μ-4,4′-Bipyridine-κ²N:N′-bis­[triaqua­(pyridine-2,4-dicarboxyl­ato-κ²N,O)cobalt(II)] dihydrate

The title centrosymmetric dinuclear complex, [Co₂(C₇H₃NO₄)₂(C₁₀H₈N₂)(H₂O)₆]·2H₂O, has been synthesized hydro­thermally. The cobalt(II) ion is coordinated in a slightly distorted octa­hedral environment by one N atom and one carboxylate O atom in N,O-chelating mode from one 2,4-pyridine­dicarboxyl­ate ligand, by one N atom from 4,4′-bipyridine, and by three water mol­ecules. O—H...O hydrogen bonds link mol­ecules into a three-dimensional framework.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.052
• wR factor = 0.145
• Data-to-parameter ratio = 12.8

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.14
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.46
PLAT369_ALERT_2_C Long   C(sp2)-C(sp2) Bond  C4     -   C7     ...       1.53 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          8
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          1
              C24 H26 Co2 N4 O14

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

   3 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
   0 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

µ-4,4'-Bipyridine-κ²N:N'-bis[triaqua(pyridine-2,4-dicarboxylato- κ²N,O)cobalt(II)] dihydrate

Crystal data

[Co2(C7H3NO4)2(C10H8N2)(H2O)6]·2H2O	Z = 1
Mr = 748.38	F(000) = 384
Triclinic, P1	Dx = 1.711 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.413 (1) Å	Cell parameters from 126 reflections
b = 9.763 (2) Å	θ = 2.6–25°
c = 12.113 (2) Å	µ = 1.23 mm^−1
α = 79.54 (3)°	T = 293 K
β = 79.26 (3)°	Needle, red
γ = 80.61 (3)°	0.33 × 0.12 × 0.09 mm
V = 726.1 (2) Å^3

Data collection

Bruker APEX area-dector diffractometer	3074 independent reflections
Radiation source: fine-focus sealed tube	2285 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.026
φ and ω scans	θmax = 27.2°, θmin = 2.1°
Absorption correction: multi-scan (Blessing, 1995)	h = −8→7
Tmin = 0.688, Tmax = 0.898	k = −12→12
4961 measured reflections	l = −15→11

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)] = 0.052	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.145	H atoms treated by a mixture of independent and constrained refinement
S = 1.12	w = 1/[σ^2(Fo^2) + (0.0691P)^2 + 0.6587P] where P = (Fo^2 + 2Fc^2)/3
3074 reflections	(Δ/σ)max < 0.001
241 parameters	Δρmax = 1.29 e Å^−3
0 restraints	Δρmin = −0.61 e Å^−3

