Acta Cryst. (2009). E65, m1284 [ doi:10.1107/S1600536809039580 ]
![[mu]](/logos/entities/mu_rmgif.gif)
4-succinato-tetrakis[aquaphenanthrolinecopper(II)] tetranitrate tetrahydrateIn the title compound, [Cu4(C4H4O4)2(C12H8N2)4(H2O)4](NO3)4·4H2O, the complete tetracation is generated by crystallographic inversion symmetry. Both unique Cu2+ ions are coordinated by an N,N'-bidentate phenanthroline molecule, two O-monodentate bis-bridging succinate dianions and a water molecule, resulting in distorted CuN2O3 square-based pyramidal geometries for the metal ions, with the water molecule occupying the apical site. In the crystal, the components are linked by O-H
O hydrogen bonds and aromatic ![[pi]](/logos/entities/pi_rmgif.gif)
- stacking interactions [minimum centroid-centroid separation = 3.537 (2) Å].
The solvothermal systhesis was carried out in telflon-lined stainless steel autoclave. A mixture of Cu(NO3)2.2H2O, phenantholine and succinic acid (mole ratio 1:1:1) in (H2O)/MeOH (2:1) was heated at 423 K for 72 h. Green slabs of (I) in a green solution were obtained.
All the H atoms were located in a difference map and their positions and Uiso(H) value were freely refined.
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
![[Figure 1]](./hb5112fig1thm.gif)
| Fig. 1. The molecular structure of (I), with 50% probability displacement ellipsoids for non-H atoms. |
| [Cu4(C4H4O4)2(C12H8N2)4(H2O)4](NO3)4·4H2O | Z = 2 |
| Mr = 1599.29 | F(000) = 1632 |
| Monoclinic, P21/c | Dx = 1.694 Mg m−3 |
| Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
| a = 8.9180 (1) Å | Cell parameters from 23295 reflections |
| b = 34.1090 (2) Å | µ = 1.44 mm−1 |
| c = 10.3620 (2) Å | T = 293 K |
| β = 96.031 (1)° | Slab, green |
| V = 3134.51 (7) Å3 | 0.20 × 0.19 × 0.10 mm |
| Bruker SMART 1K CCD diffractometer | 7772 reflections with I > 2σ(I) |
| Radiation source: fine-focus sealed tube | Rint = 0.018 |
| graphite | θmax = 30.5°, θmin = 1.2° |
| ω scans | h = −12→9 |
| 23089 measured reflections | k = −37→48 |
| 8980 independent reflections | l = −13→14 |
| Refinement on F2 | Primary atom site location: structure-invariant direct methods |
| Least-squares matrix: full | Secondary atom site location: difference Fourier map |
| R[F2 > 2σ(F2)] = 0.064 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.191 | H atoms treated by a mixture of independent and constrained refinement |
| S = 1.05 | w = 1/[σ2(Fo2) + (0.1023P)2 + 8.0138P] where P = (Fo2 + 2Fc2)/3 |
| 8980 reflections | (Δ/σ)max < 0.001 |
| 463 parameters | Δρmax = 2.88 e Å−3 |
| 101 restraints | Δρmin = −1.59 e Å−3 |
| [Cu4(C4H4O4)2(C12H8N2)4(H2O)4](NO3)4·4H2O | V = 3134.51 (7) Å3 |
