metal-organic compounds
In the polymeric mixed-valence title compound, [Cu2ICuII(C6H5N5)2Cl2], the CuII atom is chelated by two pyridyltetrazolate (C6H5N5−) anions, resulting in a CuN4 square planar arrangement. The two independent CuI cations adopt approximate CuCl2N and CuN2Cl trigonal planar geometries. The pyridyltetrazolate anions serve to bridge the different copper ions into an almost flat ribbon. Adjacent ribbons are linked by a weak CuII–Cl bond [2.742 (2) Å] into a layer structure.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806040682/hb2165sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806040682/hb2165Isup2.hkl |
CCDC reference: 627682
Computing details top
Data collection: RAPID-AUTO (Rigaku/MSC, 2004); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: SHELXL97.
(I) top
Crystal data top
[Cu2Cl2(C6H5N5)2] | F(000) = 1084 |
Mr = 553.80 | Dx = 2.208 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 11235 reflections |
a = 9.560 (4) Å | θ = 3.1–27.5° |
b = 13.306 (6) Å | µ = 4.14 mm−1 |
c = 13.832 (7) Å | T = 295 K |
β = 108.81 (2)° | Block, green |
V = 1666 (1) Å3 | 0.22 × 0.20 × 0.20 mm |
Z = 4 |
Data collection top
Rigaku RAXIS-RAPID IP diffractometer | 3800 independent reflections |
Radiation source: fine-focus sealed tube | 2726 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.049 |
ω scan | θmax = 27.5°, θmin = 3.1° |
Absorption correction: multi-scan ABSCOR (Higashi, 1995) | h = −11→12 |
Tmin = 0.192, Tmax = 0.492 | k = −17→17 |
15730 measured reflections | l = −17→17 |
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)] = 0.052 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.152 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0946P)2 + 0.2899P] where P = (Fo2 + 2Fc2)/3 |
3800 reflections | (Δ/σ)max = 0.001 |
244 parameters | Δρmax = 2.46 e Å−3 |
0 restraints | Δρmin = −0.62 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Cu1 | 0.75614 (6) | 0.85499 (4) | 0.74956 (4) | 0.03332 (19) | |
Cu2 | 0.15922 (7) | 0.96140 (4) | 0.44929 (5) | 0.0401 (2) | |
Cu3 | 0.34285 (7) | 1.17714 (4) | 0.56061 (5) | 0.0395 (2) | |
Cl1 | 0.12024 (15) | 1.12485 (9) | 0.42353 (10) | 0.0454 (3) | |
Cl2 | 0.34816 (16) | 1.33676 (9) | 0.58839 (10) | 0.0456 (3) | |
N1 | 0.7975 (4) | 1.0043 (3) | 0.7848 (3) | 0.0292 (8) | |
N2 | 0.5694 (4) | 0.9141 (3) | 0.6631 (3) | 0.0336 (8) | |
