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
CCDC reference: 272011
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (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
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).
Crystal data top
2[Co(C12H8N2)(H2O)4](C10H2O8) | Z = 1 |
Mr = 872.52 | F(000) = 448 |
Triclinic, P1 | Dx = 1.669 Mg m−3 |
a = 7.3184 (4) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 9.8767 (6) Å | Cell parameters from 7794 reflections |
c = 12.5639 (7) Å | θ = 2.2–27.4° |
α = 76.600 (3)° | µ = 1.04 mm−1 |
β = 88.384 (3)° | T = 293 K |
γ = 79.414 (3)° | Needle, red |
V = 868.28 (9) Å3 | 0.38 × 0.12 × 0.12 mm |
Data collection top
Rigaku R-AXIS RAPID IP diffractometer | 3866 independent reflections |
Radiation source: rotating anode | 3295 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
Oscillation scans | θmax = 27.4°, θmin = 2.2° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −9→9 |
Tmin = 0.693, Tmax = 0.885 | k = −12→12 |
6047 measured reflections | l = −16→16 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.035 | H 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 reflections | Δρmax = 0.38 e Å−3 |
278 parameters | Δρmin = −0.39 e Å−3 |
8 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction 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 | x | y | z | Uiso*/Ueq | |
Co1 | 0.64053 (4) | 0.85894 (3) | 0.22108 (2) | 0.02526 (10) | |
N1 | 0.6826 (2) | 0.63377 (17) | 0.27844 (14) | 0.0289 (4) | |
N2 | 0.6988 (3) | 0.83307 (18) | 0.38971 (14) | 0.0316 (4) | |
O1 | 0.5820 (3) | 0.86066 (18) | 0.06008 (13) | 0.0463 (4) | |
O2 | 0.9114 (3) | 0.86898 (18) | 0.1854 (2) | 0.0563 (6) | |
O3 | 0.3538 (2) | 0.87296 (14) | 0.24863 (12) | 0.0290 (3) | |
O4 | 0.5925 (2) | 1.08613 (15) | 0.19283 (13) | 0.0345 (3) | |
C1 | 0.6759 (3) | 0.5367 (2) | 0.2226 (2) | 0.0388 (5) | |
H1B | 0.6554 | 0.5654 | 0.1473 | 0.047* | |
C2 | 0.6984 (4) | 0.3928 (3) | 0.2721 (3) | 0.0526 (7) | |
H2B | 0.6927 | 0.3271 | 0.2305 | 0.063* | |
C3 | 0.7291 (4) | 0.3496 (3) | 0.3828 (3) | 0.0546 (7) | |
H3B | 0.7438 | 0.2539 | 0.4168 | 0.065* | |
C4 | 0.7383 (3) | 0.4483 (2) | 0.4447 (2) | 0.0423 (5) | |
C5 | 0.7749 (4) | 0.4127 (3) | 0.5604 (2) | 0.0548 (7) | |
H5A | 0.7902 | 0.3184 | 0.5981 | 0.066* | |
C6 | 0.7875 (4) | 0.5117 (3) | 0.6155 (2) | 0.0559 (7) | |
H6A | 0.8125 | 0.4851 | 0.6904 | 0.067* | |
C7 | 0.7629 (3) | 0.6577 (3) | 0.56032 (19) | 0.0428 (5) | |
C8 | 0.7767 (4) | 0.7667 (3) | 0.6128 (2) | 0.0561 (7) | |
H8A | 0.8022 | 0.7457 | 0.6875 | 0.067* | |