| Mr = 1599.29 | Z = 2 |
| Monoclinic, P21/c | Mo Kα radiation |
| a = 8.9180 (1) Å | µ = 1.44 mm−1 |
| b = 34.1090 (2) Å | T = 293 K |
| c = 10.3620 (2) Å | 0.20 × 0.19 × 0.10 mm |
| β = 96.031 (1)° |
| Bruker SMART 1K CCD diffractometer | 7772 reflections with I > 2σ(I) |
| 23089 measured reflections | Rint = 0.018 |
| 8980 independent reflections | θmax = 30.5° |
| R[F2 > 2σ(F2)] = 0.064 | H atoms treated by a mixture of independent and constrained refinement |
| wR(F2) = 0.191 | Δρmax = 2.88 e Å−3 |
| S = 1.05 | Δρmin = −1.59 e Å−3 |
| 8980 reflections | Absolute structure: ? |
| 463 parameters | Flack parameter: ? |
| 101 restraints | Rogers parameter: ? |
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. |
| x | y | z | Uiso*/Ueq | ||
| Cu1 | 0.28697 (5) | 0.045902 (12) | 0.25937 (4) | 0.02773 (12) | |
| Cu2 | 0.45414 (5) | 0.092420 (12) | 0.07025 (4) | 0.02759 (12) | |
| O1 | 0.5954 (3) | 0.05491 (8) | 0.1565 (3) | 0.0403 (6) | |
| O2 | 0.4661 (3) | 0.01290 (8) | 0.2689 (3) | 0.0384 (6) | |
| O3 | 0.6118 (4) | 0.11127 (12) | −0.0618 (3) | 0.0431 (7) | |
| O4 | 0.1350 (5) | 0.01289 (11) | 0.3799 (4) | 0.0577 (9) | |
| O5 | 0.2091 (3) | 0.02148 (9) | 0.0939 (3) | 0.0366 (6) | |
| O6 | 0.3553 (4) | 0.05135 (8) | −0.0390 (3) | 0.0396 (6) | |
| O7 | −0.1911 (12) | 0.2391 (4) | 0.0691 (10) | 0.191 (2) | |
| O8 | −0.1382 (12) | 0.2708 (4) | 0.2187 (10) | 0.191 (2) | |
| O9 | −0.3494 (12) | 0.2700 (4) | 0.1619 (9) | 0.191 (2) | |
| O10 | −0.0018 (6) | 0.06202 (15) | 0.6390 (5) | 0.0804 (7) | |
| O11 | −0.1232 (6) | 0.11331 (15) | 0.5928 (5) | 0.0804 (7) | |
| O12 | −0.0996 (6) | 0.07141 (15) | 0.4439 (5) | 0.0804 (7) | |
| O13 | 0.8466 (5) | 0.06449 (13) | −0.1270 (4) | 0.0529 (8) | |
| O14 | 0.6181 (10) | 0.18964 (17) | −0.1023 (7) | 0.105 (2) | |
| N1 | 0.1424 (3) | 0.09146 (9) | 0.2426 (3) | 0.0281 (5) | |
| N2 | 0.3661 (3) | 0.07455 (9) | 0.4221 (3) | 0.0299 (6) | |
| N3 | 0.2987 (3) | 0.13232 (9) | −0.0008 (3) | 0.0313 (6) | |
| N4 | 0.5046 (3) | 0.13445 (8) | 0.2033 (3) | 0.0285 (5) | |
| N5 | −0.0754 (7) | 0.08168 (19) | 0.5574 (6) | 0.0804 (7) | |
| N6 | −0.2256 (16) | 0.2581 (4) | 0.1483 (12) | 0.191 (2) | |
| C1 | 0.0277 (4) | 0.09854 (12) | 0.1527 (4) | 0.0348 (7) | |
| H1 | 0.0070 | 0.0806 | 0.0856 | 0.042* | |
| C2 | −0.0628 (5) | 0.13195 (14) | 0.1556 (5) | 0.0442 (9) | |
| H2 | −0.1422 | 0.1359 | 0.0912 | 0.053* | |
| C3 | −0.0343 (5) | 0.15882 (13) | 0.2536 (5) | 0.0441 (9) | |
| H3 | −0.0919 | 0.1815 | 0.2547 | 0.053* | |
| C4 | 0.0829 (4) | 0.15163 (11) | 0.3524 (4) | 0.0357 (7) | |
| C5 | 0.1192 (6) | 0.17666 (13) | 0.4627 (5) | 0.0502 (11) | |
