metal-organic compounds
In the centrosymmetric title compound, [Cu2(C8H4O4)Cl2(C12H8N2)2(H2O)2], each Cu atom is surrounded by an O atom from a terephthalate dianion, a water molecule, a Cl atom and the N atoms from a 1,10-phenanthroline heterocycle in an octahedral arrangement. The terephthalate dianion, which functions as a bridge between two Cu atoms, lies on a special position of site symmetry.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804002107/cf6325sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804002107/cf6325Isup2.hkl |
CCDC reference: 236015
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean (C-C) = 0.004 Å
- R factor = 0.029
- wR factor = 0.076
- Data-to-parameter ratio = 12.5
checkCIF/PLATON results
No syntax errors found No errors found in this datablock
Computing details top
Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
µ-Terephthalato-bis[aquachloro(1,10-phenanthroline)copper(II)] top
Crystal data top
[Cu2(C8H4O4)Cl2(C12H8N2)2(H2O)2] | Z = 1 |
Mr = 758.55 | F(000) = 384 |
Triclinic, P1 | Dx = 1.710 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.6846 (10) Å | Cell parameters from 678 reflections |
b = 9.7645 (11) Å | θ = 2.4–22.0° |
c = 10.4676 (12) Å | µ = 1.68 mm−1 |
α = 63.154 (2)° | T = 273 K |
β = 68.579 (2)° | Prism, green |
γ = 78.644 (2)° | 0.40 × 0.31 × 0.28 mm |
V = 736.74 (15) Å3 |
Data collection top
Bruker APEX area-detector diffractometer | 2628 independent reflections |
Radiation source: fine-focus sealed tube | 2458 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.014 |
φ and ω scans | θmax = 25.2°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −10→10 |
Tmin = 0.545, Tmax = 0.632 | k = −11→11 |
5423 measured reflections | l = −12→12 |
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)] = 0.029 | H-atom parameters constrained |
wR(F2) = 0.076 | w = 1/[σ2(Fo2) + (0.043P)2 + 0.2928P] where P = (Fo2 + 2Fc2)/3 |
S = 1.09 | (Δ/σ)max = 0.001 |
2628 reflections | Δρmax = 0.32 e Å−3 |
210 parameters | Δρmin = −0.29 e Å−3 |
0 restraints | Extinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0009 (2) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Cu1 | 0.43734 (3) | 0.71383 (3) | 0.11959 (3) | 0.03259 (12) | |
Cl1 | 0.55379 (7) | 0.44824 (7) | 0.22996 (6) | 0.03937 (16) | |
O1 | 0.62490 (19) | 0.8257 (2) | 0.07777 (19) | 0.0417 (4) | |
O2 | 0.8032 (2) | 0.8133 (2) | −0.1341 (2) | 0.0481 (5) | |
O3 | 0.50599 (19) | 0.75379 (19) | −0.09812 (17) | 0.0411 (4) | |
H3B | 0.4859 | 0.6794 | −0.1052 | 0.062* | |
H3 | 0.6033 | 0.7769 | −0.1386 | 0.062* | |
N1 | 0.3192 (2) | 0.7729 (2) | 0.2951 (2) | 0.0340 (4) | |
N2 | 0.2099 (2) | 0.6428 (2) | 0.1731 (2) | 0.0300 (4) | |
C1 | 0.3807 (3) | 0.8296 (3) | 0.3590 (3) | 0.0432 (6) | |
H1 | 0.4934 | 0.8470 | 0.3216 | 0.052* | |
C2 | 0.2821 (3) | 0.8641 (3) | 0.4806 (3) | 0.0471 (6) | |
H2 | 0.3296 | 0.9026 | 0.5237 | 0.057* | |
C3 | 0.1168 (3) | 0.8416 (3) | 0.5364 (3) | 0.0416 (6) | |