Special details

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
Co1	0.14240 (8)	0.04839 (5)	0.28137 (5)	0.0280 (2)
O1	−0.1574 (4)	0.0998 (3)	0.3745 (2)	0.0334 (7)
O2	−0.4475 (5)	0.2595 (3)	0.3735 (3)	0.0427 (8)
O3	−0.0254 (5)	0.7844 (3)	0.0700 (3)	0.0439 (8)
O4	−0.3478 (5)	0.7432 (3)	0.1608 (3)	0.0526 (9)
N1	0.0875 (5)	0.2738 (3)	0.2358 (3)	0.0293 (7)
N2	0.1027 (5)	−0.1685 (3)	0.3414 (3)	0.0312 (8)
C1	−0.2559 (6)	0.2209 (4)	0.3428 (3)	0.0302 (9)
C2	−0.1188 (6)	0.3236 (4)	0.2664 (3)	0.0301 (9)
C3	−0.2020 (7)	0.4599 (4)	0.2317 (3)	0.0308 (9)
H3A	−0.3470	0.4901	0.2523	0.037*
C4	−0.0678 (7)	0.5525 (4)	0.1654 (3)	0.0316 (9)
C5	0.1451 (7)	0.5024 (4)	0.1373 (4)	0.0383 (10)
H5A	0.2400	0.5617	0.0942	0.046*
C6	0.2163 (7)	0.3632 (4)	0.1735 (4)	0.0395 (10)
H6A	0.3606	0.3303	0.1537	0.047*
C7	−0.1561 (7)	0.7058 (4)	0.1282 (4)	0.0346 (9)
C8	0.2592 (7)	−0.2665 (4)	0.3721 (4)	0.0462 (12)
H8A	0.3990	−0.2455	0.3528	0.055*
C9	0.2266 (7)	−0.3960 (5)	0.4303 (4)	0.0460 (12)
H9A	0.3436	−0.4615	0.4467	0.055*
C10	0.0224 (6)	−0.4317 (4)	0.4655 (3)	0.0279 (8)
C11	−0.1409 (7)	−0.3313 (4)	0.4317 (4)	0.0360 (10)
H11A	−0.2819	−0.3498	0.4504	0.043*
C12	−0.0948 (7)	−0.2034 (4)	0.3701 (4)	0.0338 (9)
H12A	−0.2076	−0.1382	0.3473	0.041*
O1W	0.4429 (5)	0.0130 (4)	0.1835 (3)	0.0468 (9)
O2W	−0.0009 (6)	0.0398 (4)	0.1394 (3)	0.0437 (8)
O3W	0.3060 (6)	0.0431 (4)	0.4142 (3)	0.0478 (9)
O4W	0.4062 (7)	0.7919 (4)	0.9872 (4)	0.0632 (11)
H1WB	0.499 (8)	−0.054 (6)	0.167 (4)	0.045 (16)*
H3WA	0.255 (10)	0.013 (7)	0.478 (5)	0.07 (2)*
H3WB	0.383 (8)	0.106 (5)	0.416 (4)	0.044 (14)*
H2WA	0.045 (10)	0.087 (7)	0.084 (5)	0.07 (2)*
H4WA	0.274 (14)	0.792 (8)	1.011 (6)	0.10 (3)*
H2WB	−0.021 (10)	−0.037 (7)	0.116 (5)	0.08 (2)*
H1WA	0.499 (10)	0.076 (7)	0.128 (6)	0.08 (2)*
H4WB	0.474 (16)	0.786 (11)	1.050 (9)	0.16 (4)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0279 (3)	0.0192 (3)	0.0339 (3)	−0.0047 (2)	−0.0030 (2)	0.0026 (2)
O1	0.0330 (15)	0.0196 (13)	0.0392 (16)	−0.0031 (11)	0.0043 (12)	0.0062 (12)
O2	0.0291 (16)	0.0288 (15)	0.062 (2)	−0.0034 (12)	0.0036 (14)	0.0027 (14)
O3	0.0445 (18)	0.0294 (16)	0.0512 (19)	−0.0078 (14)	−0.0042 (15)	0.0102 (14)
O4	0.0393 (19)	0.0318 (17)	0.070 (2)	0.0063 (14)	0.0022 (16)	0.0150 (16)
N1	0.0301 (17)	0.0159 (15)	0.0379 (19)	−0.0027 (13)	0.0009 (14)	−0.0008 (13)
N2	0.0338 (18)	0.0210 (16)	0.0370 (19)	−0.0073 (14)	−0.0037 (15)	0.0011 (14)
C1	0.028 (2)	0.0236 (19)	0.037 (2)	−0.0048 (16)	−0.0027 (17)	−0.0003 (16)
C2	0.029 (2)	0.026 (2)	0.034 (2)	−0.0054 (16)	−0.0011 (16)	−0.0046 (16)
C3	0.032 (2)	0.0221 (19)	0.035 (2)	−0.0028 (16)	−0.0037 (17)	0.0022 (16)
C4	0.036 (2)	0.0238 (19)	0.032 (2)	−0.0025 (17)	−0.0049 (17)	0.0015 (16)
C5	0.033 (2)	0.023 (2)	0.052 (3)	−0.0095 (17)	0.0048 (19)	0.0039 (18)
C6	0.033 (2)	0.025 (2)	0.053 (3)	−0.0043 (17)	0.005 (2)	0.0027 (19)
C7	0.034 (2)	0.022 (2)	0.044 (2)	−0.0022 (16)	−0.0054 (18)	0.0023 (18)
C8	0.027 (2)	0.026 (2)	0.074 (3)	−0.0047 (17)	−0.007 (2)	0.023 (2)
C9	0.026 (2)	0.036 (2)	0.066 (3)	−0.0016 (18)	−0.009 (2)	0.017 (2)
C10	0.032 (2)	0.0217 (19)	0.030 (2)	−0.0047 (15)	−0.0063 (16)	−0.0002 (16)
C11	0.029 (2)	0.023 (2)	0.054 (3)	−0.0043 (16)	−0.0101 (19)	0.0042 (18)
C12	0.033 (2)	0.0182 (18)	0.049 (3)	−0.0029 (16)	−0.0117 (18)	0.0048 (17)
O1W	0.0428 (19)	0.0252 (17)	0.058 (2)	0.0017 (15)	0.0141 (16)	0.0028 (16)
O2W	0.062 (2)	0.0350 (18)	0.0375 (19)	−0.0163 (16)	−0.0160 (16)	0.0034 (15)
O3W	0.053 (2)	0.056 (2)	0.040 (2)	−0.0315 (18)	−0.0156 (16)	0.0106 (16)
O4W	0.041 (2)	0.068 (3)	0.068 (3)	−0.0054 (19)	0.005 (2)	0.007 (2)