| H5 | 0.0631 | 0.1993 | 0.4711 | 0.060* | |
| C6 | 0.2326 (6) | 0.16796 (14) | 0.5539 (4) | 0.0524 (11) | |
| H6 | 0.2540 | 0.1849 | 0.6237 | 0.063* | |
| C7 | 0.3218 (5) | 0.13296 (12) | 0.5464 (4) | 0.0396 (8) | |
| C8 | 0.4391 (6) | 0.12140 (15) | 0.6398 (4) | 0.0508 (11) | |
| H8 | 0.4656 | 0.1369 | 0.7124 | 0.061* | |
| C9 | 0.5138 (6) | 0.08717 (15) | 0.6231 (4) | 0.0507 (11) | |
| H9 | 0.5903 | 0.0790 | 0.6852 | 0.061* | |
| C10 | 0.4754 (5) | 0.06441 (13) | 0.5126 (4) | 0.0404 (8) | |
| H10 | 0.5284 | 0.0413 | 0.5021 | 0.049* | |
| C11 | 0.2887 (4) | 0.10818 (11) | 0.4393 (3) | 0.0302 (6) | |
| C12 | 0.1680 (4) | 0.11755 (10) | 0.3420 (3) | 0.0287 (6) | |
| C13 | 0.1976 (5) | 0.12984 (14) | −0.1039 (4) | 0.0409 (8) | |
| H13 | 0.1950 | 0.1075 | −0.1555 | 0.049* | |
| C14 | 0.0944 (5) | 0.16024 (16) | −0.1369 (5) | 0.0503 (11) | |
| H14 | 0.0256 | 0.1580 | −0.2105 | 0.060* | |
| C15 | 0.0946 (5) | 0.19314 (14) | −0.0612 (5) | 0.0495 (10) | |
| H15 | 0.0250 | 0.2131 | −0.0818 | 0.059* | |
| C16 | 0.2019 (5) | 0.19638 (12) | 0.0489 (4) | 0.0401 (8) | |
| C17 | 0.2115 (6) | 0.22905 (12) | 0.1378 (5) | 0.0513 (11) | |
| H17 | 0.1425 | 0.2495 | 0.1242 | 0.062* | |
| C18 | 0.3176 (6) | 0.23065 (12) | 0.2398 (6) | 0.0529 (11) | |
| H18 | 0.3224 | 0.2524 | 0.2941 | 0.063* | |
| C19 | 0.4237 (5) | 0.19925 (11) | 0.2661 (4) | 0.0385 (8) | |
| C20 | 0.5367 (6) | 0.19841 (13) | 0.3722 (5) | 0.0478 (10) | |
| H20 | 0.5482 | 0.2194 | 0.4295 | 0.057* | |
| C21 | 0.6289 (5) | 0.16652 (14) | 0.3902 (4) | 0.0446 (9) | |
| H21 | 0.7046 | 0.1660 | 0.4591 | 0.053* | |
| C22 | 0.6097 (4) | 0.13465 (12) | 0.3049 (4) | 0.0346 (7) | |
| H22 | 0.6723 | 0.1129 | 0.3195 | 0.042* | |
| C23 | 0.4138 (4) | 0.16638 (10) | 0.1835 (4) | 0.0300 (6) | |
| C24 | 0.3028 (4) | 0.16508 (10) | 0.0740 (3) | 0.0303 (6) | |
| C25 | 0.5830 (4) | 0.02380 (10) | 0.2196 (3) | 0.0288 (6) | |
| C26 | 0.7229 (4) | −0.00119 (11) | 0.2433 (3) | 0.0307 (7) | |
| C27 | 0.2562 (4) | 0.02685 (10) | −0.0151 (3) | 0.0276 (6) | |
| C28 | 0.1862 (4) | 0.00277 (12) | −0.1284 (4) | 0.0319 (7) | |
| H13D | 0.865 (7) | 0.0669 (19) | −0.191 (7) | 0.054 (19)* | |
| H13C | 0.840 (8) | 0.042 (2) | −0.128 (7) | 0.07 (2)* | |
| H4 | 0.624 (7) | 0.132 (2) | −0.075 (6) | 0.055 (18)* | |
| H16 | 0.671 (7) | 0.0999 (18) | −0.081 (6) | 0.047 (16)* | |
| H24 | 0.101 (10) | −0.0089 (12) | 0.393 (9) | 0.11 (3)* | |
| H23 | 0.080 (6) | 0.0256 (17) | 0.422 (5) | 0.065 (19)* | |
| H28B | 0.173 (7) | −0.0210 (18) | −0.092 (6) | 0.057 (16)* | |
| H26B | 0.704 (7) | −0.0255 (19) | 0.270 (6) | 0.058 (16)* | |
| H26A | 0.773 (6) | 0.0080 (14) | 0.316 (5) | 0.039 (12)* | |
