metal-organic compounds
In the crystal structure of the title compound, [Cu3(C12H7N2O)2Cl2]n, the mixed-valence CuI/CuII cation and the cuprate(I) anion both lie on centres of inversion. The O atom of one half of the planar N,N′-chelated dinuclear copper cation binds to the Cu atom of the other half; the geometry around the metal atom is square-planar, owing to the symmetry-related metal atom at a distance of 2.3945 (5) Å. The dinuclear cations are bridged through the anions to form an infinite linear chain.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805013632/hg6178sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805013632/hg6178Isup2.hkl |
CCDC reference: 274422
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.004 Å
- R factor = 0.032
- wR factor = 0.091
- Data-to-parameter ratio = 15.0
checkCIF/PLATON results
No syntax errors found
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.374 0.585 Tmin' and Tmax expected: 0.401 0.548 RR' = 0.875 Please check that your absorption correction is appropriate. PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.82 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.94
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.937 Tmax scaled 0.548 Tmin scaled 0.351
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 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: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
catena-Poly[[bis(µ-1,10-phenanthrolin-2-olato-
κ3N,N':O)dicopper(I,II)(Cu—Cu)]-µ-chloro-copper(I)-µ-chloro] top
Crystal data top
[Cu3(C12H7N2O)2Cl2] | Z = 1 |
Mr = 651.91 | F(000) = 323 |
Triclinic, P1 | Dx = 1.976 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.0588 (6) Å | Cell parameters from 2232 reflections |
b = 8.3638 (6) Å | θ = 2.7–28.1° |
c = 10.5690 (8) Å | µ = 3.16 mm−1 |
α = 112.301 (1)° | T = 295 K |
β = 94.096 (1)° | Block, dark blue |
γ = 104.930 (1)° | 0.28 × 0.26 × 0.19 mm |
V = 547.73 (7) Å3 |
Data collection top
Bruker APEX area-detector diffractometer | 2407 independent reflections |
Radiation source: fine-focus sealed tube | 2155 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.017 |
φ and ω scans | θmax = 27.5°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −9→9 |
Tmin = 0.374, Tmax = 0.585 | k = −10→10 |
4698 measured reflections | l = −13→13 |
Refinement top
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)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.091 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0614P)2] where P = (Fo2 + 2Fc2)/3 |
2407 reflections | (Δ/σ)max = 0.001 |
160 parameters | Δρmax = 0.40 e Å−3 |
0 restraints | Δρmin = −0.30 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Cu1 | −0.02079 (5) | 0.55892 (4) | 0.61873 (3) | 0.0406 (1) | |
Cu2 | 0.5000 | 0.5000 | 0.5000 | 0.0545 (2) | |
Cl1 | 0.3858 (1) | 0.5625 (1) | 0.6850 (1) | 0.0594 (2) | |
O1 | 0.0716 (3) | 0.8031 (2) | 0.64009 (16) | 0.0449 (4) | |