C9 | 0.7530 (5) | 0.9021 (4) | 0.5544 (2) | 0.0618 (8) | |
H9A | 0.7626 | 0.9747 | 0.5884 | 0.074* | |
C10 | 0.7139 (4) | 0.9320 (3) | 0.4422 (2) | 0.0477 (6) | |
H10A | 0.6979 | 1.0257 | 0.4029 | 0.057* | |
C11 | 0.7244 (3) | 0.6968 (2) | 0.44710 (17) | 0.0304 (4) | |
C12 | 0.7135 (3) | 0.5908 (2) | 0.38810 (17) | 0.0298 (4) | |
O21 | 0.2228 (2) | 0.70249 (16) | 0.14356 (13) | 0.0342 (3) | |
O22 | 0.4001 (2) | 0.68251 (16) | −0.00092 (13) | 0.0349 (3) | |
O23 | 0.2179 (3) | 0.14526 (16) | 0.14907 (18) | 0.0542 (5) | |
O24 | −0.0594 (3) | 0.13250 (18) | 0.0991 (2) | 0.0714 (7) | |
C21 | 0.2588 (3) | 0.66550 (18) | 0.05477 (16) | 0.0254 (4) | |
C22 | 0.1239 (3) | 0.58368 (18) | 0.02119 (15) | 0.0231 (4) | |
C23 | 0.1527 (3) | 0.43885 (19) | 0.06703 (15) | 0.0242 (4) | |
H23A | 0.2564 | 0.3973 | 0.1119 | 0.029* | |
C24 | 0.0304 (3) | 0.35463 (18) | 0.04742 (15) | 0.0229 (4) | |
C25 | 0.0657 (3) | 0.19882 (19) | 0.10259 (16) | 0.0253 (4) | |
H1A | 0.533 (5) | 0.800 (3) | 0.043 (3) | 0.080* | |
H2A | 0.935 (5) | 0.947 (2) | 0.155 (3) | 0.080* | |
H2C | 0.986 (4) | 0.806 (3) | 0.168 (3) | 0.080* | |
H3A | 0.298 (4) | 0.952 (2) | 0.219 (3) | 0.080* | |
H3C | 0.317 (5) | 0.818 (3) | 0.218 (3) | 0.080* | |
H4A | 0.486 (2) | 1.127 (4) | 0.174 (3) | 0.080* | |
H4B | 0.654 (4) | 1.133 (3) | 0.149 (2) | 0.080* | |
H1C | 0.615 (5) | 0.916 (3) | 0.009 (2) | 0.080* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.03251 (16) | 0.01954 (14) | 0.02431 (15) | −0.00737 (10) | −0.00060 (10) | −0.00402 (9) |
N1 | 0.0315 (9) | 0.0235 (8) | 0.0316 (9) | −0.0057 (6) | −0.0006 (7) | −0.0055 (6) |
N2 | 0.0375 (10) | 0.0280 (8) | 0.0297 (9) | −0.0055 (7) | −0.0048 (7) | −0.0071 (7) |
O1 | 0.0804 (13) | 0.0398 (9) | 0.0272 (8) | −0.0310 (9) | 0.0078 (8) | −0.0103 (7) |
O2 | 0.0437 (10) | 0.0249 (8) | 0.0986 (16) | −0.0095 (7) | 0.0281 (10) | −0.0112 (9) |
O3 | 0.0332 (8) | 0.0230 (7) | 0.0308 (7) | −0.0064 (6) | −0.0050 (6) | −0.0044 (5) |
O4 | 0.0441 (9) | 0.0224 (7) | 0.0370 (8) | −0.0104 (6) | 0.0005 (7) | −0.0032 (6) |
C1 | 0.0482 (13) | 0.0293 (11) | 0.0412 (12) | −0.0068 (9) | −0.0002 (10) | −0.0132 (9) |
C2 | 0.0640 (17) | 0.0273 (11) | 0.0707 (19) | −0.0097 (11) | −0.0001 (14) | −0.0188 (12) |
C3 | 0.0640 (17) | 0.0214 (11) | 0.0721 (19) | −0.0087 (10) | −0.0001 (14) | 0.0023 (11) |
C4 | 0.0415 (13) | 0.0278 (11) | 0.0507 (14) | −0.0057 (9) | 0.0000 (11) | 0.0048 (9) |
C5 | 0.0595 (17) | 0.0409 (14) | 0.0489 (15) | −0.0066 (12) | −0.0021 (13) | 0.0183 (12) |
C6 | 0.0592 (17) | 0.0626 (18) | 0.0333 (13) | −0.0055 (14) | −0.0037 (12) | 0.0101 (12) |