| H28A | 0.098 (7) | 0.0156 (19) | −0.140 (6) | 0.065 (18)* | |
| H14B | 0.669 (8) | 0.200 (2) | −0.155 (6) | 0.10 (3)* | |
| H14C | 0.679 (10) | 0.198 (3) | −0.044 (8) | 0.09 (3)* |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Cu1 | 0.0279 (2) | 0.0305 (2) | 0.0247 (2) | 0.00133 (15) | 0.00241 (15) | −0.00501 (15) |
| Cu2 | 0.0291 (2) | 0.0243 (2) | 0.0287 (2) | 0.00061 (14) | −0.00019 (15) | −0.00122 (14) |
| O1 | 0.0387 (14) | 0.0304 (13) | 0.0505 (16) | 0.0070 (11) | −0.0019 (12) | 0.0056 (11) |
| O2 | 0.0359 (13) | 0.0400 (14) | 0.0402 (14) | 0.0100 (11) | 0.0079 (11) | 0.0007 (11) |
| O3 | 0.0407 (16) | 0.0469 (19) | 0.0435 (16) | 0.0031 (14) | 0.0136 (13) | 0.0056 (14) |
| O4 | 0.072 (2) | 0.0434 (18) | 0.063 (2) | −0.0140 (17) | 0.0327 (19) | −0.0013 (16) |
| O5 | 0.0366 (13) | 0.0438 (15) | 0.0298 (12) | −0.0025 (11) | 0.0053 (10) | −0.0122 (11) |
| O6 | 0.0477 (16) | 0.0338 (13) | 0.0368 (14) | −0.0110 (11) | 0.0018 (12) | −0.0077 (11) |
| O7 | 0.146 (4) | 0.276 (7) | 0.139 (4) | 0.073 (4) | −0.043 (3) | −0.078 (4) |
| O8 | 0.146 (4) | 0.276 (7) | 0.139 (4) | 0.073 (4) | −0.043 (3) | −0.078 (4) |
| O9 | 0.146 (4) | 0.276 (7) | 0.139 (4) | 0.073 (4) | −0.043 (3) | −0.078 (4) |
| O10 | 0.0886 (18) | 0.0729 (15) | 0.0775 (16) | 0.0048 (13) | −0.0016 (13) | −0.0012 (13) |
| O11 | 0.0886 (18) | 0.0729 (15) | 0.0775 (16) | 0.0048 (13) | −0.0016 (13) | −0.0012 (13) |
| O12 | 0.0886 (18) | 0.0729 (15) | 0.0775 (16) | 0.0048 (13) | −0.0016 (13) | −0.0012 (13) |
| O13 | 0.062 (2) | 0.051 (2) | 0.048 (2) | 0.0071 (17) | 0.0155 (17) | −0.0016 (16) |
| O14 | 0.169 (7) | 0.059 (3) | 0.089 (4) | −0.035 (4) | 0.023 (5) | 0.007 (3) |
| N1 | 0.0273 (13) | 0.0322 (14) | 0.0246 (12) | −0.0023 (10) | 0.0023 (10) | −0.0017 (10) |
| N2 | 0.0325 (14) | 0.0333 (14) | 0.0235 (12) | −0.0018 (11) | 0.0004 (11) | −0.0009 (11) |
| N3 | 0.0293 (14) | 0.0331 (14) | 0.0307 (14) | 0.0010 (11) | −0.0004 (11) | 0.0028 (11) |
| N4 | 0.0275 (13) | 0.0258 (13) | 0.0316 (14) | 0.0000 (10) | 0.0008 (11) | −0.0001 (10) |
| N5 | 0.0886 (18) | 0.0729 (15) | 0.0775 (16) | 0.0048 (13) | −0.0016 (13) | −0.0012 (13) |
| N6 | 0.146 (4) | 0.276 (7) | 0.139 (4) | 0.073 (4) | −0.043 (3) | −0.078 (4) |
| C1 | 0.0276 (16) | 0.0421 (19) | 0.0333 (17) | −0.0040 (14) | −0.0037 (13) | −0.0033 (14) |
| C2 | 0.0297 (18) | 0.053 (2) | 0.048 (2) | 0.0044 (16) | −0.0056 (16) | 0.0041 (19) |
| C3 | 0.0336 (18) | 0.038 (2) | 0.060 (3) | 0.0081 (15) | 0.0050 (17) | 0.0029 (18) |
| C4 | 0.0380 (18) | 0.0296 (16) | 0.0399 (19) | 0.0033 (14) | 0.0060 (15) | −0.0033 (14) |
| C5 | 0.064 (3) | 0.0328 (19) | 0.055 (3) | 0.0055 (19) | 0.010 (2) | −0.0127 (18) |
