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The title compound, [Co(H2O)6][Co(C7H3NO4)2]·2H2O, was obtained by a hydro­thermal reaction of cobalt chloride hexahydrate, 2,6-pyridine­di­carboxyl­ic acid, and Et3N (molar ratio 1:1:7). The compound contains six-coordinated CoII ions, with six O atoms of water mol­ecules attached to the Co atoms in the two independent centrosymmetric cations and four O and two N atoms of two trans 2,6-pyridine­di­carboxyl­ate groups bonded to the Co atom in the anion. Intermolecular hydrogen-bonding interactions are present, linking the cobalt complex cations, anions and uncoordinated water mol­ecules in the crystal structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803027491/ob6327sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803027491/ob6327Isup2.hkl
Contains datablock I

CCDC reference: 231810

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.012 Å
  • R factor = 0.094
  • wR factor = 0.228
  • Data-to-parameter ratio = 17.1

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O11 - H11A ... ? PLAT420_ALERT_2_B D-H Without Acceptor O12 - H12A ... ? PLAT420_ALERT_2_B D-H Without Acceptor O12 - H12B ... ? PLAT420_ALERT_2_B D-H Without Acceptor O15 - H15A ... ?
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Co2 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Co3 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 12 PLAT355_ALERT_3_C Long O-H Bond (0.82A) O10 - H10B = 1.01 Ang. PLAT355_ALERT_3_C Long O-H Bond (0.82A) O13 - H13A = 1.05 Ang. PLAT355_ALERT_3_C Long O-H Bond (0.82A) O14 - H14A = 1.01 Ang. PLAT355_ALERT_3_C Long O-H Bond (0.82A) O15 - H15A = 1.03 Ang. PLAT355_ALERT_3_C Long O-H Bond (0.82A) O15 - H15B = 1.04 Ang. PLAT737_ALERT_1_C D...A Calc 2.849(9), Rep 2.85(2) ...... 2.22 su-Rat O13 -O2 1.555 2.675 PLAT737_ALERT_1_C D...A Calc 2.790(8), Rep 2.79(3) ...... 3.75 su-Rat O9 -O2 1.555 2.576 PLAT737_ALERT_1_C D...A Calc 2.690(9), Rep 2.69(3) ...... 3.33 su-Rat O10 -O4 1.555 2.466 PLAT737_ALERT_1_C D...A Calc 2.759(8), Rep 2.76(2) ...... 2.50 su-Rat O10 -O6 1.555 2.566 PLAT737_ALERT_1_C D...A Calc 3.157(14), Rep 3.16(4) ...... 2.86 su-Rat O13 -O15 1.555 1.554 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 Co H12 O6 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 5 H2 O