C7 | 0.0395 (13) | 0.0571 (15) | 0.0276 (11) | −0.0057 (11) | −0.0023 (9) | −0.0034 (10) |
C8 | 0.0634 (18) | 0.075 (2) | 0.0307 (13) | −0.0080 (15) | −0.0088 (12) | −0.0168 (12) |
C9 | 0.079 (2) | 0.0680 (19) | 0.0480 (16) | −0.0114 (16) | −0.0148 (15) | −0.0325 (14) |
C10 | 0.0648 (17) | 0.0380 (13) | 0.0452 (14) | −0.0093 (11) | −0.0107 (12) | −0.0180 (10) |
C11 | 0.0273 (10) | 0.0337 (10) | 0.0283 (10) | −0.0050 (8) | −0.0015 (8) | −0.0034 (8) |
C12 | 0.0279 (10) | 0.0268 (10) | 0.0318 (10) | −0.0062 (8) | −0.0001 (8) | 0.0004 (8) |
O21 | 0.0388 (8) | 0.0330 (8) | 0.0369 (8) | −0.0119 (6) | 0.0004 (6) | −0.0159 (6) |
O22 | 0.0332 (8) | 0.0377 (8) | 0.0375 (8) | −0.0145 (6) | 0.0026 (6) | −0.0099 (6) |
O23 | 0.0462 (10) | 0.0201 (7) | 0.0881 (14) | −0.0043 (7) | −0.0329 (10) | 0.0065 (8) |
O24 | 0.0435 (11) | 0.0260 (9) | 0.130 (2) | −0.0151 (8) | −0.0277 (12) | 0.0226 (10) |
C21 | 0.0295 (10) | 0.0161 (8) | 0.0290 (9) | −0.0035 (7) | −0.0060 (8) | −0.0016 (7) |
C22 | 0.0276 (9) | 0.0187 (8) | 0.0233 (9) | −0.0057 (7) | −0.0004 (7) | −0.0044 (7) |
C23 | 0.0265 (9) | 0.0200 (8) | 0.0246 (9) | −0.0031 (7) | −0.0063 (7) | −0.0025 (7) |
C24 | 0.0274 (9) | 0.0171 (8) | 0.0239 (9) | −0.0043 (7) | −0.0005 (7) | −0.0034 (6) |
C25 | 0.0300 (10) | 0.0176 (8) | 0.0270 (9) | −0.0046 (7) | −0.0002 (8) | −0.0022 (7) |
Geometric parameters (Å, º) top
Co1—O1 | 2.0750 (17) | C4—C5 | 1.434 (4) |
Co1—O2 | 2.0350 (18) | C5—C6 | 1.339 (5) |
Co1—O3 | 2.1016 (15) | C5—H5A | 0.9300 |
Co1—O4 | 2.1524 (15) | C6—C7 | 1.429 (4) |
Co1—N1 | 2.1397 (16) | C6—H6A | 0.9300 |
Co1—N2 | 2.1204 (18) | C7—C8 | 1.405 (4) |
N1—C1 | 1.321 (3) | C7—C11 | 1.407 (3) |
N1—C12 | 1.357 (3) | C8—C9 | 1.350 (4) |
N2—C10 | 1.322 (3) | C8—H8A | 0.9300 |
N2—C11 | 1.353 (3) | C9—C10 | 1.397 (4) |
O1—H1A | 0.82 (3) | C9—H9A | 0.9300 |
O1—H1C | 0.80 (3) | C10—H10A | 0.9300 |
O2—H2A | 0.82 (3) | C11—C12 | 1.430 (3) |
O2—H2C | 0.82 (3) | O21—C21 | 1.259 (2) |
O3—H3A | 0.82 (3) | O22—C21 | 1.247 (2) |
O3—H3C | 0.82 (3) | O23—C25 | 1.241 (3) |
O4—H4A | 0.82 (2) | O24—C25 | 1.227 (3) |
O4—H4B | 0.82 (3) | C21—C22 | 1.510 (3) |
C1—C2 | 1.394 (3) | C22—C23 | 1.392 (2) |
C1—H1B | 0.9300 | C22—C24i | 1.396 (3) |
C2—C3 | 1.369 (4) | C23—C24 | 1.391 (3) |
C2—H2B | 0.9300 | C23—H23A | 0.9300 |
C3—C4 | 1.393 (4) | C24—C22i | 1.396 (3) |
C3—H3B | 0.9300 | C24—C25 | 1.512 (2) |
C4—C12 | 1.403 (3) | | |
| | | |
O1—Co1—O2 | 91.32 (9) | C3—C4—C12 | 116.7 (2) |
O1—Co1—O3 | 86.90 (7) | C3—C4—C5 | 124.2 (2) |
O1—Co1—O4 | 93.85 (7) | C12—C4—C5 | 119.1 (2) |
