Download citation
Download citation
link to html
By reaction of cobalt(II) sulfate with 5-hydroxy­isophthalic acid and 2,2′-bi­pyridine in a water–di­methyl­form­amide solution, the title novel sulfate-anion-bridged inorganic–organic hybrid, [Co(C10H8N2)(H2O)2SO4]n, has been synthesized. Structural characterization of the complex shows that it displays a polymeric linear structure, formed by sulfate bridges between six-coordinate CoII ions that lie on twofold rotation axes. Hydrogen bonding between chains results in a two-dimensional framework stucture.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804019038/cv6350sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804019038/cv6350Isup2.hkl
Contains datablock I

CCDC reference: 251609

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.027
  • wR factor = 0.071
  • Data-to-parameter ratio = 11.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 3 O3 -CO1 -N1 -C5 148.60 0.40 2.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 8 O3 -CO1 -N1 -C1 -30.60 0.50 2.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 29 O1 -CO1 -O1 -S1 150.93 0.17 2.555 1.555 1.555 1.555
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 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

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) and XP in SHELXTL (Bruker, 2002); software used to prepare material for publication: SHELXL97.

catena-Poly[[diaqua(2,2'-bipyridine-κ2N,N')cobalt(II)]-µ-sulfato] top
Crystal data top
[Co(C10H8N2)(H2O)2]SO4F(000) = 708
Mr = 347.21Dx = 1.801 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C2ycCell parameters from 1150 reflections
a = 15.524 (12) Åθ = 2.8–25.2°
b = 12.802 (10) ŵ = 1.53 mm1
c = 6.601 (5) ÅT = 298 K
β = 102.56 (3)°Prism, pink
V = 1280.5 (17) Å30.30 × 0.10 × 0.08 mm
Z = 4
Data collection top
Bruker APEX CCD area-detector
diffractometer
1150 independent reflections
Radiation source: fine-focus sealed tube1116 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.018
φ and ω scansθmax = 25.2°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1817
Tmin = 0.629, Tmax = 0.885k = 1515
3266 measured reflectionsl = 77
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)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.071H atoms treated by a mixture of independent and constrained refinement
S = 1.13 w = 1/[σ2(Fo2) + (0.0321P)2 + 1.982P]
where P = (Fo2 + 2Fc2)/3
1150 reflections(Δ/σ)max < 0.001
97 parametersΔρmax = 0.32 e Å3
0 restraintsΔρmin = 0.32 e Å3
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
O30.09775 (12)0.61282 (14)0.2508 (3)0.0289 (4)
H30.10060.59940.13100.043*
C40.22810 (16)0.9334 (2)0.3151 (4)0.0371 (6)
H40.28890.92630.33370.045*
C30.18946 (18)1.0309 (2)0.3041 (4)0.0357 (6)
H3A0.22411.09070.31400.043*
C20.09889 (17)1.03913 (18)0.2782 (4)0.0295 (5)
H20.07201.10430.27120.035*
Co10.00000.72499 (3)0.25000.02029 (16)
S10.00000.65952 (6)0.25000.0235 (2)
N10.08648 (12)0.85289 (14)0.2726 (3)0.0228 (4)
C10.04876 (15)0.94849 (17)0.2628 (3)0.0223 (5)
C50.17439 (16)0.84696 (19)0.2978 (4)0.0310 (5)
