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The title compound, [Co(C12H8N2)(H2O)4]2(C10H2O8), consists of discrete tetra­aqua­(1,10-phenanthroline)cobalt(II) cations and 1,2,4,5-benzene­tetra­carboxyl­ate anions. The CoII atom is octa­hedrally coordinated by two N atoms of the 1,10-phenanthroline ligand and four O atoms of water mol­ecules. The anion lies on an inversion centre. A two-dimensional hydrogen-bonding network is formed by O atoms of benzene­tetra­carboxyl­ate and the coordinated water mol­ecules.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680501161X/is6065sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680501161X/is6065Isup2.hkl
Contains datablock I

CCDC reference: 272011

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.035
  • wR factor = 0.087
  • Data-to-parameter ratio = 13.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C25 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.47 PLAT417_ALERT_2_C Short Inter D-H..H-D H1C .. H1C .. 2.11 Ang.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 5 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 1 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: RAPID-AUTO (Rigaku, 2001); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1994); software used to prepare material for publication: SHELXTL (Siemens, 1995).

(I) top
Crystal data top
2[Co(C12H8N2)(H2O)4](C10H2O8)Z = 1
Mr = 872.52F(000) = 448
Triclinic, P1Dx = 1.669 Mg m3
a = 7.3184 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.8767 (6) ÅCell parameters from 7794 reflections
c = 12.5639 (7) Åθ = 2.2–27.4°
α = 76.600 (3)°µ = 1.04 mm1
β = 88.384 (3)°T = 293 K
γ = 79.414 (3)°Needle, red
V = 868.28 (9) Å30.38 × 0.12 × 0.12 mm
Data collection top
Rigaku R-AXIS RAPID IP
diffractometer
3866 independent reflections
Radiation source: rotating anode3295 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
Oscillation scansθmax = 27.4°, θmin = 2.2°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 99
Tmin = 0.693, Tmax = 0.885k = 1212
6047 measured reflectionsl = 1616
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.035H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.087 w = 1/[σ2(Fo2) + (0.0453P)2 + 0.4128P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
3866 reflectionsΔρmax = 0.38 e Å3
278 parametersΔρmin = 0.39 e Å3
8 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0101 (15)
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
Co10.64053 (4)0.85894 (3)0.22108 (2)0.02526 (10)
N10.6826 (2)0.63377 (17)0.27844 (14)0.0289 (4)
N20.6988 (3)0.83307 (18)0.38971 (14)0.0316 (4)
O10.5820 (3)0.86066 (18)0.06008 (13)0.0463 (4)
O20.9114 (3)0.86898 (18)0.1854 (2)0.0563 (6)
O30.3538 (2)0.87296 (14)0.24863 (12)0.0290 (3)
O40.5925 (2)1.08613 (15)0.19283 (13)0.0345 (3)
C10.6759 (3)0.5367 (2)0.2226 (2)0.0388 (5)
H1B0.65540.56540.14730.047*
C20.6984 (4)0.3928 (3)0.2721 (3)0.0526 (7)
H2B0.69270.32710.23050.063*
C30.7291 (4)0.3496 (3)0.3828 (3)0.0546 (7)
H3B0.74380.25390.41680.065*
C40.7383 (3)0.4483 (2)0.4447 (2)0.0423 (5)
C50.7749 (4)0.4127 (3)0.5604 (2)0.0548 (7)