N3 | 0.4397 (5) | 0.8832 (3) | 0.5970 (3) | 0.0415 (10) | |
N4 | 0.3608 (4) | 0.9611 (3) | 0.5606 (3) | 0.0410 (10) | |
N5 | 0.4349 (4) | 1.0470 (3) | 0.6019 (3) | 0.0326 (8) | |
N6 | 0.7118 (4) | 0.7061 (3) | 0.7136 (3) | 0.0317 (8) | |
N7 | 0.9472 (4) | 0.7980 (3) | 0.8272 (3) | 0.0339 (9) | |
N8 | 1.0817 (4) | 0.8293 (3) | 0.8891 (3) | 0.0401 (9) | |
N9 | 1.1603 (4) | 0.7510 (3) | 0.9276 (3) | 0.0427 (10) | |
N10 | 1.0792 (4) | 0.6656 (3) | 0.8938 (3) | 0.0345 (8) | |
C1 | 0.9184 (5) | 1.0420 (3) | 0.8545 (4) | 0.0369 (10) | |
H1 | 0.9944 | 0.9988 | 0.8892 | 0.044* | |
C2 | 0.9327 (5) | 1.1442 (3) | 0.8760 (4) | 0.0385 (11) | |
H2 | 1.0175 | 1.1690 | 0.9245 | 0.046* | |
C3 | 0.8207 (5) | 1.2086 (3) | 0.8251 (4) | 0.0407 (11) | |
H3 | 0.8281 | 1.2771 | 0.8395 | 0.049* | |
C4 | 0.6964 (5) | 1.1700 (3) | 0.7517 (4) | 0.0352 (10) | |
H4 | 0.6205 | 1.2123 | 0.7149 | 0.042* | |
C5 | 0.6873 (5) | 1.0681 (3) | 0.7344 (3) | 0.0286 (9) | |
C6 | 0.5626 (5) | 1.0148 (3) | 0.6648 (3) | 0.0285 (9) | |
C7 | 0.5892 (5) | 0.6658 (3) | 0.6482 (4) | 0.0346 (10) | |
H7 | 0.5146 | 0.7084 | 0.6103 | 0.042* | |
C8 | 0.5696 (6) | 0.5634 (4) | 0.6349 (4) | 0.0387 (11) | |
H8 | 0.4825 | 0.5376 | 0.5897 | 0.046* | |
C9 | 0.6807 (6) | 0.4997 (3) | 0.6893 (4) | 0.0408 (11) | |
H9 | 0.6700 | 0.4305 | 0.6807 | 0.049* | |
C10 | 0.8087 (5) | 0.5399 (3) | 0.7569 (4) | 0.0398 (11) | |
H10 | 0.8845 | 0.4981 | 0.7949 | 0.048* | |
C11 | 0.8216 (5) | 0.6430 (3) | 0.7668 (3) | 0.0303 (9) | |
C12 | 0.9511 (5) | 0.6976 (3) | 0.8315 (3) | 0.0296 (9) |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0268 (3) | 0.0199 (3) | 0.0428 (4) | 0.0012 (2) | −0.0032 (2) | −0.0001 (2) |
Cu2 | 0.0350 (3) | 0.0293 (3) | 0.0476 (4) | −0.0045 (2) | 0.0015 (3) | −0.0058 (2) |
Cu3 | 0.0447 (4) | 0.0238 (3) | 0.0479 (4) | 0.0056 (3) | 0.0122 (3) | 0.0014 (2) |
Cl1 | 0.0440 (7) | 0.0282 (6) | 0.0508 (7) | 0.0062 (5) | −0.0030 (6) | −0.0010 (5) |
Cl2 | 0.0601 (8) | 0.0246 (5) | 0.0542 (8) | −0.0040 (5) | 0.0215 (6) | −0.0052 (5) |
N1 | 0.0280 (18) | 0.0219 (17) | 0.035 (2) | −0.0003 (15) | 0.0058 (16) | −0.0014 (15) |
N2 | 0.0266 (19) | 0.0246 (18) | 0.040 (2) | −0.0016 (16) | −0.0023 (16) | −0.0028 (15) |
N3 | 0.039 (2) | 0.0266 (19) | 0.046 (2) | −0.0017 (18) | −0.0051 (18) | −0.0062 (17) |
N4 | 0.032 (2) | 0.027 (2) | 0.051 (3) | −0.0002 (17) | −0.0052 (19) | −0.0053 (17) |