N1 | 0.1318 (3) | 0.6921 (3) | 0.4204 (2) | 0.0364 (4) | |
N2 | 0.1079 (3) | 0.4013 (3) | 0.1938 (2) | 0.0405 (4) | |
C1 | 0.1404 (3) | 0.8331 (3) | 0.5396 (2) | 0.0379 (5) | |
C2 | 0.2247 (3) | 1.0136 (3) | 0.5498 (2) | 0.0437 (6) | |
C3 | 0.2929 (4) | 1.0435 (3) | 0.4422 (3) | 0.0453 (5) | |
C4 | 0.2833 (3) | 0.8939 (3) | 0.3153 (3) | 0.0409 (5) | |
C5 | 0.3542 (4) | 0.9094 (4) | 0.1959 (3) | 0.0515 (6) | |
C6 | 0.3433 (4) | 0.7608 (4) | 0.0800 (3) | 0.0502 (6) | |
C7 | 0.2610 (3) | 0.5826 (4) | 0.0734 (3) | 0.0433 (5) | |
C8 | 0.2450 (4) | 0.4200 (4) | −0.0416 (3) | 0.0498 (6) | |
C9 | 0.1664 (4) | 0.2566 (4) | −0.0355 (3) | 0.0542 (7) | |
C10 | 0.0978 (4) | 0.2531 (3) | 0.0850 (3) | 0.0497 (6) | |
C11 | 0.1903 (3) | 0.5651 (3) | 0.1895 (2) | 0.0371 (5) | |
C12 | 0.2019 (3) | 0.7223 (3) | 0.3115 (2) | 0.0360 (5) | |
H2 | 0.2325 | 1.1121 | 0.6321 | 0.052* | |
H3 | 0.3464 | 1.1618 | 0.4506 | 0.054* | |
H5 | 0.4090 | 1.0242 | 0.1978 | 0.062* | |
H6 | 0.3901 | 0.7751 | 0.0037 | 0.060* | |
H8 | 0.2880 | 0.4241 | −0.1218 | 0.060* | |
H9 | 0.1585 | 0.1490 | −0.1102 | 0.065* | |
H10 | 0.0428 | 0.1412 | 0.0880 | 0.060* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0612 (2) | 0.0301 (2) | 0.0304 (2) | 0.0123 (1) | 0.0115 (1) | 0.0129 (1) |
Cu2 | 0.0685 (3) | 0.0440 (3) | 0.0514 (3) | 0.0093 (2) | 0.0137 (2) | 0.0249 (2) |
Cl1 | 0.0625 (4) | 0.0654 (5) | 0.0559 (4) | 0.0173 (3) | 0.0156 (3) | 0.0319 (4) |
O1 | 0.066 (1) | 0.033 (1) | 0.035 (1) | 0.016 (1) | 0.013 (1) | 0.013 (1) |
N1 | 0.044 (1) | 0.030 (1) | 0.034 (1) | 0.009 (1) | 0.005 (1) | 0.014 (1) |
N2 | 0.050 (1) | 0.037 (1) | 0.033 (1) | 0.009 (1) | 0.010 (1) | 0.014 (1) |
C1 | 0.043 (1) | 0.033 (1) | 0.037 (1) | 0.013 (1) | 0.005 (1) | 0.013 (1) |
C2 | 0.048 (1) | 0.031 (1) | 0.046 (2) | 0.011 (1) | 0.005 (1) | 0.011 (1) |
C3 | 0.046 (1) | 0.033 (1) | 0.056 (2) | 0.007 (1) | 0.009 (1) | 0.021 (1) |
C4 | 0.037 (1) | 0.040 (1) | 0.046 (1) | 0.008 (1) | 0.007 (1) | 0.020 (1) |
C5 | 0.050 (1) | 0.051 (2) | 0.059 (2) | 0.007 (1) | 0.011 (1) | 0.034 (1) |
C6 | 0.050 (1) | 0.061 (2) | 0.050 (2) | 0.013 (1) | 0.020 (1) | 0.033 (1) |
C7 | 0.038 (1) | 0.054 (1) | 0.041 (1) | 0.012 (1) | 0.009 (1) | 0.023 (1) |
C8 | 0.050 (1) | 0.063 (2) | 0.037 (1) | 0.016 (1) | 0.017 (1) | 0.021 (1) |
C9 | 0.064 (2) | 0.053 (2) | 0.039 (1) | 0.018 (1) | 0.016 (1) | 0.012 (1) |
C10 | 0.064 (2) | 0.038 (1) | 0.041 (1) | 0.012 (1) | 0.014 (1) | 0.012 (1) |
C11 | 0.037 (1) | 0.039 (1) | 0.036 (1) | 0.011 (1) | 0.007 (1) | 0.018 (1) |
C12 | 0.035 (1) | 0.038 (1) | 0.037 (1) | 0.010 (1) | 0.005 (1) | 0.018 (1) |
Geometric parameters (Å, º) top
Cu1—Cu1i | 2.3945 (5) | C4—C5 | 1.429 (3) |
Cu1—Cl1 | 2.8947 (8) | C5—C6 | 1.354 (4) |
Cu1—O1 | 1.894 (2) | C6—C7 | 1.426 (3) |
Cu1—N1i | 1.908 (2) | C7—C11 | 1.400 (3) |
Cu1—N2i | 2.048 (2) | C7—C8 | 1.410 (4) |
Cu2—Cl1 | 2.1009 (7) | C8—C9 | 1.364 (4) |
Cu2—Cl1ii | 2.1009 (7) | C9—C10 | 1.402 (3) |
O1—C1 | 1.281 (3) | C11—C12 | 1.429 (3) |
