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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806040682/hb2165sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806040682/hb2165Isup2.hkl
Contains datablock I

CCDC reference: 627682

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.052
  • wR factor = 0.152
  • Data-to-parameter ratio = 15.6

checkCIF/PLATON results

No syntax errors found



Alert level A ABSTM02_ALERT_3_A The ratio of expected to reported Tmax/Tmin(RR') is < 0.50 Tmin and Tmax reported: 0.192 0.492 Tmin(prime) and Tmax expected: 0.391 0.437 RR(prime) = 0.437 Please check that your absorption correction is appropriate.
Author Response: The ratio is given by the absorption correction program; the large difference is a reflection of the quality of the less-than-optimum quality of the crystal. Indeed, the final difference Fourier map shows a large peak.
 A statement on this is added to the refinement.

PLAT061_ALERT_3_A Tmax/Tmin Range Test RR' too Large .............       0.41
Author Response: See above.

Alert level C DIFMX01_ALERT_2_C The maximum difference density is > 0.1*ZMAX*0.75 _refine_diff_density_max given = 2.460 Test value = 2.175 DIFMX02_ALERT_1_C The maximum difference density is > 0.1*ZMAX*0.75 The relevant atom site should be identified. PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.89 PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 3.97 PLAT097_ALERT_2_C Maximum (Positive) Residual Density ............ 2.46 e/A    PLAT150_ALERT_1_C Volume as Calculated Differs from that Given ... 1666.00 Ang-3 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7
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 0.888 Tmax scaled 0.437 Tmin scaled 0.171
Author Response: The ratio is given by the absorption correction program; the large difference is a reflection of the quality of the less-than-optimum quality of the crystal. Indeed, the final difference Fourier map shows a large peak.
 A statement on this is added to the refinement.


2 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 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 4 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