H3A | 0.0505 | 0.8650 | 0.6171 | 0.050* | |
C4 | 0.0473 (3) | 0.7824 (2) | 0.4702 (2) | 0.0351 (5) | |
C5 | −0.1244 (3) | 0.7483 (3) | 0.5230 (3) | 0.0412 (6) | |
H5 | −0.1980 | 0.7731 | 0.6006 | 0.049* | |
C6 | −0.1802 (3) | 0.6808 (3) | 0.4614 (3) | 0.0402 (5) | |
H6 | −0.2918 | 0.6598 | 0.4975 | 0.048* | |
C7 | −0.0708 (3) | 0.6408 (2) | 0.3414 (2) | 0.0325 (5) | |
C8 | −0.1192 (3) | 0.5628 (3) | 0.2790 (3) | 0.0381 (5) | |
H8 | −0.2290 | 0.5380 | 0.3113 | 0.046* | |
C9 | −0.0032 (3) | 0.5239 (3) | 0.1702 (3) | 0.0392 (5) | |
H9 | −0.0334 | 0.4692 | 0.1303 | 0.047* | |
C10 | 0.1603 (3) | 0.5655 (3) | 0.1187 (3) | 0.0359 (5) | |
H10 | 0.2372 | 0.5385 | 0.0439 | 0.043* | |
C11 | 0.0956 (3) | 0.6770 (2) | 0.2853 (2) | 0.0281 (4) | |
C12 | 0.1550 (3) | 0.7483 (2) | 0.3511 (2) | 0.0296 (4) | |
C13 | 0.7632 (3) | 0.8495 (2) | −0.0261 (2) | 0.0324 (5) | |
C14 | 0.8857 (3) | 0.9282 (2) | −0.0130 (2) | 0.0295 (4) | |
C15 | 0.8351 (3) | 1.0011 (2) | 0.0840 (2) | 0.0325 (5) | |
H15 | 0.7242 | 1.0022 | 0.1407 | 0.039* | |
C16 | 1.0519 (3) | 0.9279 (2) | −0.0968 (2) | 0.0328 (5) | |
H16 | 1.0874 | 0.8796 | −0.1621 | 0.039* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.02356 (17) | 0.04665 (19) | 0.03506 (18) | −0.01165 (11) | −0.00056 (11) | −0.02593 (14) |
Cl1 | 0.0326 (3) | 0.0498 (3) | 0.0447 (3) | −0.0055 (2) | −0.0096 (2) | −0.0276 (3) |
O1 | 0.0287 (8) | 0.0611 (10) | 0.0458 (9) | −0.0197 (7) | 0.0023 (7) | −0.0348 (8) |
O2 | 0.0338 (9) | 0.0768 (12) | 0.0499 (10) | −0.0201 (8) | 0.0012 (8) | −0.0440 (10) |
O3 | 0.0345 (9) | 0.0584 (10) | 0.0393 (9) | −0.0166 (7) | −0.0026 (7) | −0.0290 (8) |
N1 | 0.0299 (10) | 0.0423 (10) | 0.0347 (10) | −0.0081 (8) | −0.0039 (8) | −0.0223 (8) |
N2 | 0.0261 (9) | 0.0364 (9) | 0.0299 (9) | −0.0072 (7) | −0.0047 (7) | −0.0166 (8) |
C1 | 0.0395 (13) | 0.0563 (15) | 0.0445 (13) | −0.0128 (11) | −0.0092 (11) | −0.0287 (12) |
C2 | 0.0558 (16) | 0.0542 (15) | 0.0455 (14) | −0.0073 (12) | −0.0158 (12) | −0.0307 (12) |
C3 | 0.0513 (15) | 0.0433 (13) | 0.0327 (12) | −0.0010 (11) | −0.0080 (11) | −0.0223 (10) |
C4 | 0.0385 (12) | 0.0330 (11) | 0.0301 (11) | −0.0001 (9) | −0.0066 (9) | −0.0139 (9) |
C5 | 0.0346 (13) | 0.0469 (13) | 0.0325 (12) | 0.0014 (10) | 0.0010 (10) | −0.0186 (10) |
C6 | 0.0244 (11) | 0.0462 (13) | 0.0379 (12) | −0.0023 (10) | −0.0005 (9) | −0.0140 (11) |
C7 | 0.0268 (11) | 0.0340 (11) | 0.0306 (11) | −0.0039 (8) | −0.0079 (9) | −0.0081 (9) |
C8 | 0.0283 (11) | 0.0437 (13) | 0.0386 (12) | −0.0119 (10) | −0.0100 (10) | −0.0103 (10) |
C9 | 0.0423 (13) | 0.0448 (13) | 0.0369 (12) | −0.0158 (10) | −0.0135 (10) | −0.0158 (10) |
C10 | 0.0374 (12) | 0.0421 (12) | 0.0332 (11) | −0.0099 (10) | −0.0066 (10) | −0.0199 (10) |
C11 | 0.0267 (10) | 0.0289 (10) | 0.0266 (10) | −0.0033 (8) | −0.0060 (8) | −0.0106 (8) |
C12 | 0.0293 (11) | 0.0308 (11) | 0.0279 (10) | −0.0039 (8) | −0.0055 (9) | −0.0130 (9) |
C13 | 0.0276 (11) | 0.0369 (11) | 0.0358 (12) | −0.0081 (9) | −0.0059 (9) | −0.0181 (10) |