O1—Co1—N1 | 95.59 (7) | C6—C5—C4 | 121.8 (2) |
O1—Co1—N2 | 173.67 (7) | C6—C5—H5A | 119.1 |
O2—Co1—O3 | 173.48 (6) | C4—C5—H5A | 119.1 |
O2—Co1—O4 | 86.87 (7) | C5—C6—C7 | 120.6 (2) |
O2—Co1—N1 | 95.98 (7) | C5—C6—H6A | 119.7 |
O2—Co1—N2 | 90.37 (9) | C7—C6—H6A | 119.7 |
O3—Co1—O4 | 86.99 (6) | C8—C7—C11 | 117.2 (2) |
O3—Co1—N1 | 90.44 (6) | C8—C7—C6 | 123.6 (2) |
O3—Co1—N2 | 92.07 (6) | C11—C7—C6 | 119.2 (3) |
O4—Co1—N1 | 170.07 (6) | C9—C8—C7 | 119.8 (2) |
O4—Co1—N2 | 92.33 (6) | C9—C8—H8A | 120.1 |
N1—Co1—N2 | 78.17 (7) | C7—C8—H8A | 120.1 |
C1—N1—C12 | 118.32 (18) | C8—C9—C10 | 119.4 (3) |
C1—N1—Co1 | 128.82 (15) | C8—C9—H9A | 120.3 |
C12—N1—Co1 | 112.82 (13) | C10—C9—H9A | 120.3 |
C10—N2—C11 | 118.4 (2) | N2—C10—C9 | 122.8 (2) |
C10—N2—Co1 | 127.93 (16) | N2—C10—H10A | 118.6 |
C11—N2—Co1 | 113.70 (14) | C9—C10—H10A | 118.6 |
Co1—O1—H1A | 123 (3) | N2—C11—C7 | 122.4 (2) |
Co1—O1—H1C | 123 (3) | N2—C11—C12 | 117.51 (18) |
H1A—O1—H1C | 114 (4) | C7—C11—C12 | 120.1 (2) |
Co1—O2—H2A | 117 (3) | N1—C12—C4 | 123.1 (2) |
Co1—O2—H2C | 125 (3) | N1—C12—C11 | 117.68 (17) |
H2A—O2—H2C | 111 (4) | C4—C12—C11 | 119.2 (2) |
Co1—O3—H3A | 110 (3) | O22—C21—O21 | 125.34 (19) |
Co1—O3—H3C | 108 (3) | O22—C21—C22 | 119.36 (17) |
H3A—O3—H3C | 106 (4) | O21—C21—C22 | 115.09 (17) |
Co1—O4—H4A | 116 (3) | C23—C22—C24i | 119.00 (17) |
Co1—O4—H4B | 121 (3) | C23—C22—C21 | 116.79 (17) |
H4A—O4—H4B | 102 (3) | C24i—C22—C21 | 124.13 (16) |
N1—C1—C2 | 122.5 (2) | C24—C23—C22 | 121.71 (18) |
N1—C1—H1B | 118.7 | C24—C23—H23A | 119.1 |
C2—C1—H1B | 118.7 | C22—C23—H23A | 119.1 |
C3—C2—C1 | 119.1 (2) | C23—C24—C22i | 119.29 (16) |
C3—C2—H2B | 120.5 | C23—C24—C25 | 119.23 (17) |
C1—C2—H2B | 120.5 | C22i—C24—C25 | 121.48 (16) |
C2—C3—C4 | 120.3 (2) | O24—C25—O23 | 123.67 (18) |
C2—C3—H3B | 119.9 | O24—C25—C24 | 117.67 (18) |
C4—C3—H3B | 119.9 | O23—C25—C24 | 118.66 (17) |
Symmetry code: (i) −x, −y+1, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···O22 | 0.82 (3) | 1.83 (3) | 2.646 (3) | 173 (4) |
O1—H1C···O1ii | 0.80 (3) | 2.39 (3) | 2.874 (3) | 120 (3) |
O1—H1C···O23iii | 0.80 (3) | 2.44 (3) | 2.979 (3) | 126 (3) |
O2—H2A···O24iv | 0.82 (3) | 1.81 (2) | 2.623 (3) | 168 (3) |
O2—H2C···O21v | 0.82 (3) | 1.90 (3) | 2.670 (3) | 157 (3) |
O3—H3A···O23vi | 0.82 (3) | 1.90 (3) | 2.705 (2) | 168 (3) |
O3—H3C···O21 | 0.82 (3) | 1.86 (3) | 2.682 (2) | 177 (4) |
O4—H4A···O23vi | 0.82 (2) | 1.96 (2) | 2.740 (3) | 157 (4) |
O4—H4B···O22ii | 0.82 (3) | 2.27 (3) | 2.919 (2) | 137 (3) |
O4—H4B···O24iv | 0.82 (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. |