| C6 | 0.076 (3) | 0.041 (2) | 0.040 (2) | 0.001 (2) | 0.004 (2) | −0.0183 (18) |
| C7 | 0.052 (2) | 0.0382 (19) | 0.0274 (16) | −0.0061 (16) | 0.0000 (15) | −0.0065 (14) |
| C8 | 0.067 (3) | 0.055 (3) | 0.0281 (18) | −0.009 (2) | −0.0080 (18) | −0.0079 (17) |
| C9 | 0.057 (3) | 0.060 (3) | 0.0311 (19) | −0.001 (2) | −0.0140 (18) | 0.0008 (18) |
| C10 | 0.044 (2) | 0.045 (2) | 0.0307 (17) | 0.0021 (16) | −0.0045 (15) | 0.0051 (15) |
| C11 | 0.0355 (17) | 0.0324 (16) | 0.0225 (14) | −0.0036 (13) | 0.0025 (12) | −0.0024 (12) |
| C12 | 0.0289 (15) | 0.0295 (15) | 0.0279 (15) | −0.0003 (12) | 0.0043 (12) | −0.0034 (12) |
| C13 | 0.0392 (19) | 0.051 (2) | 0.0314 (17) | 0.0005 (17) | −0.0034 (15) | 0.0014 (16) |
| C14 | 0.043 (2) | 0.065 (3) | 0.040 (2) | 0.004 (2) | −0.0099 (17) | 0.010 (2) |
| C15 | 0.044 (2) | 0.048 (2) | 0.054 (3) | 0.0117 (19) | −0.0056 (19) | 0.015 (2) |
| C16 | 0.0401 (19) | 0.0319 (18) | 0.048 (2) | 0.0054 (15) | 0.0032 (16) | 0.0113 (16) |
| C17 | 0.056 (3) | 0.0281 (18) | 0.068 (3) | 0.0121 (17) | 0.001 (2) | 0.0058 (19) |
| C18 | 0.062 (3) | 0.0242 (17) | 0.072 (3) | 0.0041 (17) | 0.004 (2) | −0.0074 (19) |
| C19 | 0.042 (2) | 0.0251 (16) | 0.048 (2) | −0.0041 (14) | 0.0037 (16) | −0.0028 (15) |
| C20 | 0.053 (2) | 0.040 (2) | 0.049 (2) | −0.0090 (18) | −0.0010 (19) | −0.0123 (18) |
| C21 | 0.041 (2) | 0.050 (2) | 0.040 (2) | −0.0082 (17) | −0.0066 (16) | −0.0077 (17) |
| C22 | 0.0298 (16) | 0.0386 (18) | 0.0343 (17) | −0.0006 (13) | −0.0018 (13) | 0.0008 (14) |
| C23 | 0.0308 (16) | 0.0243 (14) | 0.0346 (16) | −0.0019 (12) | 0.0018 (13) | 0.0015 (12) |
| C24 | 0.0302 (15) | 0.0274 (15) | 0.0335 (16) | 0.0011 (12) | 0.0044 (13) | 0.0052 (12) |
| C25 | 0.0325 (16) | 0.0280 (15) | 0.0248 (14) | 0.0066 (12) | −0.0026 (12) | −0.0060 (11) |
| C26 | 0.0326 (16) | 0.0332 (17) | 0.0250 (15) | 0.0076 (13) | −0.0036 (12) | −0.0022 (13) |
| C27 | 0.0254 (14) | 0.0275 (15) | 0.0287 (15) | 0.0053 (11) | −0.0021 (11) | −0.0070 (12) |
| C28 | 0.0272 (15) | 0.0353 (17) | 0.0320 (16) | 0.0006 (13) | −0.0024 (12) | −0.0101 (14) |
| Cu1—O2 | 1.948 (3) | C4—C12 | 1.398 (5) |
| Cu1—O5 | 1.966 (3) | C4—C5 | 1.437 (6) |
| Cu1—N2 | 2.011 (3) | C5—C6 | 1.342 (7) |
| Cu1—N1 | 2.015 (3) | C5—H5 | 0.9300 |
| Cu1—O4 | 2.240 (3) | C6—C7 | 1.441 (6) |
| Cu1—Cu2 | 3.0322 (6) | C6—H6 | 0.9300 |
| Cu2—O1 | 1.946 (3) | C7—C11 | 1.401 (5) |
| Cu2—O6 | 1.952 (3) | C7—C8 | 1.405 (6) |
| Cu2—N4 | 2.007 (3) | C8—C9 | 1.364 (7) |
| Cu2—N3 | 2.025 (3) | C8—H8 | 0.9300 |
| Cu2—O3 | 2.160 (3) | C9—C10 | 1.396 (6) |
| O1—C25 | 1.258 (5) | C9—H9 | 0.9300 |
| O2—C25 | 1.264 (5) | C10—H10 | 0.9300 |