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 = 553.80Dx = 2.208 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 11235 reflections
a = 9.560 (4) Åθ = 3.1–27.5°
b = 13.306 (6) ŵ = 4.14 mm1
c = 13.832 (7) ÅT = 295 K
β = 108.81 (2)°Block, green
V = 1666 (1) Å30.22 × 0.20 × 0.20 mm
Z = 4
Data collection top
Rigaku RAXIS-RAPID IP
diffractometer
3800 independent reflections
Radiation source: fine-focus sealed tube2726 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.049
ω scanθmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan
ABSCOR (Higashi, 1995)
h = 1112
Tmin = 0.192, Tmax = 0.492k = 1717
15730 measured reflectionsl = 1717
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.052Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.152H-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 parametersΔρmax = 2.46 e Å3
0 restraintsΔρmin = 0.62 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu10.75614 (6)0.85499 (4)0.74956 (4)0.03332 (19)
Cu20.15922 (7)0.96140 (4)0.44929 (5)0.0401 (2)
Cu30.34285 (7)1.17714 (4)0.56061 (5)0.0395 (2)
Cl10.12024 (15)1.12485 (9)0.42353 (10)0.0454 (3)
Cl20.34816 (16)1.33676 (9)0.58839 (10)0.0456 (3)
N10.7975 (4)1.0043 (3)0.7848 (3)0.0292 (8)
N20.5694 (4)0.9141 (3)0.6631 (3)0.0336 (8)
N30.4397 (5)0.8832 (3)0.5970 (3)0.0415 (10)
N40.3608 (4)0.9611 (3)0.5606 (3)0.0410 (10)
N50.4349 (4)1.0470 (3)0.6019 (3)0.0326 (8)
N60.7118 (4)0.7061 (3)0.7136 (3)0.0317 (8)
N70.9472 (4)0.7980 (3)0.8272 (3)0.0339 (9)
N81.0817 (4)0.8293 (3)0.8891 (3)0.0401 (9)
N91.1603 (4)0.7510 (3)0.9276 (3)0.0427 (10)
N101.0792 (4)0.6656 (3)0.8938 (3)0.0345 (8)
C10.9184 (5)1.0420 (3)0.8545 (4)0.0369 (10)
H10.99440.99880.88920.044*
C20.9327 (5)1.1442 (3)0.8760 (4)0.0385 (11)
H21.01751.16900.92450.046*
C30.8207 (5)1.2086 (3)0.8251 (4)0.0407 (11)
H30.82811.27710.83950.049*
C40.6964 (5)1.1700 (3)0.7517 (4)0.0352 (10)
H40.62051.21230.71490.042*
C50.6873 (5)1.0681 (3)0.7344 (3)0.0286 (9)
C60.5626 (5)1.0148 (3)0.6648 (3)0.0285 (9)
C70.5892 (5)0.6658 (3)0.6482 (4)0.0346 (10)
H70.51460.70840.61030.042*
C80.5696 (6)0.5634 (4)0.6349 (4)0.0387 (11)
H80.48250.53760.58970.046*
C90.6807 (6)0.4997 (3)0.6893 (4)0.0408 (11)
H90.67000.43050.68070.049*
C100.8087 (5)0.5399 (3)0.7569 (4)0.0398 (11)
H100.88450.49810.79490.048*
C110.8216 (5)0.6430 (3)0.7668 (3)0.0303 (9)
C120.9511 (5)0.6976 (3)0.8315 (3)0.0296 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0268 (3)0.0199 (3)0.0428 (4)0.0012 (2)0.0032 (2)0.0001 (2)
Cu20.0350 (3)0.0293 (3)0.0476 (4)0.0045 (2)0.0015 (3)0.0058 (2)
Cu30.0447 (4)0.0238 (3)0.0479 (4)0.0056 (3)0.0122 (3)0.0014 (2)
Cl10.0440 (7)0.0282 (6)0.0508 (7)0.0062 (5)0.0030 (6)0.0010 (5)
Cl20.0601 (8)0.0246 (5)0.0542 (8)0.0040 (5)0.0215 (6)0.0052 (5)
N10.0280 (18)0.0219 (17)0.035 (2)0.0003 (15)0.0058 (16)0.0014 (15)