N1—C1 | 1.344 (3) | C2—H2 | 0.93 |
N1—C12 | 1.369 (3) | C3—H3 | 0.93 |
N2—C10 | 1.313 (3) | C5—H5 | 0.93 |
N2—C11 | 1.363 (3) | C6—H6 | 0.93 |
C1—C2 | 1.431 (3) | C8—H8 | 0.93 |
C2—C3 | 1.349 (3) | C9—H9 | 0.93 |
C3—C4 | 1.427 (4) | C10—H10 | 0.93 |
C4—C12 | 1.385 (3) | ||
Cl1—Cu1—O1 | 90.51 (6) | C5—C6—C7 | 120.9 (2) |
Cl1—Cu1—N1i | 93.70 (6) | C11—C7—C8 | 116.6 (2) |
Cl1—Cu1—N2i | 100.65 (6) | C11—C7—C6 | 118.3 (2) |
O1—Cu1—N1i | 173.96 (7) | C8—C7—C6 | 125.1 (2) |
O1—Cu1—N2i | 99.69 (7) | C9—C8—C7 | 120.1 (2) |
N1i—Cu1—N2i | 83.80 (8) | C8—C9—C10 | 119.1 (2) |
O1—Cu1—Cu1i | 92.97 (5) | N2—C10—C9 | 122.8 (2) |
N1i—Cu1—Cu1i | 83.07 (6) | N2—C11—C7 | 123.1 (2) |
N2i—Cu1—Cu1i | 165.92 (6) | N2—C11—C12 | 116.3 (2) |
Cu1i—Cu1—Cl1 | 85.27 (2) | C7—C11—C12 | 120.6 (2) |
Cl1—Cu2—Cl1ii | 180 | N1—C12—C4 | 123.6 (2) |
Cu2—Cl1—Cu1 | 107.52 (3) | N1—C12—C11 | 116.5 (2) |
C1—O1—Cu1 | 117.9 (1) | C4—C12—C11 | 119.9 (2) |
C1—N1—C12 | 120.1 (2) | C3—C2—H2 | 119.4 |
C1—N1—Cu1i | 126.2 (2) | C1—C2—H2 | 119.4 |
C12—N1—Cu1i | 113.7 (1) | C2—C3—H3 | 119.9 |
C10—N2—C11 | 118.4 (2) | C4—C3—H3 | 119.9 |
C10—N2—Cu1i | 132.0 (2) | C6—C5—H5 | 119.3 |
C11—N2—Cu1i | 109.6 (2) | C4—C5—H5 | 119.3 |
O1—C1—N1 | 119.5 (2) | C5—C6—H6 | 119.6 |
O1—C1—C2 | 121.8 (2) | C7—C6—H6 | 119.6 |
N1—C1—C2 | 118.7 (2) | C9—C8—H8 | 120.0 |
C3—C2—C1 | 121.2 (2) | C7—C8—H8 | 120.0 |
C2—C3—C4 | 120.1 (2) | C8—C9—H9 | 120.5 |
C12—C4—C5 | 118.8 (2) | C10—C9—H9 | 120.5 |
C12—C4—C3 | 116.2 (2) | N2—C10—H10 | 118.6 |
C5—C4—C3 | 124.9 (2) | C9—C10—H10 | 118.6 |
C6—C5—C4 | 121.5 (2) | ||
O1—Cu1—Cl1—Cu2 | −85.03 (6) | C7—C8—C9—C10 | 1.6 (4) |
N1i—Cu1—Cl1—Cu2 | 90.63 (6) | C11—N2—C10—C9 | −0.6 (4) |
N2i—Cu1—Cl1—Cu2 | 175.01 (6) | Cu1i—N2—C10—C9 | 179.5 (2) |
Cu1i—Cu1—Cl1—Cu2 | 7.91 (3) | C8—C9—C10—N2 | −0.9 (4) |
N2i—Cu1—O1—C1 | 179.9 (2) | C10—N2—C11—C7 | 1.3 (3) |
Cu1i—Cu1—O1—C1 | −6.2 (2) | Cu1i—N2—C11—C7 | −178.8 (2) |
Cl1—Cu1—O1—C1 | 79.1 (2) | C10—N2—C11—C12 | −178.7 (2) |
Cu1—O1—C1—N1 | 4.7 (3) | Cu1i—N2—C11—C12 | 1.2 (2) |
Cu1—O1—C1—C2 | −176.1 (2) | C8—C7—C11—N2 | −0.5 (3) |
C12—N1—C1—O1 | 179.0 (2) | C6—C7—C11—N2 | 179.6 (2) |
Cu1i—N1—C1—O1 | 0.9 (3) | C8—C7—C11—C12 | 179.4 (2) |
C12—N1—C1—C2 | −0.3 (3) | C6—C7—C11—C12 | −0.4 (3) |
Cu1i—N1—C1—C2 | −178.4 (2) | C1—N1—C12—C4 | −0.3 (3) |
O1—C1—C2—C3 | −178.6 (2) | Cu1i—N1—C12—C4 | 178.1 (2) |
N1—C1—C2—C3 | 0.6 (3) | C1—N1—C12—C11 | 179.0 (2) |
C1—C2—C3—C4 | −0.4 (4) | Cu1i—N1—C12—C11 | −2.7 (3) |
C2—C3—C4—C12 | −0.1 (3) | C5—C4—C12—N1 | 179.2 (2) |
C2—C3—C4—C5 | −178.8 (2) | C3—C4—C12—N1 | 0.5 (3) |
C12—C4—C5—C6 | 0.0 (4) | C5—C4—C12—C11 | 0.0 (3) |
C3—C4—C5—C6 | 178.7 (2) | C3—C4—C12—C11 | −178.7 (2) |
C4—C5—C6—C7 | −0.3 (4) | N2—C11—C12—N1 | 0.9 (3) |
C5—C6—C7—C11 | 0.5 (4) | C7—C11—C12—N1 | −179.1 (2) |
C5—C6—C7—C8 | −179.4 (2) | N2—C11—C12—C4 | −179.9 (2) |
C11—C7—C8—C9 | −0.9 (4) | C7—C11—C12—C4 | 0.2 (3) |
C6—C7—C8—C9 | 178.9 (2) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1. |