H50.20030.78120.30400.037*
O20.07670 (11)0.59307 (13)0.3397 (3)0.0337 (4)
O10.02089 (13)0.72654 (12)0.0852 (2)0.0326 (4)
H10.0907 (19)0.560 (2)0.289 (5)0.035 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O30.0372 (10)0.0215 (9)0.0277 (9)0.0041 (8)0.0063 (8)0.0031 (8)
C40.0267 (13)0.0518 (16)0.0329 (15)0.0084 (12)0.0065 (11)0.0008 (13)
C30.0416 (15)0.0369 (14)0.0286 (14)0.0168 (11)0.0078 (11)0.0020 (11)
C20.0413 (14)0.0223 (11)0.0245 (13)0.0055 (10)0.0063 (11)0.0006 (9)
Co10.0259 (3)0.0170 (2)0.0186 (2)0.0000.00612 (17)0.000
S10.0365 (5)0.0182 (4)0.0176 (4)0.0000.0102 (3)0.000
N10.0258 (10)0.0233 (10)0.0195 (10)0.0009 (8)0.0053 (8)0.0017 (7)
C10.0311 (13)0.0221 (11)0.0139 (11)0.0015 (9)0.0055 (9)0.0006 (8)
C50.0288 (12)0.0342 (13)0.0299 (13)0.0034 (11)0.0060 (10)0.0024 (10)
O20.0403 (10)0.0314 (9)0.0301 (9)0.0097 (8)0.0095 (8)0.0036 (7)
O10.0544 (11)0.0271 (9)0.0178 (9)0.0153 (8)0.0112 (8)0.0024 (6)
Geometric parameters (Å, º) top
O3—Co12.088 (2)Co1—N1i2.102 (2)
O3—H30.8200Co1—O12.166 (2)
O3—H10.74 (3)Co1—O1i2.166 (2)
C4—C51.375 (4)S1—O11.4758 (17)
C4—C31.380 (4)S1—O1ii1.4758 (17)
C4—H40.9300S1—O21.4783 (19)
C3—C21.383 (4)S1—O2ii1.4783 (19)
C3—H3A0.9300N1—C51.341 (3)
C2—C11.389 (3)N1—C11.352 (3)
C2—H20.9300C1—C1i1.486 (5)
Co1—O3i2.088 (2)C5—H50.9300
Co1—N12.102 (2)
Co1—O3—H3109.5O3i—Co1—O1i87.49 (7)
Co1—O3—H1118 (2)O3—Co1—O1i93.24 (7)
H3—O3—H1100.4N1—Co1—O1i88.23 (7)
C5—C4—C3118.3 (2)N1i—Co1—O1i90.96 (7)
C5—C4—H4120.8O1—Co1—O1i178.95 (8)
C3—C4—H4120.8O1—S1—O1ii108.91 (14)
C4—C3—C2119.6 (2)O1—S1—O2110.04 (11)
C4—C3—H3A120.2O1ii—S1—O2109.06 (10)
C2—C3—H3A120.2O1—S1—O2ii109.06 (10)
C3—C2—C1119.0 (2)O1ii—S1—O2ii110.04 (11)
C3—C2—H2120.5O2—S1—O2ii109.73 (15)
C1—C2—H2120.5C5—N1—C1118.4 (2)
O3i—Co1—O393.11 (12)C5—N1—Co1125.59 (16)
O3i—Co1—N1171.24 (7)C1—N1—Co1116.00 (16)
O3—Co1—N194.76 (9)N1—C1—C2121.5 (2)
O3i—Co1—N1i94.76 (9)N1—C1—C1i115.17 (12)
O3—Co1—N1i171.24 (7)C2—C1—C1i123.31 (14)
N1—Co1—N1i77.67 (12)N1—C5—C4123.2 (2)
O3i—Co1—O193.24 (7)N1—C5—H5118.4
O3—Co1—O187.49 (7)C4—C5—H5118.4
N1—Co1—O190.96 (7)S1—O1—Co1137.71 (10)
N1i—Co1—O188.23 (7)
C5—C4—C3—C20.6 (4)Co1—N1—C1—C1i0.1 (3)
C4—C3—C2—C10.3 (4)C3—C2—C1—N10.0 (3)
O3i—Co1—N1—C5148.6 (4)C3—C2—C1—C1i179.3 (3)
O3—Co1—N1—C55.27 (19)C1—N1—C5—C40.3 (4)
N1i—Co1—N1—C5179.2 (2)Co1—N1—C5—C4178.90 (18)
O1—Co1—N1—C592.82 (19)C3—C4—C5—N10.6 (4)
O1i—Co1—N1—C587.83 (19)O1ii—S1—O1—Co1143.3 (2)
O3i—Co1—N1—C130.6 (5)O2—S1—O1—Co197.17 (18)
O3—Co1—N1—C1175.56 (16)O2ii—S1—O1—Co123.2 (2)
N1i—Co1—N1—C10.03 (11)O3i—Co1—O1—S175.58 (19)
O1—Co1—N1—C188.00 (16)O3—Co1—O1—S117.40 (17)
O1i—Co1—N1—C191.34 (16)N1—Co1—O1—S1112.12 (19)
C5—N1—C1—C20.0 (3)N1i—Co1—O1—S1170.24 (18)
Co1—N1—C1—C2179.27 (17)O1i—Co1—O1—S1150.93 (17)
C5—N1—C1—C1i179.3 (2)
Symmetry codes: (i) x, y, z+1/2; (ii) x, y, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H1···O2iii0.74 (3)2.01 (3)2.735 (3)169 (3)
O3—H3···S10.822.773.377 (3)133
O3—H3···O2ii0.821.882.674 (3)163
Symmetry codes: (ii) x, y, z1/2; (iii) x, y+1, z.
 

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