H5A0.79020.31840.59810.066*
C60.7875 (4)0.5117 (3)0.6155 (2)0.0559 (7)
H6A0.81250.48510.69040.067*
C70.7629 (3)0.6577 (3)0.56032 (19)0.0428 (5)
C80.7767 (4)0.7667 (3)0.6128 (2)0.0561 (7)
H8A0.80220.74570.68750.067*
C90.7530 (5)0.9021 (4)0.5544 (2)0.0618 (8)
H9A0.76260.97470.58840.074*
C100.7139 (4)0.9320 (3)0.4422 (2)0.0477 (6)
H10A0.69791.02570.40290.057*
C110.7244 (3)0.6968 (2)0.44710 (17)0.0304 (4)
C120.7135 (3)0.5908 (2)0.38810 (17)0.0298 (4)
O210.2228 (2)0.70249 (16)0.14356 (13)0.0342 (3)
O220.4001 (2)0.68251 (16)0.00092 (13)0.0349 (3)
O230.2179 (3)0.14526 (16)0.14907 (18)0.0542 (5)
O240.0594 (3)0.13250 (18)0.0991 (2)0.0714 (7)
C210.2588 (3)0.66550 (18)0.05477 (16)0.0254 (4)
C220.1239 (3)0.58368 (18)0.02119 (15)0.0231 (4)
C230.1527 (3)0.43885 (19)0.06703 (15)0.0242 (4)
H23A0.25640.39730.11190.029*
C240.0304 (3)0.35463 (18)0.04742 (15)0.0229 (4)
C250.0657 (3)0.19882 (19)0.10259 (16)0.0253 (4)
H1A0.533 (5)0.800 (3)0.043 (3)0.080*
H2A0.935 (5)0.947 (2)0.155 (3)0.080*
H2C0.986 (4)0.806 (3)0.168 (3)0.080*
H3A0.298 (4)0.952 (2)0.219 (3)0.080*
H3C0.317 (5)0.818 (3)0.218 (3)0.080*
H4A0.486 (2)1.127 (4)0.174 (3)0.080*
H4B0.654 (4)1.133 (3)0.149 (2)0.080*
H1C0.615 (5)0.916 (3)0.009 (2)0.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.03251 (16)0.01954 (14)0.02431 (15)0.00737 (10)0.00060 (10)0.00402 (9)
N10.0315 (9)0.0235 (8)0.0316 (9)0.0057 (6)0.0006 (7)0.0055 (6)
N20.0375 (10)0.0280 (8)0.0297 (9)0.0055 (7)0.0048 (7)0.0071 (7)
O10.0804 (13)0.0398 (9)0.0272 (8)0.0310 (9)0.0078 (8)0.0103 (7)
O20.0437 (10)0.0249 (8)0.0986 (16)0.0095 (7)0.0281 (10)0.0112 (9)
O30.0332 (8)0.0230 (7)0.0308 (7)0.0064 (6)0.0050 (6)0.0044 (5)
O40.0441 (9)0.0224 (7)0.0370 (8)0.0104 (6)0.0005 (7)0.0032 (6)
C10.0482 (13)0.0293 (11)0.0412 (12)0.0068 (9)0.0002 (10)0.0132 (9)
C20.0640 (17)0.0273 (11)0.0707 (19)0.0097 (11)0.0001 (14)0.0188 (12)
C30.0640 (17)0.0214 (11)0.0721 (19)0.0087 (10)0.0001 (14)0.0023 (11)
C40.0415 (13)0.0278 (11)0.0507 (14)0.0057 (9)0.0000 (11)0.0048 (9)
C50.0595 (17)0.0409 (14)0.0489 (15)0.0066 (12)0.0021 (13)0.0183 (12)
C60.0592 (17)0.0626 (18)0.0333 (13)0.0055 (14)0.0037 (12)0.0101 (12)
C70.0395 (13)0.0571 (15)0.0276 (11)0.0057 (11)0.0023 (9)0.0034 (10)
C80.0634 (18)0.075 (2)0.0307 (13)0.0080 (15)0.0088 (12)0.0168 (12)
C90.079 (2)0.0680 (19)0.0480 (16)0.0114 (16)0.0148 (15)0.0325 (14)
C100.0648 (17)0.0380 (13)0.0452 (14)0.0093 (11)0.0107 (12)0.0180 (10)
C110.0273 (10)0.0337 (10)0.0283 (10)0.0050 (8)0.0015 (8)0.0034 (8)
C120.0279 (10)0.0268 (10)0.0318 (10)0.0062 (8)0.0001 (8)0.0004 (8)
O210.0388 (8)0.0330 (8)0.0369 (8)0.0119 (6)0.0004 (6)0.0159 (6)
O220.0332 (8)0.0377 (8)0.0375 (8)0.0145 (6)0.0026 (6)0.0099 (6)
O230.0462 (10)0.0201 (7)0.0881 (14)0.0043 (7)0.0329 (10)0.0065 (8)
O240.0435 (11)0.0260 (9)0.130 (2)0.0151 (8)0.0277 (12)0.0226 (10)
C210.0295 (10)0.0161 (8)0.0290 (9)0.0035 (7)0.0060 (8)0.0016 (7)
C220.0276 (9)0.0187 (8)0.0233 (9)0.0057 (7)0.0004 (7)0.0044 (7)
C230.0265 (9)0.0200 (8)0.0246 (9)0.0031 (7)0.0063 (7)0.0025 (7)
C240.0274 (9)0.0171 (8)0.0239 (9)0.0043 (7)0.0005 (7)0.0034 (6)
