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In the title complex, [Co(C5H5N)2(H2O)4](C2H3O2)2, the octa­hedral cation is hydrogen bonded to the acetate anions via the coordinated water mol­ecules. The cation and anions lie on a crystallographic mirror plane.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806010257/tk2017sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806010257/tk2017Isup2.hkl
Contains datablock I

CCDC reference: 605200

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.023
  • wR factor = 0.065
  • Data-to-parameter ratio = 16.3

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.05 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - N2 .. 5.68 su PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.16 Ratio
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 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Siemens, 1995); cell refinement: SAINT (Siemens, 1995); data reduction: SAINT and XPREP (Siemens, 1995); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and WinGX32 (Farrugia, 1999); software used to prepare material for publication: enCIFer (Version 1.0; Allen et al., 2004).

tetraaquadipyridylcobalt(II) acetate top
Crystal data top
[Co(C5H5N)2(H2O)4](C2H3O2)2F(000) = 426
Mr = 407.28Dx = 1.494 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 6128 reflections
a = 8.3770 (13) Åθ = 2.5–28.2°
b = 9.6030 (15) ŵ = 0.99 mm1
c = 11.6700 (18) ÅT = 150 K
β = 105.286 (2)°Prism, orange
V = 905.6 (2) Å30.40 × 0.30 × 0.20 mm
Z = 2
Data collection top
Bruker SMART 1000 CCD
diffractometer
2304 independent reflections
Radiation source: sealed tube2148 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.018
ω scansθmax = 28.3°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
h = 1111
Tmin = 0.668, Tmax = 0.820k = 1212
8936 measured reflectionsl = 1514
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)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.065H atoms treated by a mixture of independent and constrained refinement
S = 1.05 w = 1/[σ2(Fo2) + (0.0396P)2 + 0.2088P]
where P = (Fo2 + 2Fc2)/3
2304 reflections(Δ/σ)max = 0.001
141 parametersΔρmax = 0.41 e Å3
4 restraintsΔρmin = 0.20 e Å3
Special details top

Experimental. The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 150(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Cryostream and data were collected at this temperature. 145 standard reflections were obtained by recollecting the first 50 CCD frames at the end of data collection. They were then used for a decay correction, giving an overall decay of 0.39%.