| O3—H4 | 0.73 (7) | C11—C12 | 1.432 (5) |
| O3—H16 | 0.70 (6) | C13—C14 | 1.405 (6) |
| O4—H24 | 0.82 (5) | C13—H13 | 0.9300 |
| O4—H23 | 0.82 (6) | C14—C15 | 1.369 (7) |
| O5—C27 | 1.259 (4) | C14—H14 | 0.9300 |
| O6—C27 | 1.260 (5) | C15—C16 | 1.415 (6) |
| O7—N6 | 1.114 (14) | C15—H15 | 0.9300 |
| O8—N6 | 1.099 (14) | C16—C24 | 1.403 (5) |
| O9—N6 | 1.199 (14) | C16—C17 | 1.443 (7) |
| O10—N5 | 1.216 (8) | C17—C18 | 1.344 (7) |
| O11—N5 | 1.231 (8) | C17—H17 | 0.9300 |
| O12—N5 | 1.224 (8) | C18—C19 | 1.436 (6) |
| O13—H13D | 0.70 (7) | C18—H18 | 0.9300 |
| O13—H13C | 0.75 (8) | C19—C23 | 1.407 (5) |
| O14—H14B | 0.83 (7) | C19—C20 | 1.411 (6) |
| O14—H14C | 0.82 (8) | C20—C21 | 1.364 (7) |
| N1—C1 | 1.331 (4) | C20—H20 | 0.9300 |
| N1—C12 | 1.362 (4) | C21—C22 | 1.400 (6) |
| N2—C10 | 1.326 (5) | C21—H21 | 0.9300 |
| N2—C11 | 1.360 (5) | C22—H22 | 0.9300 |
| N3—C13 | 1.327 (5) | C23—C24 | 1.426 (5) |
| N3—C24 | 1.358 (5) | C25—C26 | 1.510 (5) |
| N4—C22 | 1.334 (5) | C26—C28i | 1.510 (5) |
| N4—C23 | 1.359 (4) | C26—H26B | 0.90 (6) |
| C1—C2 | 1.399 (6) | C26—H26A | 0.89 (5) |
| C1—H1 | 0.9300 | C27—C28 | 1.513 (4) |
| C2—C3 | 1.371 (7) | C28—C26i | 1.510 (5) |
| C2—H2 | 0.9300 | C28—H28B | 0.91 (6) |
| C3—C4 | 1.406 (6) | C28—H28A | 0.90 (7) |
| C3—H3 | 0.9300 | ||
| O2—Cu1—O5 | 90.69 (12) | C5—C6—C7 | 121.6 (4) |
| O2—Cu1—N2 | 91.42 (12) | C5—C6—H6 | 119.2 |
| O5—Cu1—N2 | 175.95 (12) | C7—C6—H6 | 119.2 |
| O2—Cu1—N1 | 164.53 (12) | C11—C7—C8 | 117.1 (4) |
| O5—Cu1—N1 | 95.00 (12) | C11—C7—C6 | 118.1 (4) |
| N2—Cu1—N1 | 82.10 (12) | C8—C7—C6 | 124.8 (4) |
| O2—Cu1—O4 | 102.84 (14) | C9—C8—C7 | 119.4 (4) |
| O5—Cu1—O4 | 95.40 (14) | C9—C8—H8 | 120.3 |
| N2—Cu1—O4 | 87.49 (14) | C7—C8—H8 | 120.3 |
| N1—Cu1—O4 | 90.95 (14) | C8—C9—C10 | 120.0 (4) |
| O2—Cu1—Cu2 | 83.04 (9) | C8—C9—H9 | 120.0 |
| O5—Cu1—Cu2 | 79.10 (9) | C10—C9—H9 | 120.0 |
| N2—Cu1—Cu2 | 97.73 (9) | N2—C10—C9 | 122.3 (4) |
| N1—Cu1—Cu2 | 83.93 (8) | N2—C10—H10 | 118.9 |
| O4—Cu1—Cu2 | 172.09 (12) | C9—C10—H10 | 118.9 |
| O1—Cu2—O6 | 91.46 (13) | N2—C11—C7 | 123.0 (3) |
| O1—Cu2—N4 | 93.81 (12) | N2—C11—C12 | 116.7 (3) |
| O6—Cu2—N4 | 164.98 (13) | C7—C11—C12 | 120.2 (3) |
| O1—Cu2—N3 | 173.84 (13) | N1—C12—C4 | 123.5 (3) |
| O6—Cu2—N3 | 91.23 (13) | N1—C12—C11 | 116.2 (3) |
| N4—Cu2—N3 | 82.25 (12) | C4—C12—C11 | 120.3 (3) |
| O1—Cu2—O3 | 93.07 (14) | N3—C13—C14 | 121.4 (4) |
| O6—Cu2—O3 | 97.50 (14) | N3—C13—H13 | 119.3 |
| N4—Cu2—O3 | 96.25 (14) | C14—C13—H13 | 119.3 |
| N3—Cu2—O3 | 92.07 (14) | C15—C14—C13 | 120.3 (4) |
| O1—Cu2—Cu1 | 72.40 (9) | C15—C14—H14 | 119.9 |
| O6—Cu2—Cu1 | 77.09 (9) | C13—C14—H14 | 119.9 |