N5 | 0.0288 (19) | 0.0216 (17) | 0.039 (2) | −0.0039 (15) | −0.0010 (16) | 0.0001 (15) |
N6 | 0.0299 (19) | 0.0218 (17) | 0.040 (2) | 0.0020 (16) | 0.0059 (16) | −0.0010 (15) |
N7 | 0.0261 (19) | 0.0279 (19) | 0.039 (2) | 0.0002 (16) | −0.0011 (16) | 0.0007 (16) |
N8 | 0.032 (2) | 0.0292 (19) | 0.048 (2) | 0.0031 (17) | −0.0018 (18) | 0.0008 (17) |
N9 | 0.030 (2) | 0.036 (2) | 0.052 (3) | 0.0000 (18) | 0.0001 (19) | −0.0020 (19) |
N10 | 0.030 (2) | 0.0287 (18) | 0.042 (2) | 0.0029 (16) | 0.0064 (17) | 0.0036 (16) |
C1 | 0.030 (2) | 0.033 (2) | 0.041 (3) | 0.001 (2) | 0.002 (2) | 0.002 (2) |
C2 | 0.033 (2) | 0.036 (3) | 0.042 (3) | −0.010 (2) | 0.005 (2) | −0.008 (2) |
C3 | 0.038 (3) | 0.028 (2) | 0.054 (3) | −0.005 (2) | 0.011 (2) | −0.008 (2) |
C4 | 0.033 (2) | 0.024 (2) | 0.045 (3) | 0.000 (2) | 0.008 (2) | −0.0011 (19) |
C5 | 0.023 (2) | 0.026 (2) | 0.036 (2) | −0.0034 (18) | 0.0081 (18) | 0.0015 (17) |
C6 | 0.024 (2) | 0.0212 (19) | 0.038 (2) | −0.0031 (18) | 0.0060 (18) | −0.0005 (17) |
C7 | 0.028 (2) | 0.031 (2) | 0.039 (3) | 0.005 (2) | 0.0032 (19) | −0.0011 (19) |
C8 | 0.037 (3) | 0.032 (2) | 0.040 (3) | −0.001 (2) | 0.003 (2) | −0.006 (2) |
C9 | 0.042 (3) | 0.023 (2) | 0.058 (3) | −0.007 (2) | 0.017 (2) | −0.006 (2) |
C10 | 0.031 (2) | 0.029 (2) | 0.054 (3) | 0.006 (2) | 0.006 (2) | 0.008 (2) |
C11 | 0.024 (2) | 0.030 (2) | 0.037 (2) | −0.0003 (18) | 0.0093 (18) | −0.0022 (17) |
C12 | 0.026 (2) | 0.028 (2) | 0.033 (2) | 0.0009 (18) | 0.0060 (18) | 0.0009 (17) |
Geometric parameters (Å, º) top
Cu1—N1 | 2.053 (4) | N8—N9 | 1.295 (5) |
Cu1—N2 | 1.964 (4) | N9—N10 | 1.370 (5) |
Cu1—N6 | 2.054 (4) | N10—C12 | 1.320 (6) |
Cu1—N7 | 1.949 (4) | N10—Cu2iii | 1.911 (4) |
Cu1—Cl2i | 2.742 (2) | C1—C2 | 1.390 (6) |
Cu2—N4 | 2.043 (4) | C1—H1 | 0.9300 |
Cu2—N10ii | 1.911 (4) | C2—C3 | 1.375 (7) |
Cu2—Cl1 | 2.216 (2) | C2—H2 | 0.9300 |
Cu3—N5 | 1.943 (4) | C3—C4 | 1.389 (7) |
Cu3—Cl1 | 2.451 (2) | C3—H3 | 0.9300 |
Cu3—Cl2 | 2.156 (2) | C4—C5 | 1.375 (6) |
N1—C1 | 1.341 (6) | C4—H4 | 0.9300 |
N1—C5 | 1.357 (6) | C5—C6 | 1.453 (6) |
N2—C6 | 1.343 (5) | C7—C8 | 1.380 (6) |
N2—N3 | 1.346 (5) | C7—H7 | 0.9300 |
N3—N4 | 1.285 (5) | C8—C9 | 1.377 (7) |
N4—N5 | 1.369 (5) | C8—H8 | 0.9300 |
N5—C6 | 1.321 (6) | C9—C10 | 1.385 (7) |
N6—C7 | 1.341 (6) | C9—H9 | 0.9300 |
N6—C11 | 1.360 (6) | C10—C11 | 1.381 (6) |
