z−1/2.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
E-alerts
Follow Acta Cryst. on Twitter
Twitter
Follow us on facebook
Facebook
Sign up for RSS feeds
RSS