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 16 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 6 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

Hexaaquacobalt(II) trans-bis(η3-pyridine-2,6- dicarboxylato-κ3O,N,O')cobaltate(II) dihydrate top
Crystal data top
[Co(H2O)6][Co(C7H3NO4)2]·2H2OZ = 2
Mr = 592.20F(000) = 604
Triclinic, P1Dx = 1.746 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.258 (6) ÅCell parameters from 2061 reflections
b = 11.615 (8) Åθ = 2.5–25°
c = 12.873 (9) ŵ = 1.55 mm1
α = 108.694 (11)°T = 295 K
β = 99.900 (12)°Columnar, red
γ = 98.089 (13)°0.30 × 0.10 × 0.10 mm
V = 1126.6 (13) Å3
Data collection top
Bruker SMART CCD area-detector
diffractometer
5293 independent reflections
Radiation source: fine-focus sealed tube2686 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.083
φ and ω scansθmax = 28.4°, θmin = 1.7°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1995)
h = 1110
Tmin = 0.678, Tmax = 0.856k = 1415
11729 measured reflectionsl = 1717
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)] = 0.094Hydrogen site location: difference Fourier map
wR(F2) = 0.228H-atom parameters not refined
S = 1.06 w = 1/[σ2(Fo2) + (0.1003P)2]
where P = (Fo2 + 2Fc2)/3
5293 reflections(Δ/σ)max = 0.001
310 parametersΔρmax = 1.02 e Å3
0 restraintsΔρmin = 0.84 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
Co10.13678 (14)0.78395 (10)0.24512 (8)0.0333 (3)
Co20.50000.50000.50000.0289 (4)
Co30.50001.00000.00000.0474 (5)
O10.3179 (7)0.9405 (5)0.2462 (4)0.0358 (13)
O20.4653 (7)1.1293 (5)0.3514 (4)0.0440 (15)
O30.0326 (7)0.7051 (5)0.3210 (5)0.0462 (15)
O40.0792 (7)0.7114 (6)0.4888 (5)0.0510 (16)
O50.3134 (7)0.6686 (5)0.2785 (4)0.0427 (14)
O60.4431 (8)0.5230 (6)0.1907 (5)0.0534 (17)
O70.0548 (7)0.8293 (5)0.1319 (5)0.0448 (15)
O80.1324 (8)0.8077 (6)0.0488 (5)0.0580 (18)
O90.6308 (8)0.6407 (5)0.4862 (4)0.0477 (16)
O100.6450 (7)0.4713 (5)0.6125 (4)0.0457 (15)
O110.6881 (9)0.3723 (6)0.3572 (6)0.066 (2)
O120.5336 (10)0.8420 (8)0.0474 (7)0.096 (3)
O130.3786 (9)0.8811 (7)0.1686 (5)0.070 (2)
O140.2697 (7)0.9892 (5)0.0470 (5)0.0486 (15)
O150.1131 (16)0.6459 (10)0.6583 (9)0.142 (4)
O160.0081 (13)1.0959 (7)0.2047 (6)0.102 (3)
N10.1909 (7)0.9068 (5)0.4044 (5)0.0247 (13)
N20.1499 (8)0.6746 (5)0.0913 (5)0.0288 (14)
C10.3685 (10)1.0317 (7)0.3363 (7)0.0342 (19)
C20.2998 (9)1.0161 (7)0.4345 (6)0.0287 (17)
C30.3378 (10)1.0988 (7)0.5433 (7)0.0361 (19)