N7—C12 | 1.337 (5) | C10—H10 | 0.9300 |
N7—N8 | 1.360 (5) | C11—C12 | 1.466 (6) |
N1—Cu1—N2 | 79.9 (2) | C12—N10—N9 | 105.0 (4) |
N1—Cu1—N6 | 179.2 (1) | C12—N10—Cu2iii | 135.6 (3) |
N1—Cu1—N7 | 99.9 (2) | N9—N10—Cu2iii | 119.1 (3) |
N1—Cu1—Cl2i | 89.1 (1) | N1—C1—C2 | 121.5 (4) |
N2—Cu1—N6 | 99.4 (2) | N1—C1—H1 | 119.2 |
N2—Cu1—N7 | 175.8 (2) | C2—C1—H1 | 119.2 |
N2—Cu1—Cl2i | 92.0 (1) | C3—C2—C1 | 119.6 (4) |
N6—Cu1—N7 | 80.9 (2) | C3—C2—H2 | 120.2 |
N6—Cu1—Cl2i | 90.7 (1) | C1—C2—H2 | 120.2 |
N7—Cu1—Cl2i | 92.2 (1) | C2—C3—C4 | 119.0 (4) |
N4—Cu2—N10ii | 117.4 (2) | C2—C3—H3 | 120.5 |
N4—Cu2—Cl1 | 101.1 (1) | C4—C3—H3 | 120.5 |
N10ii—Cu2—Cl1 | 141.1 (1) | C5—C4—C3 | 118.9 (4) |
N5—Cu3—Cl1 | 99.9 (1) | C5—C4—H4 | 120.5 |
N5—Cu3—Cl2 | 147.5 (1) | C3—C4—H4 | 120.5 |
Cl1—Cu3—Cl2 | 112.5 (1) | N1—C5—C4 | 122.2 (4) |
Cu2—Cl1—Cu3 | 95.5 (1) | N1—C5—C6 | 111.8 (4) |
Cu3—Cl2—Cu1iv | 103.8 (1) | C4—C5—C6 | 126.1 (4) |
C1—N1—C5 | 118.8 (4) | N5—C6—N2 | 110.6 (4) |
C1—N1—Cu1 | 126.0 (3) | N5—C6—C5 | 131.7 (4) |
C5—N1—Cu1 | 115.1 (3) | N2—C6—C5 | 117.6 (4) |
C6—N2—N3 | 106.1 (4) | N6—C7—C8 | 122.5 (4) |
C6—N2—Cu1 | 115.4 (3) | N6—C7—H7 | 118.8 |
N3—N2—Cu1 | 138.5 (3) | C8—C7—H7 | 118.8 |
N4—N3—N2 | 108.4 (4) | C9—C8—C7 | 119.1 (5) |
N3—N4—N5 | 110.5 (4) | C9—C8—H8 | 120.4 |
N3—N4—Cu2 | 126.1 (3) | C7—C8—H8 | 120.4 |
N5—N4—Cu2 | 123.3 (3) | C8—C9—C10 | 119.3 (4) |
C6—N5—N4 | 104.4 (3) | C8—C9—H9 | 120.3 |
C6—N5—Cu3 | 135.8 (3) | C10—C9—H9 | 120.3 |
N4—N5—Cu3 | 119.8 (3) | C11—C10—C9 | 118.8 (4) |
C7—N6—C11 | 118.2 (4) | C11—C10—H10 | 120.6 |
C7—N6—Cu1 | 128.1 (3) | C9—C10—H10 | 120.6 |
C11—N6—Cu1 | 113.7 (3) | N6—C11—C10 | 122.1 (4) |
C12—N7—N8 | 105.7 (4) | N6—C11—C12 | 112.1 (4) |
C12—N7—Cu1 | 114.9 (3) | C10—C11—C12 | 125.8 (4) |
N8—N7—Cu1 | 139.1 (3) | N10—C12—N7 | 111.0 (4) |
N9—N8—N7 | 108.5 (4) | N10—C12—C11 | 131.4 (4) |
N8—N9—N10 | 109.7 (4) | N7—C12—C11 | 117.5 (4) |
N10ii—Cu2—Cl1—Cu3 | −175.86 (19) | N8—N9—N10—C12 | 1.7 (5) |
N4—Cu2—Cl1—Cu3 | −4.52 (13) | N8—N9—N10—Cu2iii | −173.5 (3) |
N5—Cu3—Cl1—Cu2 | 6.02 (13) | C5—N1—C1—C2 | 0.1 (7) |
Cl2—Cu3—Cl1—Cu2 | −171.07 (6) | Cu1—N1—C1—C2 | −176.9 (3) |
N5—Cu3—Cl2—Cu1iv | −77.5 (2) | N1—C1—C2—C3 | 0.1 (7) |
Cl1—Cu3—Cl2—Cu1iv | 97.18 (7) | C1—C2—C3—C4 | −1.1 (7) |
N7—Cu1—N1—C1 | −8.4 (4) | C2—C3—C4—C5 | 1.8 (7) |
N2—Cu1—N1—C1 | 175.8 (4) | C1—N1—C5—C4 | 0.7 (6) |