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*/UeqOcc. (<1)
Co10.77092 (2)0.25000.744294 (15)0.01468 (8)
O30.46939 (10)0.86571 (8)0.61182 (7)0.02343 (18)
O40.08767 (11)0.86590 (8)0.90271 (7)0.02581 (19)
O10.88230 (10)0.40379 (9)0.86625 (7)0.02318 (18)
H1O0.9462 (17)0.4691 (14)0.8630 (13)0.028*
H2O0.8966 (18)0.3866 (16)0.9422 (11)0.028*
O20.66030 (10)0.09583 (8)0.62259 (7)0.02111 (17)
H3O0.6028 (16)0.0264 (14)0.6321 (12)0.025*
H4O0.6281 (17)0.1154 (16)0.5475 (11)0.025*
N20.57367 (16)0.25000.83100 (11)0.0188 (3)
N10.96660 (16)0.25000.65721 (11)0.0181 (3)
C10.2921 (2)0.25000.91493 (14)0.0295 (4)
H10.19470.25000.94210.035*
C20.36399 (16)0.12599 (14)0.89483 (11)0.0303 (3)
H20.31840.03930.90940.036*
C51.17234 (16)0.37414 (14)0.58921 (11)0.0307 (3)
H51.21730.46080.57390.037*
C90.51852 (19)0.75000.65807 (13)0.0192 (3)
C70.0961 (2)0.75000.85494 (14)0.0213 (3)
C41.03447 (15)0.36942 (12)0.63392 (10)0.0245 (2)
H40.98600.45480.64870.029*
C30.50406 (15)0.13083 (12)0.85293 (10)0.0244 (2)
H30.55310.04540.83910.029*
C100.6418 (3)0.75000.77855 (17)0.0425 (5)
H10A0.69910.66010.79180.064*0.50
H10B0.58360.76520.84020.064*0.50
H10C0.72260.82460.78190.064*0.50
C80.1210 (3)0.75000.73081 (16)0.0408 (5)
H8A0.20450.68030.72610.061*0.50
H8B0.15840.84230.71310.061*0.50
H8C0.01620.72740.67300.061*0.50
C61.2429 (2)0.25000.56747 (15)0.0312 (4)
H61.33840.25000.53800.037*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.01538 (12)0.01280 (11)0.01534 (11)0.0000.00310 (8)0.000
O30.0298 (4)0.0158 (4)0.0223 (4)0.0012 (3)0.0027 (3)0.0019 (3)
O40.0372 (5)0.0178 (4)0.0226 (4)0.0049 (3)0.0081 (3)0.0006 (3)
O10.0294 (4)0.0218 (4)0.0178 (4)0.0098 (3)0.0051 (3)0.0026 (3)
O20.0262 (4)0.0179 (4)0.0178 (4)0.0063 (3)0.0031 (3)0.0008 (3)
N20.0188 (6)0.0182 (6)0.0190 (6)0.0000.0041 (5)0.000
N10.0169 (6)0.0194 (6)0.0177 (6)0.0000.0041 (5)0.000
C10.0188 (7)0.0498 (11)0.0201 (7)0.0000.0055 (6)0.000
C20.0288 (6)0.0359 (7)0.0273 (6)0.0107 (5)0.0095 (5)0.0003 (5)
C50.0283 (6)0.0365 (7)0.0302 (6)0.0109 (5)0.0124 (5)0.0006 (5)
C90.0220 (7)0.0185 (7)0.0184 (7)0.0000.0074 (6)0.000
C70.0251 (8)0.0181 (7)0.0210 (7)0.0000.0063 (6)0.000
C40.0255 (6)0.0230 (6)0.0263 (5)0.0031 (4)0.0091 (4)0.0008 (4)
C30.0270 (6)0.0207 (6)0.0270 (5)0.0030 (4)0.0097 (4)0.0011 (4)
C100.0556 (13)0.0251 (9)0.0316 (9)0.0000.0150 (9)0.000
C80.0734 (15)0.0268 (9)0.0289 (9)0.0000.0256 (10)0.000
C60.0204 (8)0.0513 (11)0.0234 (8)0.0000.0088 (6)0.000
Geometric parameters (Å, º) top
Co1—O2i2.0914 (8)C2—C31.3859 (17)
Co1—O1i2.0921 (8)C2—H20.9500
Co1—N12.1444 (13)C5—C61.3833 (16)
Co1—N22.1531 (13)C5—C41.3878 (17)