C40.2610 (11)1.0641 (8)0.6218 (6)0.041 (2)
C50.1517 (10)0.9538 (8)0.5901 (6)0.0350 (19)
C60.1185 (9)0.8751 (7)0.4794 (6)0.0270 (17)
C70.0064 (11)0.7537 (8)0.4284 (7)0.040 (2)
C80.3454 (11)0.5938 (8)0.1906 (7)0.037 (2)
C90.2511 (9)0.5965 (7)0.0796 (6)0.0276 (17)
C100.2711 (10)0.5271 (7)0.0244 (7)0.038 (2)
C110.1815 (11)0.5448 (9)0.1172 (7)0.049 (2)
C120.0745 (12)0.6266 (9)0.1059 (7)0.049 (2)
C130.0598 (9)0.6908 (7)0.0014 (6)0.0306 (18)
C140.0519 (10)0.7832 (8)0.0277 (7)0.039 (2)
H3A0.41971.18490.57030.050*
H4A0.23631.11810.69400.050*
H5A0.09840.92760.63890.050*
H9A0.65310.64610.41590.050*
H9B0.57810.72140.53560.050*
H10A0.57740.46160.67460.050*
H10B0.73380.39210.57710.050*
H10C0.35240.46240.02110.050*
H11A0.75660.28950.33780.050*
H11B0.69110.40700.29660.050*
H11C0.19060.50920.19920.050*
H12A0.49820.76650.00120.050*
H12B0.58120.84970.11470.050*
H12C0.00190.63510.15930.050*
H13A0.42180.87510.24160.050*
H13B0.32230.81390.20680.050*
H14A0.25781.07740.05970.050*
H14B0.27001.00110.12550.050*
H15A0.04580.55530.61950.050*
H15B0.07590.68770.59990.050*
H16A0.02161.10630.13630.050*
H16B0.02041.18030.24510.050*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0432 (7)0.0326 (6)0.0244 (6)0.0088 (5)0.0099 (5)0.0089 (5)
Co20.0288 (9)0.0294 (8)0.0302 (8)0.0040 (7)0.0049 (7)0.0148 (7)
Co30.0370 (11)0.0668 (12)0.0514 (11)0.0111 (9)0.0159 (8)0.0351 (10)
O10.047 (4)0.034 (3)0.026 (3)0.006 (3)0.012 (3)0.008 (2)
O20.056 (4)0.032 (3)0.044 (3)0.001 (3)0.017 (3)0.016 (3)
O30.047 (4)0.038 (3)0.042 (3)0.012 (3)0.012 (3)0.006 (3)
O40.043 (4)0.062 (4)0.051 (4)0.007 (3)0.016 (3)0.028 (3)
O50.053 (4)0.054 (4)0.026 (3)0.023 (3)0.002 (3)0.019 (3)
O60.063 (4)0.073 (4)0.041 (4)0.047 (4)0.017 (3)0.026 (3)
O70.040 (4)0.055 (4)0.042 (3)0.019 (3)0.014 (3)0.015 (3)
O80.049 (4)0.086 (5)0.056 (4)0.033 (4)0.011 (3)0.041 (4)
O90.062 (4)0.046 (3)0.032 (3)0.015 (3)0.004 (3)0.016 (3)
O100.040 (4)0.057 (4)0.043 (3)0.002 (3)0.004 (3)0.028 (3)
O110.066 (5)0.057 (4)0.062 (4)0.009 (4)0.005 (4)0.021 (4)
O120.082 (6)0.106 (6)0.116 (7)0.009 (5)0.014 (5)0.069 (6)
O130.061 (5)0.093 (5)0.045 (4)0.005 (4)0.006 (3)0.020 (4)
O140.045 (4)0.062 (4)0.044 (3)0.009 (3)0.018 (3)0.024 (3)
O150.218 (12)0.179 (10)0.132 (8)0.133 (9)0.108 (9)0.118 (8)
O160.163 (9)0.096 (6)0.066 (5)0.032 (6)0.059 (6)0.035 (5)
N10.015 (3)0.034 (3)0.030 (3)0.006 (3)0.008 (3)0.015 (3)
N20.035 (4)0.030 (3)0.023 (3)0.007 (3)0.009 (3)0.009 (3)
