Tetra­aqua­bis(pyridine-κN)cobalt(II) diacetate

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.

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

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

Crystal data

[Co(C5H5N)2(H2O)4](C2H3O2)2	F(000) = 426
Mr = 407.28	Dx = 1.494 Mg m^−3
Monoclinic, P21/m	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yb	Cell parameters from 6128 reflections
a = 8.3770 (13) Å	θ = 2.5–28.2°
b = 9.6030 (15) Å	µ = 0.99 mm^−1
c = 11.6700 (18) Å	T = 150 K
β = 105.286 (2)°	Prism, orange
V = 905.6 (2) Å^3	0.40 × 0.30 × 0.20 mm
Z = 2

Data collection

Bruker SMART 1000 CCD diffractometer	2304 independent reflections
Radiation source: sealed tube	2148 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.018
ω scans	θmax = 28.3°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −11→11
Tmin = 0.668, Tmax = 0.820	k = −12→12
8936 measured reflections	l = −15→14

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.023	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.065	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0396P)^2 + 0.2088P] where P = (Fo^2 + 2Fc^2)/3
2304 reflections	(Δ/σ)max = 0.001
141 parameters	Δρmax = 0.41 e Å^−3
4 restraints	Δρmin = −0.20 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Co1	0.77092 (2)	0.2500	0.744294 (15)	0.01468 (8)
O3	0.46939 (10)	0.86571 (8)	0.61182 (7)	0.02343 (18)
O4	0.08767 (11)	0.86590 (8)	0.90271 (7)	0.02581 (19)
O1	0.88230 (10)	0.40379 (9)	0.86625 (7)	0.02318 (18)
H1O	0.9462 (17)	0.4691 (14)	0.8630 (13)	0.028*
H2O	0.8966 (18)	0.3866 (16)	0.9422 (11)	0.028*
O2	0.66030 (10)	0.09583 (8)	0.62259 (7)	0.02111 (17)
H3O	0.6028 (16)	0.0264 (14)	0.6321 (12)	0.025*
H4O	0.6281 (17)	0.1154 (16)	0.5475 (11)	0.025*
N2	0.57367 (16)	0.2500	0.83100 (11)	0.0188 (3)
N1	0.96660 (16)	0.2500	0.65721 (11)	0.0181 (3)
C1	0.2921 (2)	0.2500	0.91493 (14)	0.0295 (4)
H1	0.1947	0.2500	0.9421	0.035*
C2	0.36399 (16)	0.12599 (14)	0.89483 (11)	0.0303 (3)
H2	0.3184	0.0393	0.9094	0.036*
C5	1.17234 (16)	0.37414 (14)	0.58921 (11)	0.0307 (3)
H5	1.2173	0.4608	0.5739	0.037*
C9	0.51852 (19)	0.7500	0.65807 (13)	0.0192 (3)
C7	0.0961 (2)	0.7500	0.85494 (14)	0.0213 (3)
C4	1.03447 (15)	0.36942 (12)	0.63392 (10)	0.0245 (2)
H4	0.9860	0.4548	0.6487	0.029*
C3	0.50406 (15)	0.13083 (12)	0.85293 (10)	0.0244 (2)
H3	0.5531	0.0454	0.8391	0.029*
C10	0.6418 (3)	0.7500	0.77855 (17)	0.0425 (5)
H10A	0.6991	0.6601	0.7918	0.064*	0.50
H10B	0.5836	0.7652	0.8402	0.064*	0.50
H10C	0.7226	0.8246	0.7819	0.064*	0.50
C8	0.1210 (3)	0.7500	0.73081 (16)	0.0408 (5)
H8A	0.2045	0.6803	0.7261	0.061*	0.50
H8B	0.1584	0.8423	0.7131	0.061*	0.50
H8C	0.0162	0.7274	0.6730	0.061*	0.50
C6	1.2429 (2)	0.2500	0.56747 (15)	0.0312 (4)
H6	1.3384	0.2500	0.5380	0.037*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.01538 (12)	0.01280 (11)	0.01534 (11)	0.000	0.00310 (8)	0.000
O3	0.0298 (4)	0.0158 (4)	0.0223 (4)	−0.0012 (3)	0.0027 (3)	0.0019 (3)
O4	0.0372 (5)	0.0178 (4)	0.0226 (4)	0.0049 (3)	0.0081 (3)	−0.0006 (3)
O1	0.0294 (4)	0.0218 (4)	0.0178 (4)	−0.0098 (3)	0.0051 (3)	−0.0026 (3)
O2	0.0262 (4)	0.0179 (4)	0.0178 (4)	−0.0063 (3)	0.0031 (3)	−0.0008 (3)
N2	0.0188 (6)	0.0182 (6)	0.0190 (6)	0.000	0.0041 (5)	0.000
N1	0.0169 (6)	0.0194 (6)	0.0177 (6)	0.000	0.0041 (5)	0.000
C1	0.0188 (7)	0.0498 (11)	0.0201 (7)	0.000	0.0055 (6)	0.000
C2	0.0288 (6)	0.0359 (7)	0.0273 (6)	−0.0107 (5)	0.0095 (5)	−0.0003 (5)
C5	0.0283 (6)	0.0365 (7)	0.0302 (6)	−0.0109 (5)	0.0124 (5)	0.0006 (5)
C9	0.0220 (7)	0.0185 (7)	0.0184 (7)	0.000	0.0074 (6)	0.000
C7	0.0251 (8)	0.0181 (7)	0.0210 (7)	0.000	0.0063 (6)	0.000
C4	0.0255 (6)	0.0230 (6)	0.0263 (5)	−0.0031 (4)	0.0091 (4)	−0.0008 (4)
C3	0.0270 (6)	0.0207 (6)	0.0270 (5)	−0.0030 (4)	0.0097 (4)	−0.0011 (4)
C10	0.0556 (13)	0.0251 (9)	0.0316 (9)	0.000	−0.0150 (9)	0.000
C8	0.0734 (15)	0.0268 (9)	0.0289 (9)	0.000	0.0256 (10)	0.000
C6	0.0204 (8)	0.0513 (11)	0.0234 (8)	0.000	0.0088 (6)	0.000