N20.0266 (19)0.0246 (18)0.040 (2)0.0016 (16)0.0023 (16)0.0028 (15)
N30.039 (2)0.0266 (19)0.046 (2)0.0017 (18)0.0051 (18)0.0062 (17)
N40.032 (2)0.027 (2)0.051 (3)0.0002 (17)0.0052 (19)0.0053 (17)
N50.0288 (19)0.0216 (17)0.039 (2)0.0039 (15)0.0010 (16)0.0001 (15)
N60.0299 (19)0.0218 (17)0.040 (2)0.0020 (16)0.0059 (16)0.0010 (15)
N70.0261 (19)0.0279 (19)0.039 (2)0.0002 (16)0.0011 (16)0.0007 (16)
N80.032 (2)0.0292 (19)0.048 (2)0.0031 (17)0.0018 (18)0.0008 (17)
N90.030 (2)0.036 (2)0.052 (3)0.0000 (18)0.0001 (19)0.0020 (19)
N100.030 (2)0.0287 (18)0.042 (2)0.0029 (16)0.0064 (17)0.0036 (16)
C10.030 (2)0.033 (2)0.041 (3)0.001 (2)0.002 (2)0.002 (2)
C20.033 (2)0.036 (3)0.042 (3)0.010 (2)0.005 (2)0.008 (2)
C30.038 (3)0.028 (2)0.054 (3)0.005 (2)0.011 (2)0.008 (2)
C40.033 (2)0.024 (2)0.045 (3)0.000 (2)0.008 (2)0.0011 (19)
C50.023 (2)0.026 (2)0.036 (2)0.0034 (18)0.0081 (18)0.0015 (17)
C60.024 (2)0.0212 (19)0.038 (2)0.0031 (18)0.0060 (18)0.0005 (17)
C70.028 (2)0.031 (2)0.039 (3)0.005 (2)0.0032 (19)0.0011 (19)
C80.037 (3)0.032 (2)0.040 (3)0.001 (2)0.003 (2)0.006 (2)
C90.042 (3)0.023 (2)0.058 (3)0.007 (2)0.017 (2)0.006 (2)
C100.031 (2)0.029 (2)0.054 (3)0.006 (2)0.006 (2)0.008 (2)
C110.024 (2)0.030 (2)0.037 (2)0.0003 (18)0.0093 (18)0.0022 (17)
C120.026 (2)0.028 (2)0.033 (2)0.0009 (18)0.0060 (18)0.0009 (17)
Geometric parameters (Å, º) top
Cu1—N12.053 (4)N8—N91.295 (5)
Cu1—N21.964 (4)N9—N101.370 (5)
Cu1—N62.054 (4)N10—C121.320 (6)
Cu1—N71.949 (4)N10—Cu2iii1.911 (4)
Cu1—Cl2i2.742 (2)C1—C21.390 (6)
Cu2—N42.043 (4)C1—H10.9300
Cu2—N10ii1.911 (4)C2—C31.375 (7)
Cu2—Cl12.216 (2)C2—H20.9300
Cu3—N51.943 (4)C3—C41.389 (7)
Cu3—Cl12.451 (2)C3—H30.9300
Cu3—Cl22.156 (2)C4—C51.375 (6)
N1—C11.341 (6)C4—H40.9300
N1—C51.357 (6)C5—C61.453 (6)
N2—C61.343 (5)C7—C81.380 (6)
N2—N31.346 (5)C7—H70.9300
N3—N41.285 (5)C8—C91.377 (7)
N4—N51.369 (5)C8—H80.9300
N5—C61.321 (6)C9—C101.385 (7)
N6—C71.341 (6)C9—H90.9300
N6—C111.360 (6)C10—C111.381 (6)
N7—C121.337 (5)C10—H100.9300
N7—N81.360 (5)C11—C121.466 (6)
N1—Cu1—N279.9 (2)C12—N10—N9105.0 (4)
N1—Cu1—N6179.2 (1)C12—N10—Cu2iii135.6 (3)
N1—Cu1—N799.9 (2)N9—N10—Cu2iii119.1 (3)
N1—Cu1—Cl2i89.1 (1)N1—C1—C2121.5 (4)
N2—Cu1—N699.4 (2)N1—C1—H1119.2
N2—Cu1—N7175.8 (2)C2—C1—H1119.2
N2—Cu1—Cl2i92.0 (1)C3—C2—C1119.6 (4)
N6—Cu1—N780.9 (2)C3—C2—H2120.2
N6—Cu1—Cl2i90.7 (1)C1—C2—H2120.2
N7—Cu1—Cl2i92.2 (1)C2—C3—C4119.0 (4)
N4—Cu2—N10ii117.4 (2)C2—C3—H3120.5
N4—Cu2—Cl1101.1 (1)C4—C3—H3120.5
N10ii—Cu2—Cl1141.1 (1)C5—C4—C3118.9 (4)
N5—Cu3—Cl199.9 (1)C5—C4—H4120.5
N5—Cu3—Cl2147.5 (1)C3—C4—H4120.5
Cl1—Cu3—Cl2112.5 (1)N1—C5—C4122.2 (4)
Cu2—Cl1—Cu395.5 (1)N1—C5—C6111.8 (4)
Cu3—Cl2—Cu1iv103.8 (1)C4—C5—C6126.1 (4)
C1—N1—C5118.8 (4)N5—C6—N2110.6 (4)
C1—N1—Cu1126.0 (3)N5—C6—C5131.7 (4)
C5—N1—Cu1115.1 (3)N2—C6—C5117.6 (4)
C6—N2—N3106.1 (4)N6—C7—C8122.5 (4)
C6—N2—Cu1115.4 (3)N6—C7—H7118.8