C250.0300 (10)0.0176 (8)0.0270 (9)0.0046 (7)0.0002 (8)0.0022 (7)
Geometric parameters (Å, º) top
Co1—O12.0750 (17)C4—C51.434 (4)
Co1—O22.0350 (18)C5—C61.339 (5)
Co1—O32.1016 (15)C5—H5A0.9300
Co1—O42.1524 (15)C6—C71.429 (4)
Co1—N12.1397 (16)C6—H6A0.9300
Co1—N22.1204 (18)C7—C81.405 (4)
N1—C11.321 (3)C7—C111.407 (3)
N1—C121.357 (3)C8—C91.350 (4)
N2—C101.322 (3)C8—H8A0.9300
N2—C111.353 (3)C9—C101.397 (4)
O1—H1A0.82 (3)C9—H9A0.9300
O1—H1C0.80 (3)C10—H10A0.9300
O2—H2A0.82 (3)C11—C121.430 (3)
O2—H2C0.82 (3)O21—C211.259 (2)
O3—H3A0.82 (3)O22—C211.247 (2)
O3—H3C0.82 (3)O23—C251.241 (3)
O4—H4A0.82 (2)O24—C251.227 (3)
O4—H4B0.82 (3)C21—C221.510 (3)
C1—C21.394 (3)C22—C231.392 (2)
C1—H1B0.9300C22—C24i1.396 (3)
C2—C31.369 (4)C23—C241.391 (3)
C2—H2B0.9300C23—H23A0.9300
C3—C41.393 (4)C24—C22i1.396 (3)
C3—H3B0.9300C24—C251.512 (2)
C4—C121.403 (3)
O1—Co1—O291.32 (9)C3—C4—C12116.7 (2)
O1—Co1—O386.90 (7)C3—C4—C5124.2 (2)
O1—Co1—O493.85 (7)C12—C4—C5119.1 (2)
O1—Co1—N195.59 (7)C6—C5—C4121.8 (2)
O1—Co1—N2173.67 (7)C6—C5—H5A119.1
O2—Co1—O3173.48 (6)C4—C5—H5A119.1
O2—Co1—O486.87 (7)C5—C6—C7120.6 (2)
O2—Co1—N195.98 (7)C5—C6—H6A119.7
O2—Co1—N290.37 (9)C7—C6—H6A119.7
O3—Co1—O486.99 (6)C8—C7—C11117.2 (2)
O3—Co1—N190.44 (6)C8—C7—C6123.6 (2)
O3—Co1—N292.07 (6)C11—C7—C6119.2 (3)
O4—Co1—N1170.07 (6)C9—C8—C7119.8 (2)
O4—Co1—N292.33 (6)C9—C8—H8A120.1
N1—Co1—N278.17 (7)C7—C8—H8A120.1
C1—N1—C12118.32 (18)C8—C9—C10119.4 (3)
C1—N1—Co1128.82 (15)C8—C9—H9A120.3
C12—N1—Co1112.82 (13)C10—C9—H9A120.3
C10—N2—C11118.4 (2)N2—C10—C9122.8 (2)
C10—N2—Co1127.93 (16)N2—C10—H10A118.6
C11—N2—Co1113.70 (14)C9—C10—H10A118.6
Co1—O1—H1A123 (3)N2—C11—C7122.4 (2)
Co1—O1—H1C123 (3)N2—C11—C12117.51 (18)
H1A—O1—H1C114 (4)C7—C11—C12120.1 (2)
Co1—O2—H2A117 (3)N1—C12—C4123.1 (2)
Co1—O2—H2C125 (3)N1—C12—C11117.68 (17)
H2A—O2—H2C111 (4)C4—C12—C11119.2 (2)
Co1—O3—H3A110 (3)O22—C21—O21125.34 (19)
Co1—O3—H3C108 (3)O22—C21—C22119.36 (17)
H3A—O3—H3C106 (4)O21—C21—C22115.09 (17)
Co1—O4—H4A116 (3)C23—C22—C24i119.00 (17)
Co1—O4—H4B121 (3)C23—C22—C21116.79 (17)
H4A—O4—H4B102 (3)C24i—C22—C21124.13 (16)
N1—C1—C2122.5 (2)C24—C23—C22121.71 (18)
N1—C1—H1B118.7C24—C23—H23A119.1
C2—C1—H1B118.7C22—C23—H23A119.1
C3—C2—C1119.1 (2)C23—C24—C22i119.29 (16)
C3—C2—H2B120.5C23—C24—C25119.23 (17)
C1—C2—H2B120.5C22i—C24—C25121.48 (16)
C2—C3—C4120.3 (2)O24—C25—O23123.67 (18)
C2—C3—H3B119.9O24—C25—C24117.67 (18)
C4—C3—H3B119.9O23—C25—C24118.66 (17)
Symmetry code: (i) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O220.82 (3)1.83 (3)2.646 (3)173 (4)
O1—H1C···O1ii0.80 (3)2.39 (3)2.874 (3)120 (3)
O1—H1C···O23iii0.80 (3)2.44 (3)2.979 (3)126 (3)
O2—H2A···O24iv0.82 (3)1.81 (2)2.623 (3)168 (3)
O2—H2C···O21v0.82 (3)1.90 (3)2.670 (3)157 (3)
O3—H3A···O23vi0.82 (3)1.90 (3)2.705 (2)168 (3)
O3—H3C···O210.82 (3)1.86 (3)2.682 (2)177 (4)
O4—H4A···O23vi0.82 (2)1.96 (2)2.740 (3)157 (4)
O4—H4B···O22ii0.82 (3)2.27 (3)2.919 (2)137 (3)
O4—H4B···O24iv0.82 (3)2.17 (3)2.845 (3)140 (3)
Symmetry codes: (ii) x+1, y+2, z; (iii) x+1, y+1, z; (iv) x+1, y+1, z; (v) x+1, y, z; (vi) x, y+1, z.
 

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