Geometric parameters (Å, º)

Co1—O2^i	2.0914 (8)	C2—C3	1.3859 (17)
Co1—O1^i	2.0921 (8)	C2—H2	0.9500
Co1—N1	2.1444 (13)	C5—C6	1.3833 (16)
Co1—N2	2.1531 (13)	C5—C4	1.3878 (17)
Co1—O1	2.0921 (8)	C5—H5	0.9500
Co1—O2	2.0914 (8)	C9—O3^ii	1.2563 (10)
O3—C9	1.2563 (10)	C9—C10	1.509 (2)
O4—C7	1.2551 (11)	C7—O4^ii	1.2551 (11)
O1—H1O	0.832 (13)	C7—C8	1.517 (2)
O1—H2O	0.878 (12)	C4—H4	0.9500
O2—H3O	0.846 (12)	C3—H3	0.9500
O2—H4O	0.867 (12)	C10—H10A	0.9800
N2—C3^i	1.3394 (13)	C10—H10B	0.9800
N2—C3	1.3394 (13)	C10—H10C	0.9800
N1—C4	1.3393 (13)	C8—H8A	0.9800
N1—C4^i	1.3393 (13)	C8—H8B	0.9800
C1—C2^i	1.3822 (17)	C8—H8C	0.9800
C1—C2	1.3822 (17)	C6—C5^i	1.3833 (16)
C1—H1	0.9500	C6—H6	0.9500
N1—Co1—N2	179.75 (4)	C3—C2—H2	120.7
O1—Co1—O1^i	89.80 (5)	C6—C5—C4	118.61 (12)
O2—Co1—O1	179.80 (3)	C6—C5—H5	120.7
O2^i—Co1—O1	90.03 (4)	C4—C5—H5	120.7
O2—Co1—O1^i	90.03 (4)	O3^ii—C9—O3	124.38 (14)
O2—Co1—O2^i	90.13 (5)	O3^ii—C9—C10	117.80 (7)
O2^i—Co1—O1^i	179.80 (3)	O3—C9—C10	117.80 (7)
O2—Co1—N1	86.30 (3)	O4—C7—O4^ii	124.95 (14)
O2^i—Co1—N1	86.30 (3)	O4—C7—C8	117.52 (7)
O1—Co1—N1	93.61 (3)	O4^ii—C7—C8	117.52 (7)
O1^i—Co1—N1	93.61 (3)	N1—C4—C5	122.96 (11)
O2—Co1—N2	93.53 (3)	N1—C4—H4	118.5
O2^i—Co1—N2	93.53 (3)	C5—C4—H4	118.5
O1—Co1—N2	86.57 (3)	N2—C3—C2	123.22 (12)
O1^i—Co1—N2	86.57 (3)	N2—C3—H3	118.4
Co1—O1—H1O	132.7 (10)	C2—C3—H3	118.4
Co1—O1—H2O	118.1 (10)	C9—C10—H10A	109.5
H1O—O1—H2O	105.7 (14)	C9—C10—H10B	109.5
Co1—O2—H3O	129.3 (10)	H10A—C10—H10B	109.5
Co1—O2—H4O	119.8 (10)	C9—C10—H10C	109.5