| N4—Cu2—Cu1 | 91.12 (9) | C14—C15—C16 | 119.1 (4) |
| N3—Cu2—Cu1 | 102.83 (9) | C14—C15—H15 | 120.5 |
| O3—Cu2—Cu1 | 164.16 (11) | C16—C15—H15 | 120.5 |
| C25—O1—Cu2 | 134.9 (3) | C24—C16—C15 | 117.2 (4) |
| C25—O2—Cu1 | 121.1 (2) | C24—C16—C17 | 118.4 (4) |
| Cu2—O3—H4 | 122 (5) | C15—C16—C17 | 124.4 (4) |
| Cu2—O3—H16 | 125 (5) | C18—C17—C16 | 121.5 (4) |
| H4—O3—H16 | 110 (7) | C18—C17—H17 | 119.2 |
| Cu1—O4—H24 | 144 (7) | C16—C17—H17 | 119.2 |
| Cu1—O4—H23 | 118 (5) | C17—C18—C19 | 121.0 (4) |
| H24—O4—H23 | 98 (7) | C17—C18—H18 | 119.5 |
| C27—O5—Cu1 | 126.8 (2) | C19—C18—H18 | 119.5 |
| C27—O6—Cu2 | 130.2 (2) | C23—C19—C20 | 116.8 (4) |
| H13D—O13—H13C | 97 (7) | C23—C19—C18 | 118.7 (4) |
| H14B—O14—H14C | 88 (8) | C20—C19—C18 | 124.4 (4) |
| C1—N1—C12 | 117.8 (3) | C21—C20—C19 | 119.6 (4) |
| C1—N1—Cu1 | 129.7 (3) | C21—C20—H20 | 120.2 |
| C12—N1—Cu1 | 112.5 (2) | C19—C20—H20 | 120.2 |
| C10—N2—C11 | 118.2 (3) | C20—C21—C22 | 120.0 (4) |
| C10—N2—Cu1 | 129.3 (3) | C20—C21—H21 | 120.0 |
| C11—N2—Cu1 | 112.4 (2) | C22—C21—H21 | 120.0 |
| C13—N3—C24 | 119.2 (3) | N4—C22—C21 | 122.1 (4) |
| C13—N3—Cu2 | 129.1 (3) | N4—C22—H22 | 119.0 |
| C24—N3—Cu2 | 111.7 (2) | C21—C22—H22 | 119.0 |
| C22—N4—C23 | 118.2 (3) | N4—C23—C19 | 123.3 (3) |
| C22—N4—Cu2 | 129.3 (3) | N4—C23—C24 | 116.6 (3) |
| C23—N4—Cu2 | 112.4 (2) | C19—C23—C24 | 120.1 (3) |
| O10—N5—O12 | 122.5 (7) | N3—C24—C16 | 122.8 (3) |
| O10—N5—O11 | 117.0 (6) | N3—C24—C23 | 117.0 (3) |
| O12—N5—O11 | 120.4 (6) | C16—C24—C23 | 120.1 (3) |
| O8—N6—O7 | 119.1 (16) | O1—C25—O2 | 125.4 (3) |
| O8—N6—O9 | 112.7 (14) | O1—C25—C26 | 116.4 (3) |
| O7—N6—O9 | 127.8 (14) | O2—C25—C26 | 118.1 (3) |
| N1—C1—C2 | 122.4 (4) | C25—C26—C28i | 113.2 (3) |
| N1—C1—H1 | 118.8 | C25—C26—H26B | 113 (4) |
| C2—C1—H1 | 118.8 | C28i—C26—H26B | 110 (4) |
| C3—C2—C1 | 119.9 (4) | C25—C26—H26A | 106 (3) |
| C3—C2—H2 | 120.1 | C28i—C26—H26A | 114 (3) |
| C1—C2—H2 | 120.1 | H26B—C26—H26A | 99 (5) |
| C2—C3—C4 | 119.2 (4) | O5—C27—O6 | 125.5 (3) |
| C2—C3—H3 | 120.4 | O5—C27—C28 | 117.9 (3) |
| C4—C3—H3 | 120.4 | O6—C27—C28 | 116.6 (3) |
| C12—C4—C3 | 117.2 (4) | C26i—C28—C27 | 114.8 (3) |
| C12—C4—C5 | 118.5 (4) | C26i—C28—H28B | 114 (4) |
| C3—C4—C5 | 124.3 (4) | C27—C28—H28B | 103 (4) |
| C6—C5—C4 | 121.3 (4) | C26i—C28—H28A | 116 (4) |
| C6—C5—H5 | 119.4 | C27—C28—H28A | 97 (4) |
| C4—C5—H5 | 119.4 | H28B—C28—H28A | 110 (5) |
| Symmetry codes: (i) −x+1, −y, −z. |
| D—H···A | D—H | H···A | D···A | D—H···A |
| O3—H4···O14 | 0.73 (7) | 1.99 (7) | 2.707 (7) | 169 (7) |
| O3—H16···O13 | 0.70 (6) | 2.07 (6) | 2.772 (6) | 177 (9) |
| O4—H23···O12 | 0.82 (6) | 2.27 (6) | 3.015 (7) | 153 (5) |