Co1—O12.0921 (8)C5—H50.9500
Co1—O22.0914 (8)C9—O3ii1.2563 (10)
O3—C91.2563 (10)C9—C101.509 (2)
O4—C71.2551 (11)C7—O4ii1.2551 (11)
O1—H1O0.832 (13)C7—C81.517 (2)
O1—H2O0.878 (12)C4—H40.9500
O2—H3O0.846 (12)C3—H30.9500
O2—H4O0.867 (12)C10—H10A0.9800
N2—C3i1.3394 (13)C10—H10B0.9800
N2—C31.3394 (13)C10—H10C0.9800
N1—C41.3393 (13)C8—H8A0.9800
N1—C4i1.3393 (13)C8—H8B0.9800
C1—C2i1.3822 (17)C8—H8C0.9800
C1—C21.3822 (17)C6—C5i1.3833 (16)
C1—H10.9500C6—H60.9500
N1—Co1—N2179.75 (4)C3—C2—H2120.7
O1—Co1—O1i89.80 (5)C6—C5—C4118.61 (12)
O2—Co1—O1179.80 (3)C6—C5—H5120.7
O2i—Co1—O190.03 (4)C4—C5—H5120.7
O2—Co1—O1i90.03 (4)O3ii—C9—O3124.38 (14)
O2—Co1—O2i90.13 (5)O3ii—C9—C10117.80 (7)
O2i—Co1—O1i179.80 (3)O3—C9—C10117.80 (7)
O2—Co1—N186.30 (3)O4—C7—O4ii124.95 (14)
O2i—Co1—N186.30 (3)O4—C7—C8117.52 (7)
O1—Co1—N193.61 (3)O4ii—C7—C8117.52 (7)
O1i—Co1—N193.61 (3)N1—C4—C5122.96 (11)
O2—Co1—N293.53 (3)N1—C4—H4118.5
O2i—Co1—N293.53 (3)C5—C4—H4118.5
O1—Co1—N286.57 (3)N2—C3—C2123.22 (12)
O1i—Co1—N286.57 (3)N2—C3—H3118.4
Co1—O1—H1O132.7 (10)C2—C3—H3118.4
Co1—O1—H2O118.1 (10)C9—C10—H10A109.5
H1O—O1—H2O105.7 (14)C9—C10—H10B109.5
Co1—O2—H3O129.3 (10)H10A—C10—H10B109.5
Co1—O2—H4O119.8 (10)C9—C10—H10C109.5
H3O—O2—H4O105.5 (13)H10A—C10—H10C109.5
C3i—N2—C3117.40 (14)H10B—C10—H10C109.5
C3i—N2—Co1121.10 (7)C7—C8—H8A109.5
C3—N2—Co1121.10 (7)C7—C8—H8B109.5
C4—N1—C4i117.80 (14)H8A—C8—H8B109.5
C4—N1—Co1120.97 (7)C7—C8—H8C109.5
C4i—N1—Co1120.97 (7)H8A—C8—H8C109.5
C2i—C1—C2118.99 (16)H8B—C8—H8C109.5
C2i—C1—H1120.5C5—C6—C5i119.03 (15)
C2—C1—H1120.5C5—C6—H6120.5
C1—C2—C3118.58 (12)C5i—C6—H6120.5
C1—C2—H2120.7
O2—Co1—N2—C3i131.43 (10)O2—Co1—N1—C4i47.79 (10)
O2i—Co1—N2—C3i41.08 (11)O2i—Co1—N1—C4i138.16 (10)
O1—Co1—N2—C3i48.74 (10)O1—Co1—N1—C4i132.04 (10)
O1i—Co1—N2—C3i138.75 (11)O1i—Co1—N1—C4i42.01 (10)
O2—Co1—N2—C341.08 (11)C2i—C1—C2—C31.3 (2)
O2i—Co1—N2—C3131.43 (10)C4i—N1—C4—C51.2 (2)
O1—Co1—N2—C3138.75 (11)Co1—N1—C4—C5173.06 (9)
O1i—Co1—N2—C348.74 (10)C6—C5—C4—N10.1 (2)
O2—Co1—N1—C4138.16 (10)C3i—N2—C3—C21.0 (2)
O2i—Co1—N1—C447.79 (10)Co1—N2—C3—C2171.74 (9)
O1—Co1—N1—C442.01 (10)C1—C2—C3—N20.1 (2)
O1i—Co1—N1—C4132.04 (10)C4—C5—C6—C5i1.0 (2)
Symmetry codes: (i) x, y+1/2, z; (ii) x, y+3/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1O···O4iii0.83 (1)1.96 (1)2.7652 (12)163 (1)
O1—H2O···O4iv0.88 (1)1.79 (1)2.6660 (12)174 (2)
O2—H3O···O3v0.85 (1)1.88 (1)2.7111 (12)165 (1)
O2—H4O···O3vi0.87 (1)1.83 (1)2.6895 (12)170 (1)
Symmetry codes: (iii) x+1, y+3/2, z; (iv) x+1, y1/2, z+2; (v) x, y1, z; (vi) x+1, y+1, z+1.
 

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