H3O—O2—H4O	105.5 (13)	H10A—C10—H10C	109.5
C3^i—N2—C3	117.40 (14)	H10B—C10—H10C	109.5
C3^i—N2—Co1	121.10 (7)	C7—C8—H8A	109.5
C3—N2—Co1	121.10 (7)	C7—C8—H8B	109.5
C4—N1—C4^i	117.80 (14)	H8A—C8—H8B	109.5
C4—N1—Co1	120.97 (7)	C7—C8—H8C	109.5
C4^i—N1—Co1	120.97 (7)	H8A—C8—H8C	109.5
C2^i—C1—C2	118.99 (16)	H8B—C8—H8C	109.5
C2^i—C1—H1	120.5	C5—C6—C5^i	119.03 (15)
C2—C1—H1	120.5	C5—C6—H6	120.5
C1—C2—C3	118.58 (12)	C5^i—C6—H6	120.5
C1—C2—H2	120.7
O2—Co1—N2—C3^i	−131.43 (10)	O2—Co1—N1—C4^i	−47.79 (10)
O2^i—Co1—N2—C3^i	−41.08 (11)	O2^i—Co1—N1—C4^i	−138.16 (10)
O1—Co1—N2—C3^i	48.74 (10)	O1—Co1—N1—C4^i	132.04 (10)
O1^i—Co1—N2—C3^i	138.75 (11)	O1^i—Co1—N1—C4^i	42.01 (10)
O2—Co1—N2—C3	41.08 (11)	C2^i—C1—C2—C3	−1.3 (2)
O2^i—Co1—N2—C3	131.43 (10)	C4^i—N1—C4—C5	−1.2 (2)
O1—Co1—N2—C3	−138.75 (11)	Co1—N1—C4—C5	173.06 (9)
O1^i—Co1—N2—C3	−48.74 (10)	C6—C5—C4—N1	0.1 (2)
O2—Co1—N1—C4	138.16 (10)	C3^i—N2—C3—C2	1.0 (2)
O2^i—Co1—N1—C4	47.79 (10)	Co1—N2—C3—C2	−171.74 (9)
O1—Co1—N1—C4	−42.01 (10)	C1—C2—C3—N2	0.1 (2)
O1^i—Co1—N1—C4	−132.04 (10)	C4—C5—C6—C5^i	1.0 (2)

Symmetry codes: (i) x, −y+1/2, z; (ii) x, −y+3/2, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1O···O4^iii	0.83 (1)	1.96 (1)	2.7652 (12)	163 (1)
O1—H2O···O4^iv	0.88 (1)	1.79 (1)	2.6660 (12)	174 (2)
O2—H3O···O3^v	0.85 (1)	1.88 (1)	2.7111 (12)	165 (1)
O2—H4O···O3^vi	0.87 (1)	1.83 (1)	2.6895 (12)	170 (1)

Symmetry codes: (iii) x+1, −y+3/2, z; (iv) −x+1, y−1/2, −z+2; (v) x, y−1, z; (vi) −x+1, −y+1, −z+1.