Geometric parameters (Å, º)

Co1—O3W	2.067 (3)	C5—C6	1.380 (6)
Co1—O1	2.075 (3)	C5—H5A	0.9300
Co1—O1W	2.078 (3)	C6—H6A	0.9300
Co1—O2W	2.116 (3)	C8—C9	1.359 (6)
Co1—N2	2.151 (3)	C8—H8A	0.9300
Co1—N1	2.157 (3)	C9—C10	1.380 (6)
O1—C1	1.275 (5)	C9—H9A	0.9300
O2—C1	1.233 (5)	C10—C11	1.380 (6)
O3—C7	1.257 (5)	C10—C10^i	1.480 (7)
O4—C7	1.235 (5)	C11—C12	1.379 (5)
N1—C6	1.333 (5)	C11—H11A	0.9300
N1—C2	1.341 (5)	C12—H12A	0.9300
N2—C8	1.326 (5)	O1W—H1WB	0.74 (5)
N2—C12	1.332 (5)	O1W—H1WA	0.89 (7)
C1—C2	1.511 (5)	O2W—H2WA	0.78 (6)
C2—C3	1.371 (5)	O2W—H2WB	0.88 (7)
C3—C4	1.391 (5)	O3W—H3WA	0.81 (6)
C3—H3A	0.9300	O3W—H3WB	0.86 (5)
C4—C5	1.374 (6)	O4W—H4WA	0.84 (8)
C4—C7	1.529 (5)	O4W—H4WB	0.93 (11)
O3W—Co1—O1	94.61 (14)	C4—C5—C6	119.3 (4)
O3W—Co1—O1W	85.80 (16)	C4—C5—H5A	120.4
O1—Co1—O1W	175.66 (12)	C6—C5—H5A	120.4
O3W—Co1—O2W	174.55 (15)	N1—C6—C5	122.9 (4)
O1—Co1—O2W	90.22 (13)	N1—C6—H6A	118.6
O1W—Co1—O2W	89.57 (15)	C5—C6—H6A	118.6
O3W—Co1—N2	88.82 (14)	O4—C7—O3	125.5 (4)
O1—Co1—N2	87.33 (12)	O4—C7—C4	117.4 (4)
O1W—Co1—N2	97.01 (14)	O3—C7—C4	117.1 (4)
O2W—Co1—N2	88.88 (14)	N2—C8—C9	123.6 (4)
O3W—Co1—N1	97.16 (14)	N2—C8—H8A	118.2
O1—Co1—N1	77.55 (11)	C9—C8—H8A	118.2
O1W—Co1—N1	98.11 (14)	C8—C9—C10	121.0 (4)
O2W—Co1—N1	86.34 (14)	C8—C9—H9A	119.5
N2—Co1—N1	164.10 (12)	C10—C9—H9A	119.5
C1—O1—Co1	116.1 (2)	C11—C10—C9	115.6 (4)
C6—N1—C2	117.9 (3)	C11—C10—C10^i	121.3 (4)
C6—N1—Co1	130.5 (3)	C9—C10—C10^i	123.1 (5)
C2—N1—Co1	111.1 (2)	C12—C11—C10	120.0 (4)
C8—N2—C12	116.2 (3)	C12—C11—H11A	120.0
C8—N2—Co1	123.7 (3)	C10—C11—H11A	120.0
C12—N2—Co1	118.8 (3)	N2—C12—C11	123.4 (4)
O2—C1—O1	125.0 (4)	N2—C12—H12A	118.3
O2—C1—C2	119.5 (3)	C11—C12—H12A	118.3
O1—C1—C2	115.5 (3)	Co1—O1W—H1WB	127 (4)
N1—C2—C3	122.5 (4)	Co1—O1W—H1WA	124 (4)
N1—C2—C1	116.1 (3)	H1WB—O1W—H1WA	102 (6)
C3—C2—C1	121.4 (4)	Co1—O2W—H2WA	114 (5)
C2—C3—C4	119.5 (4)	Co1—O2W—H2WB	126 (4)
C2—C3—H3A	120.3	H2WA—O2W—H2WB	104 (6)
C4—C3—H3A	120.3	Co1—O3W—H3WA	120 (4)
C5—C4—C3	117.9 (4)	Co1—O3W—H3WB	123 (3)
C5—C4—C7	121.7 (4)	H3WA—O3W—H3WB	109 (5)