N3—N2—Cu1138.5 (3)C8—C7—H7118.8
N4—N3—N2108.4 (4)C9—C8—C7119.1 (5)
N3—N4—N5110.5 (4)C9—C8—H8120.4
N3—N4—Cu2126.1 (3)C7—C8—H8120.4
N5—N4—Cu2123.3 (3)C8—C9—C10119.3 (4)
C6—N5—N4104.4 (3)C8—C9—H9120.3
C6—N5—Cu3135.8 (3)C10—C9—H9120.3
N4—N5—Cu3119.8 (3)C11—C10—C9118.8 (4)
C7—N6—C11118.2 (4)C11—C10—H10120.6
C7—N6—Cu1128.1 (3)C9—C10—H10120.6
C11—N6—Cu1113.7 (3)N6—C11—C10122.1 (4)
C12—N7—N8105.7 (4)N6—C11—C12112.1 (4)
C12—N7—Cu1114.9 (3)C10—C11—C12125.8 (4)
N8—N7—Cu1139.1 (3)N10—C12—N7111.0 (4)
N9—N8—N7108.5 (4)N10—C12—C11131.4 (4)
N8—N9—N10109.7 (4)N7—C12—C11117.5 (4)
N10ii—Cu2—Cl1—Cu3175.86 (19)N8—N9—N10—C121.7 (5)
N4—Cu2—Cl1—Cu34.52 (13)N8—N9—N10—Cu2iii173.5 (3)
N5—Cu3—Cl1—Cu26.02 (13)C5—N1—C1—C20.1 (7)
Cl2—Cu3—Cl1—Cu2171.07 (6)Cu1—N1—C1—C2176.9 (3)
N5—Cu3—Cl2—Cu1iv77.5 (2)N1—C1—C2—C30.1 (7)
Cl1—Cu3—Cl2—Cu1iv97.18 (7)C1—C2—C3—C41.1 (7)
N7—Cu1—N1—C18.4 (4)C2—C3—C4—C51.8 (7)
N2—Cu1—N1—C1175.8 (4)C1—N1—C5—C40.7 (6)
Cl2i—Cu1—N1—C183.7 (4)Cu1—N1—C5—C4178.1 (3)
N7—Cu1—N1—C5174.4 (3)C1—N1—C5—C6177.7 (4)
N2—Cu1—N1—C51.4 (3)Cu1—N1—C5—C60.4 (4)
Cl2i—Cu1—N1—C593.5 (3)C3—C4—C5—N11.7 (7)
N1—Cu1—N2—C62.9 (3)C3—C4—C5—C6176.5 (4)
N6—Cu1—N2—C6177.3 (3)N4—N5—C6—N20.3 (5)
Cl2i—Cu1—N2—C691.7 (3)Cu3—N5—C6—N2179.3 (3)
N1—Cu1—N2—N3179.1 (5)N4—N5—C6—C5177.2 (5)
N6—Cu1—N2—N30.6 (5)Cu3—N5—C6—C53.2 (8)
Cl2i—Cu1—N2—N390.4 (5)N3—N2—C6—N50.6 (5)
C6—N2—N3—N40.7 (5)Cu1—N2—C6—N5177.9 (3)
Cu1—N2—N3—N4177.3 (4)N3—N2—C6—C5177.3 (4)
N2—N3—N4—N50.5 (6)Cu1—N2—C6—C54.1 (5)
N2—N3—N4—Cu2175.4 (3)N1—C5—C6—N5179.7 (5)
N10ii—Cu2—N4—N30.1 (5)C4—C5—C6—N52.0 (8)
Cl1—Cu2—N4—N3173.8 (4)N1—C5—C6—N22.9 (6)
N10ii—Cu2—N4—N5175.5 (3)C4—C5—C6—N2175.4 (4)
Cl1—Cu2—N4—N51.6 (4)C11—N6—C7—C81.5 (7)
N3—N4—N5—C60.1 (5)Cu1—N6—C7—C8176.3 (3)
Cu2—N4—N5—C6175.9 (3)N6—C7—C8—C91.2 (8)
N3—N4—N5—Cu3179.8 (3)C7—C8—C9—C100.7 (7)
Cu2—N4—N5—Cu33.7 (5)C8—C9—C10—C110.7 (7)
Cl2—Cu3—N5—C612.0 (6)C7—N6—C11—C101.5 (7)
Cl1—Cu3—N5—C6173.0 (5)Cu1—N6—C11—C10176.6 (4)
Cl2—Cu3—N5—N4168.5 (2)C7—N6—C11—C12177.3 (4)
Cl1—Cu3—N5—N46.5 (4)Cu1—N6—C11—C124.6 (5)
N7—Cu1—N6—C7174.9 (4)C9—C10—C11—N61.1 (7)
N2—Cu1—N6—C70.8 (4)C9—C10—C11—C12177.4 (4)
Cl2i—Cu1—N6—C792.9 (4)N9—N10—C12—N71.7 (5)
N7—Cu1—N6—C117.2 (3)Cu2iii—N10—C12—N7172.3 (3)
N2—Cu1—N6—C11177.0 (3)N9—N10—C12—C11175.8 (5)
Cl2i—Cu1—N6—C1184.9 (3)Cu2iii—N10—C12—C1110.2 (8)
N1—Cu1—N7—C12171.3 (3)N8—N7—C12—N101.1 (5)
N6—Cu1—N7—C128.5 (3)Cu1—N7—C12—N10173.5 (3)
Cl2i—Cu1—N7—C1281.8 (3)N8—N7—C12—C11176.8 (4)
N1—Cu1—N7—N80.7 (5)Cu1—N7—C12—C118.6 (5)
N6—Cu1—N7—N8179.5 (5)N6—C11—C12—N10179.7 (5)
Cl2i—Cu1—N7—N890.2 (5)C10—C11—C12—N101.1 (8)
C12—N7—N8—N90.0 (5)N6—C11—C12—N72.4 (6)
Cu1—N7—N8—N9172.5 (4)C10—C11—C12—N7176.3 (4)
N7—N8—N9—N101.1 (5)
Symmetry codes: (i) x+1, y1/2, z+3/2; (ii) x1, y+3/2, z1/2; (iii) x+1, y+3/2, z+1/2; (iv) x+1, y+1/2, z+3/2.
 

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