Cl2i—Cu1—N1—C1 | 83.7 (4) | Cu1—N1—C5—C4 | 178.1 (3) |
N7—Cu1—N1—C5 | 174.4 (3) | C1—N1—C5—C6 | −177.7 (4) |
N2—Cu1—N1—C5 | −1.4 (3) | Cu1—N1—C5—C6 | −0.4 (4) |
Cl2i—Cu1—N1—C5 | −93.5 (3) | C3—C4—C5—N1 | −1.7 (7) |
N1—Cu1—N2—C6 | 2.9 (3) | C3—C4—C5—C6 | 176.5 (4) |
N6—Cu1—N2—C6 | −177.3 (3) | N4—N5—C6—N2 | 0.3 (5) |
Cl2i—Cu1—N2—C6 | 91.7 (3) | Cu3—N5—C6—N2 | −179.3 (3) |
N1—Cu1—N2—N3 | −179.1 (5) | N4—N5—C6—C5 | −177.2 (5) |
N6—Cu1—N2—N3 | 0.6 (5) | Cu3—N5—C6—C5 | 3.2 (8) |
Cl2i—Cu1—N2—N3 | −90.4 (5) | N3—N2—C6—N5 | −0.6 (5) |
C6—N2—N3—N4 | 0.7 (5) | Cu1—N2—C6—N5 | 177.9 (3) |
Cu1—N2—N3—N4 | −177.3 (4) | N3—N2—C6—C5 | 177.3 (4) |
N2—N3—N4—N5 | −0.5 (6) | Cu1—N2—C6—C5 | −4.1 (5) |
N2—N3—N4—Cu2 | 175.4 (3) | N1—C5—C6—N5 | −179.7 (5) |
N10ii—Cu2—N4—N3 | 0.1 (5) | C4—C5—C6—N5 | 2.0 (8) |
Cl1—Cu2—N4—N3 | −173.8 (4) | N1—C5—C6—N2 | 2.9 (6) |
N10ii—Cu2—N4—N5 | 175.5 (3) | C4—C5—C6—N2 | −175.4 (4) |
Cl1—Cu2—N4—N5 | 1.6 (4) | C11—N6—C7—C8 | 1.5 (7) |
N3—N4—N5—C6 | 0.1 (5) | Cu1—N6—C7—C8 | −176.3 (3) |
Cu2—N4—N5—C6 | −175.9 (3) | N6—C7—C8—C9 | −1.2 (8) |
N3—N4—N5—Cu3 | 179.8 (3) | C7—C8—C9—C10 | 0.7 (7) |
Cu2—N4—N5—Cu3 | 3.7 (5) | C8—C9—C10—C11 | −0.7 (7) |
Cl2—Cu3—N5—C6 | −12.0 (6) | C7—N6—C11—C10 | −1.5 (7) |
Cl1—Cu3—N5—C6 | 173.0 (5) | Cu1—N6—C11—C10 | 176.6 (4) |
Cl2—Cu3—N5—N4 | 168.5 (2) | C7—N6—C11—C12 | 177.3 (4) |
Cl1—Cu3—N5—N4 | −6.5 (4) | Cu1—N6—C11—C12 | −4.6 (5) |
N7—Cu1—N6—C7 | −174.9 (4) | C9—C10—C11—N6 | 1.1 (7) |
N2—Cu1—N6—C7 | 0.8 (4) | C9—C10—C11—C12 | −177.4 (4) |
Cl2i—Cu1—N6—C7 | 92.9 (4) | N9—N10—C12—N7 | −1.7 (5) |
N7—Cu1—N6—C11 | 7.2 (3) | Cu2iii—N10—C12—N7 | 172.3 (3) |
N2—Cu1—N6—C11 | −177.0 (3) | N9—N10—C12—C11 | 175.8 (5) |
Cl2i—Cu1—N6—C11 | −84.9 (3) | Cu2iii—N10—C12—C11 | −10.2 (8) |
N1—Cu1—N7—C12 | 171.3 (3) | N8—N7—C12—N10 | 1.1 (5) |
N6—Cu1—N7—C12 | −8.5 (3) | Cu1—N7—C12—N10 | −173.5 (3) |
Cl2i—Cu1—N7—C12 | 81.8 (3) | N8—N7—C12—C11 | −176.8 (4) |
N1—Cu1—N7—N8 | −0.7 (5) | Cu1—N7—C12—C11 | 8.6 (5) |
N6—Cu1—N7—N8 | 179.5 (5) | N6—C11—C12—N10 | −179.7 (5) |
Cl2i—Cu1—N7—N8 | −90.2 (5) | C10—C11—C12—N10 | −1.1 (8) |
C12—N7—N8—N9 | 0.0 (5) | N6—C11—C12—N7 | −2.4 (6) |
Cu1—N7—N8—N9 | 172.5 (4) | C10—C11—C12—N7 | 176.3 (4) |
N7—N8—N9—N10 | −1.1 (5) |
Symmetry codes: (i) −x+1, y−1/2, −z+3/2; (ii) x−1, −y+3/2, z−1/2; (iii) x+1, −y+3/2, z+1/2; (iv) −x+1, y+1/2, −z+3/2. |