C3—C4—C7	120.4 (4)	H4WA—O4W—H4WB	108 (7)
O3W—Co1—O1—C1	113.9 (3)	Co1—N1—C2—C1	10.9 (4)
O2W—Co1—O1—C1	−68.6 (3)	O2—C1—C2—N1	−179.5 (4)
N2—Co1—O1—C1	−157.5 (3)	O1—C1—C2—N1	3.4 (5)
N1—Co1—O1—C1	17.6 (3)	O2—C1—C2—C3	1.1 (6)
O3W—Co1—N1—C6	80.7 (4)	O1—C1—C2—C3	−176.1 (4)
O1—Co1—N1—C6	173.8 (4)	N1—C2—C3—C4	−2.2 (6)
O1W—Co1—N1—C6	−6.1 (4)	C1—C2—C3—C4	177.2 (4)
O2W—Co1—N1—C6	−95.1 (4)	C2—C3—C4—C5	0.1 (6)
N2—Co1—N1—C6	−167.9 (4)	C2—C3—C4—C7	−178.6 (4)
O3W—Co1—N1—C2	−107.8 (3)	C3—C4—C5—C6	1.1 (7)
O1—Co1—N1—C2	−14.6 (3)	C7—C4—C5—C6	179.7 (4)
O1W—Co1—N1—C2	165.4 (3)	C2—N1—C6—C5	−1.7 (7)
O2W—Co1—N1—C2	76.4 (3)	Co1—N1—C6—C5	169.3 (3)
N2—Co1—N1—C2	3.6 (6)	C4—C5—C6—N1	−0.3 (7)
O3W—Co1—N2—C8	−45.8 (4)	C5—C4—C7—O4	−177.4 (4)
O1—Co1—N2—C8	−140.5 (4)	C3—C4—C7—O4	1.2 (6)
O1W—Co1—N2—C8	39.8 (4)	C5—C4—C7—O3	0.3 (6)
O2W—Co1—N2—C8	129.2 (4)	C3—C4—C7—O3	178.9 (4)
N1—Co1—N2—C8	−158.3 (5)	C12—N2—C8—C9	−0.5 (8)
O3W—Co1—N2—C12	121.0 (3)	Co1—N2—C8—C9	166.7 (4)
O1—Co1—N2—C12	26.4 (3)	N2—C8—C9—C10	−2.6 (9)
O1W—Co1—N2—C12	−153.3 (3)	C8—C9—C10—C11	3.7 (7)
O2W—Co1—N2—C12	−63.9 (3)	C8—C9—C10—C10^i	−176.5 (5)
N1—Co1—N2—C12	8.5 (7)	C9—C10—C11—C12	−2.0 (7)
Co1—O1—C1—O2	166.1 (3)	C10^i—C10—C11—C12	178.2 (5)
Co1—O1—C1—C2	−17.0 (5)	C8—N2—C12—C11	2.3 (7)
C6—N1—C2—C3	3.0 (6)	Co1—N2—C12—C11	−165.5 (4)
Co1—N1—C2—C3	−169.7 (3)	C10—C11—C12—N2	−1.0 (7)
C6—N1—C2—C1	−176.4 (4)

Symmetry code: (i) −x, −y−1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WB···O4^ii	0.74 (5)	2.07 (6)	2.791 (5)	167 (5)
O3W—H3WA···O1^iii	0.81 (6)	1.97 (6)	2.763 (5)	168 (6)
O3W—H3WB···O2^iv	0.86 (5)	1.93 (6)	2.761 (5)	163 (5)
O2W—H2WA···O3^v	0.78 (6)	2.06 (6)	2.786 (5)	155 (6)
O4W—H4WA···O3^vi	0.84 (8)	1.93 (8)	2.771 (5)	177 (8)
O2W—H2WB···O3^vii	0.88 (7)	1.94 (7)	2.808 (5)	172 (6)
O1W—H1WA···O4W^viii	0.89 (7)	1.81 (7)	2.695 (5)	176 (6)
O4W—H4WB···O4^ix	0.93 (11)	1.87 (11)	2.786 (6)	168 (9)

Symmetry codes: (ii) x+1, y−1, z; (iii) −x, −y, −z+1; (iv) x+1, y, z; (v) −x, −y+1, −z; (vi) x, y, z+1; (vii) x, y−1, z; (viii) −x+1, −y+1, −z+1; (ix) x+1, y, z+1.