C10.031 (5)0.032 (5)0.046 (5)0.009 (4)0.010 (4)0.020 (4)
C20.029 (4)0.039 (5)0.026 (4)0.022 (4)0.008 (3)0.014 (4)
C30.032 (5)0.035 (5)0.037 (5)0.009 (4)0.008 (4)0.006 (4)
C40.042 (5)0.049 (5)0.029 (4)0.016 (4)0.005 (4)0.007 (4)
C50.031 (5)0.052 (5)0.028 (4)0.013 (4)0.012 (4)0.018 (4)
C60.022 (4)0.036 (4)0.026 (4)0.011 (3)0.007 (3)0.011 (3)
C70.035 (5)0.054 (5)0.041 (5)0.013 (4)0.009 (4)0.027 (4)
C80.040 (5)0.038 (5)0.034 (5)0.002 (4)0.010 (4)0.016 (4)
C90.027 (4)0.029 (4)0.027 (4)0.008 (3)0.006 (3)0.009 (3)
C100.039 (5)0.044 (5)0.032 (4)0.009 (4)0.011 (4)0.012 (4)
C110.042 (6)0.064 (6)0.029 (5)0.003 (5)0.008 (4)0.007 (4)
C120.044 (6)0.067 (6)0.032 (5)0.014 (5)0.004 (4)0.017 (5)
C130.027 (4)0.037 (5)0.027 (4)0.009 (4)0.008 (3)0.009 (3)
C140.029 (5)0.044 (5)0.043 (5)0.001 (4)0.009 (4)0.018 (4)
Geometric parameters (Å, º) top
Co1—N22.012 (6)O12—H12A0.8709
Co1—N12.017 (6)O12—H12B0.8588
Co1—O32.106 (5)O13—H13A1.0465
Co1—O12.181 (5)O13—H13B0.7999
Co1—O52.193 (5)O14—H14A1.0063
Co1—O72.200 (6)O14—H14B0.9744
Co2—O102.107 (5)O15—H15A1.0336
Co2—O10i2.107 (5)O15—H15B1.0456
Co2—O92.118 (6)O16—H16A0.9919
Co2—O9i2.118 (6)O16—H16B0.9807
Co2—O112.148 (6)N1—C61.339 (8)
Co2—O11i2.148 (6)N1—C21.347 (9)
Co3—O142.092 (6)N2—C91.309 (9)
Co3—O14ii2.092 (6)N2—C131.346 (9)
Co3—O132.136 (6)C1—C21.523 (10)
Co3—O13ii2.136 (6)C2—C31.373 (10)
Co3—O12ii2.150 (8)C3—C41.412 (11)
Co3—O122.150 (8)C3—H3A1.0417
O1—C11.251 (9)C4—C51.355 (11)
O2—C11.230 (9)C4—H4A1.0135
O3—C71.280 (10)C5—C61.379 (10)
O4—C71.236 (9)C5—H5A0.9274
O5—C81.282 (9)C6—C71.500 (11)
O6—C81.230 (10)C8—C91.517 (10)
O7—C141.281 (9)C9—C101.375 (10)
O8—C141.225 (9)C10—C111.384 (12)
O9—H9A0.9161C10—H10C1.0811
O9—H9B0.9384C11—C121.378 (13)
O10—H10A0.9407C11—H11C1.0228
O10—H10B1.0090C12—C131.379 (11)
O11—H11A0.9756C12—H12C0.8897
O11—H11B0.9846C13—C141.507 (11)
N2—Co1—N1164.6 (2)Co3—O12—H12B122.1
N2—Co1—O3115.7 (2)H12A—O12—H12B116.7
N1—Co1—O376.6 (2)Co3—O13—H13A127.0
N2—Co1—O193.5 (2)Co3—O13—H13B144.5
N1—Co1—O174.9 (2)H13A—O13—H13B83.6
O3—Co1—O1150.8 (2)Co3—O14—H14A98.2
N2—Co1—O575.5 (2)Co3—O14—H14B118.4
N1—Co1—O595.9 (2)H14A—O14—H14B90.8
O3—Co1—O590.8 (2)H15A—O15—H15B103.1
O1—Co1—O598.4 (2)H16A—O16—H16B100.5
N2—Co1—O777.1 (2)C6—N1—C2121.2 (6)
N1—Co1—O7112.1 (2)C6—N1—Co1118.0 (5)
O3—Co1—O795.9 (2)C2—N1—Co1120.8 (5)
O1—Co1—O788.9 (2)C9—N2—C13121.3 (6)
O5—Co1—O7152.0 (2)C9—N2—Co1121.0 (5)