C14 | 0.0278 (11) | 0.0310 (11) | 0.0310 (11) | −0.0069 (8) | −0.0071 (9) | −0.0134 (9) |
C15 | 0.0237 (10) | 0.0388 (12) | 0.0359 (11) | −0.0072 (9) | −0.0019 (9) | −0.0199 (10) |
C16 | 0.0306 (11) | 0.0370 (11) | 0.0353 (11) | −0.0078 (9) | −0.0045 (9) | −0.0208 (10) |
Geometric parameters (Å, º) top
Cu1—N1 | 2.0267 (18) | C4—C5 | 1.437 (3) |
Cu1—N2 | 2.0187 (17) | C5—C6 | 1.350 (3) |
Cu1—O1 | 1.9455 (15) | C5—H5 | 0.930 |
Cu1—O3 | 1.9992 (15) | C6—C7 | 1.435 (3) |
Cu1—Cl1 | 2.4895 (7) | C6—H6 | 0.930 |
O1—C13 | 1.268 (3) | C7—C11 | 1.397 (3) |
O2—C13 | 1.245 (3) | C7—C8 | 1.400 (3) |
O3—H3B | 0.820 | C8—C9 | 1.363 (3) |
O3—H3 | 0.820 | C8—H8 | 0.930 |
N1—C1 | 1.324 (3) | C9—C10 | 1.394 (3) |
N1—C12 | 1.354 (3) | C9—H9 | 0.930 |
N2—C10 | 1.333 (3) | C10—H10 | 0.930 |
N2—C11 | 1.359 (3) | C11—C12 | 1.434 (3) |
C1—C2 | 1.394 (4) | C13—C14 | 1.505 (3) |
C1—H1 | 0.930 | C14—C16 | 1.389 (3) |
C2—C3 | 1.359 (4) | C14—C15 | 1.390 (3) |
C2—H2 | 0.930 | C15—C16i | 1.382 (3) |
C3—C4 | 1.409 (3) | C15—H15 | 0.930 |
C3—H3A | 0.930 | C16—C15i | 1.382 (3) |
C4—C12 | 1.393 (3) | C16—H16 | 0.930 |
N1—Cu1—N2 | 81.46 (7) | C4—C5—H5 | 119.5 |
N1—Cu1—O1 | 87.57 (7) | C5—C6—C7 | 121.3 (2) |
N1—Cu1—O3 | 152.70 (8) | C5—C6—H6 | 119.4 |
N1—Cu1—Cl1 | 105.83 (6) | C7—C6—H6 | 119.4 |
N2—Cu1—O1 | 165.59 (7) | C11—C7—C8 | 117.2 (2) |
N2—Cu1—O3 | 95.41 (7) | C11—C7—C6 | 118.8 (2) |
N2—Cu1—Cl1 | 93.72 (5) | C8—C7—C6 | 123.9 (2) |
O1—Cu1—O3 | 90.06 (7) | C9—C8—C7 | 119.1 (2) |
O1—Cu1—Cl1 | 98.27 (6) | C9—C8—H8 | 120.4 |
O3—Cu1—Cl1 | 101.43 (5) | C7—C8—H8 | 120.4 |
C13—O1—Cu1 | 130.41 (14) | C8—C9—C10 | 120.3 (2) |
Cu1—O3—H3B | 109.5 | C8—C9—H9 | 119.9 |
Cu1—O3—H3 | 109.5 | C10—C9—H9 | 119.9 |
H3B—O3—H3 | 114.0 | N2—C10—C9 | 122.2 (2) |
C1—N1—C12 | 118.11 (19) | N2—C10—H10 | 118.9 |
C1—N1—Cu1 | 129.07 (16) | C9—C10—H10 | 118.9 |
C12—N1—Cu1 | 112.83 (14) | N2—C11—C7 | 123.54 (19) |
C10—N2—C11 | 117.55 (18) | N2—C11—C12 | 116.53 (18) |
C10—N2—Cu1 | 129.69 (15) | C7—C11—C12 | 119.88 (19) |
C11—N2—Cu1 | 112.72 (13) | N1—C12—C4 | 123.4 (2) |
N1—C1—C2 | 122.1 (2) | N1—C12—C11 | 116.22 (18) |
N1—C1—H1 | 118.9 | C4—C12—C11 | 120.30 (19) |
C2—C1—H1 | 118.9 | O2—C13—O1 | 125.5 (2) |
C3—C2—C1 | 120.2 (2) | O2—C13—C14 | 119.27 (19) |
C3—C2—H2 | 119.9 | O1—C13—C14 | 115.20 (19) |
C1—C2—H2 | 119.9 | C16—C14—C15 | 118.85 (19) |
C2—C3—C4 | 119.0 (2) | C16—C14—C13 | 120.36 (19) |
C2—C3—H3A | 120.5 | C15—C14—C13 | 120.78 (19) |
C4—C3—H3A | 120.5 | C16i—C15—C14 | 120.7 (2) |
C12—C4—C3 | 117.1 (2) | C16i—C15—H15 | 119.7 |
C12—C4—C5 | 118.8 (2) | C14—C15—H15 | 119.7 |
C3—C4—C5 | 124.1 (2) | C15i—C16—C14 | 120.5 (2) |
C6—C5—C4 | 120.9 (2) | C15i—C16—H16 | 119.8 |
C6—C5—H5 | 119.5 | C14—C16—H16 | 119.8 |
Symmetry code: (i) −x+2, −y+2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3···O2 | 0.82 | 1.86 | 2.612 (2) | 152 |
O3—H3B···Cl1ii | 0.82 | 2.31 | 3.0743 (16) | 155 |
Symmetry code: (ii) −x+1, −y+1, −z. |