| O4—H24···O10ii | 0.82 (5) | 2.03 (6) | 2.816 (6) | 161 (8) |
| O13—H13C···O5i | 0.77 (7) | 2.24 (7) | 3.000 (5) | 167 (7) |
| O13—H13D···O10iii | 0.71 (7) | 2.23 (7) | 2.899 (7) | 159 (8) |
| O14—H14B···O9iv | 0.83 (7) | 2.15 (6) | 2.846 (13) | 142 (6) |
| O14—H14C···O7v | 0.82 (9) | 2.10 (9) | 2.874 (14) | 158 (10) |
| Symmetry codes: (ii) −x, −y, −z+1; (i) −x+1, −y, −z; (iii) x+1, y, z−1; (iv) x+1, −y+1/2, z−1/2; (v) x+1, y, z. |
| Cu1—O2 | 1.948 (3) | Cu2—O1 | 1.946 (3) |
| Cu1—O5 | 1.966 (3) | Cu2—O6 | 1.952 (3) |
| Cu1—N2 | 2.011 (3) | Cu2—N4 | 2.007 (3) |
| Cu1—N1 | 2.015 (3) | Cu2—N3 | 2.025 (3) |
| Cu1—O4 | 2.240 (3) | Cu2—O3 | 2.160 (3) |
| D—H···A | D—H | H···A | D···A | D—H···A |
| O3—H4···O14 | 0.73 (7) | 1.99 (7) | 2.707 (7) | 169 (7) |
| O3—H16···O13 | 0.70 (6) | 2.07 (6) | 2.772 (6) | 177 (9) |
| O4—H23···O12 | 0.82 (6) | 2.27 (6) | 3.015 (7) | 153 (5) |
| O4—H24···O10i | 0.82 (5) | 2.03 (6) | 2.816 (6) | 161 (8) |
| O13—H13C···O5ii | 0.77 (7) | 2.24 (7) | 3.000 (5) | 167 (7) |
| O13—H13D···O10iii | 0.71 (7) | 2.23 (7) | 2.899 (7) | 159 (8) |
| O14—H14B···O9iv | 0.83 (7) | 2.15 (6) | 2.846 (13) | 142 (6) |
| O14—H14C···O7v | 0.82 (9) | 2.10 (9) | 2.874 (14) | 158 (10) |
| Symmetry codes: (i) −x, −y, −z+1; (ii) −x+1, −y, −z; (iii) x+1, y, z−1; (iv) x+1, −y+1/2, z−1/2; (v) x+1, y, z. |
The authors thank the Royal Golden Jubilee PhD Program (RGJ) for financial support.
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McCann, S., McCann, M., Casey, R. M. T., Jackman, M., Devereux, M., McKee, V.,
& (1998). Inorg. Chim. Acta, 279, 24–29.
Padmanabhan, M., Kumary, S. M., Huang, X. & Li, J. (2005). Inorg. Chim. Acta, 358, 3537–3544.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.
The moleculular structure of the title compound, (I), consists of a tetranuclear [Cu4(phen)4(suc)2(H2O)4].4+ species and uncoordinated water molecules and nitrate anions. Each Cu(II) ion (Table 1) exhibits a distorted square pyramidal coordination geometry through one apical water oxygen atom, two phen N atoms and two carboxylate O atoms from two succinate dianions which act as bis bridging ligands toward the Cu1 and Cu2 atoms (Fig. 1). The Cu1···Cu2 distance is 3.0318 (4) Å. The succinate ions also bridge two Cu(II) ions (Cu1' and Cu2'). The Cu1 and Cu2' distance separated by the bridging succinate anion is 6.396 Å. The face-to-face π-π interactions between the phenanthroline ring enhance the stability of the structure.
The apical water molecules form hydrogen bonds with nitrate O atoms (O···O distances of 2.810–2.920 Å) and uncoordinated water O atoms (O···O distances of 2.709–2.768Å): Table 2.