O10—Co2—O10i180.000 (1)C13—N2—Co1117.6 (5)
O10—Co2—O987.8 (2)O2—C1—O1126.5 (7)
O10i—Co2—O992.2 (2)O2—C1—C2118.9 (7)
O10—Co2—O9i92.2 (2)O1—C1—C2114.7 (7)
O10i—Co2—O9i87.8 (2)N1—C2—C3120.6 (7)
O9—Co2—O9i180.000 (1)N1—C2—C1112.2 (6)
O10—Co2—O1191.7 (3)C3—C2—C1127.2 (7)
O10i—Co2—O1188.3 (2)C2—C3—C4117.7 (7)
O9—Co2—O1187.5 (2)C2—C3—H3A123.4
O9i—Co2—O1192.5 (2)C4—C3—H3A119.0
O10—Co2—O11i88.3 (2)C5—C4—C3121.0 (7)
O10i—Co2—O11i91.7 (3)C5—C4—H4A105.3
O9—Co2—O11i92.5 (2)C3—C4—H4A129.7
O9i—Co2—O11i87.5 (2)C4—C5—C6118.4 (7)
O11—Co2—O11i180.000 (1)C4—C5—H5A123.7
O14—Co3—O14ii180.0C6—C5—H5A117.9
O14—Co3—O1390.6 (2)N1—C6—C5121.1 (7)
O14ii—Co3—O1389.4 (2)N1—C6—C7113.3 (6)
O14—Co3—O13ii89.4 (2)C5—C6—C7125.5 (7)
O14ii—Co3—O13ii90.6 (2)O4—C7—O3125.6 (8)
O13—Co3—O13ii180.0 (2)O4—C7—C6120.1 (8)
O14—Co3—O12ii91.7 (3)O3—C7—C6114.3 (7)
O14ii—Co3—O12ii88.3 (3)O6—C8—O5125.4 (8)
O13—Co3—O12ii89.1 (3)O6—C8—C9119.8 (7)
O13ii—Co3—O12ii90.9 (3)O5—C8—C9114.7 (7)
O14—Co3—O1288.3 (3)N2—C9—C10122.1 (7)
O14ii—Co3—O1291.7 (3)N2—C9—C8113.6 (7)
O13—Co3—O1290.9 (3)C10—C9—C8124.3 (7)
O13ii—Co3—O1289.1 (3)C9—C10—C11117.1 (8)
O12ii—Co3—O12180.000 (1)C9—C10—H10C113.7
C1—O1—Co1117.4 (5)C11—C10—H10C129.2
C7—O3—Co1116.3 (5)C12—C11—C10121.3 (8)
C8—O5—Co1115.0 (5)C12—C11—H11C110.6
C14—O7—Co1113.7 (5)C10—C11—H11C127.8
Co2—O9—H9A114.9C11—C12—C13117.7 (7)
Co2—O9—H9B115.1C11—C12—H12C128.5
H9A—O9—H9B105.5C13—C12—H12C112.8
Co2—O10—H10A110.6N2—C13—C12120.5 (7)
Co2—O10—H10B112.2N2—C13—C14115.5 (6)
H10A—O10—H10B105.0C12—C13—C14124.1 (7)
Co2—O11—H11A135.9O8—C14—O7125.2 (8)
Co2—O11—H11B106.7O8—C14—C13119.7 (7)
H11A—O11—H11B116.9O7—C14—C13115.1 (7)
Co3—O12—H12A121.2
Symmetry codes: (i) x1, y+1, z+1; (ii) x+1, y+2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O14—H14B···O10.981.912.77 (1)147
O13—H13A···O2ii1.051.812.85 (2)169
O9—H9B···O2iii0.941.862.79 (3)172
O10—H10B···O4i1.011.712.69 (3)163
O15—H15B···O41.051.872.84 (2)154
O9—H9A···O5iv0.921.852.76 (1)176
O10—H10A···O6v0.941.832.76 (2)168
O11—H11B···O6iv0.992.493.39 (2)153
O14—H14A···O8vi1.011.832.75 (2)152
O16—H16A···O8vi0.991.982.92 (2)156
O13—H13B···O15vii0.802.383.16 (4)165
O16—H16B···O15iii0.982.323.28 (3)166
C5—H5A···O16iii0.932.343.25 (2)166
Symmetry codes: (i) x1, y+1, z+1; (ii) x+1, y+2, z; (iii) x, y+2, z+1; (iv) x1, y, z; (v) x, y+1, z+1; (vi) x, y+2, z; (vii) x, y, z1.
 

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