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The crystal structure of the centrosymmetric title compound, fully described by the name catena-poly[[(1,10-phenanthro­line-κ2N,N′)cupriocyano]copper(I)]-μ-cyano-[[(1,10-phenanthroline-κ2N,N′)cupriocyano]copper(I)]-μ-cyano-copper(I)-μ-cyano-copper(II)-μ-cyano], [Cu3(CN)3(C12H8N2)]n, consists of (Cu–CN–)n polymeric chains in which two consecutive Cu atoms in every contiguous set of four each carry a pendant (phenanthroline)coppercyano unit. The Cu atoms with pendant groups are three-coordinate, as are the phenanthroline-chelated Cu atoms; the other independent Cu atom that comprises the backbone is two-coordinate. Two adjacent chains are linked by a Cu...Cu inter­action [2.941 (1) Å] into a ribbon. All cyano groups are disordered with no distinction between C and N atoms.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806028935/ci2121sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806028935/ci2121Isup2.hkl
Contains datablock I

CCDC reference: 620744

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.008 Å
  • Disorder in main residue
  • R factor = 0.060
  • wR factor = 0.171
  • Data-to-parameter ratio = 16.5

checkCIF/PLATON results

No syntax errors found



Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.111 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.11 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.92 PLAT301_ALERT_3_C Main Residue Disorder ......................... 16.00 Perc. PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8
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 0.923 Tmax scaled 0.508 Tmin scaled 0.407 PLAT804_ALERT_5_G ARU-Pack Problem in PLATON Analysis ............ 1 Times
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 0 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 5 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); 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[[(1,10-phenanthroline-κ2N,N')cupriocyano]copper(II)]- µ-cyano-[[(1,10-phenanthroline-κ2N,N')cupriocyano]copper(II)]- µ-cyano-copper(II)-µ-cyano-copper(II)-µ-cyano] top
Crystal data top
[Cu3(CN)3(C12H8N2)]F(000) = 1760
Mr = 448.88Dx = 1.992 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 9184 reflections
a = 6.790 (1) Åθ = 3.2–27.5°
b = 24.642 (5) ŵ = 4.23 mm1
c = 18.136 (4) ÅT = 295 K
β = 99.43 (3)°Block, brown
V = 2993.5 (10) Å30.22 × 0.18 × 0.16 mm
Z = 8
Data collection top
Rigaku R-AXIS RAPID IP
diffractometer
3430 independent reflections
Radiation source: fine-focus sealed tube2232 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.111
ω scansθmax = 27.5°, θmin = 3.2°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 88
Tmin = 0.441, Tmax = 0.551k = 3231
14429 measured reflectionsl = 2323
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)] = 0.060Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.171H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0785P)2]
where P = (Fo2 + 2Fc2)/3
3430 reflections(Δ/σ)max = 0.001
208 parametersΔρmax = 0.67 e Å3
0 restraintsΔρmin = 0.85 e Å3
Special details top

Experimental. The Rint is somewhat higher than 0.10. A check with PLATON did not suggest a misassigned space group. As a full sphere of reflections was measured, the large value is probably a consequence of the crystal quality itself. The crystals were obtained hydrothermally; the products of such reactions cannot usually be re-crystallized as they are insoluble in most organic solvents.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cu10.63781 (10)0.57896 (3)0.44086 (4)0.0441 (2)
Cu21.25966 (10)0.57965 (3)0.33521 (4)0.0488 (3)
Cu30.32909 (11)0.75378 (3)0.37598 (4)0.0476 (3)
N10.8872 (8)0.5811 (2)0.4048 (3)0.043 (1)0.50
N20.4894 (7)0.6463 (2)0.4352 (3)0.037 (1)0.50
C1'0.8872 (8)0.5811 (2)0.4048 (3)0.043 (1)0.50
C2'0.4894 (7)0.6463 (2)0.4352 (3)0.037 (1)0.50
N30.2494 (6)0.7579 (2)0.2603 (3)0.042 (1)
N40.3139 (6)0.8342 (2)0.3678 (2)0.039 (1)
C10.5316 (8)0.5185 (2)0.4856 (3)0.051 (1)0.50
C21.0338 (8)0.5801 (2)0.3803 (3)0.044 (1)0.50
C31.4428 (7)0.5744 (2)0.2707 (3)0.045 (1)0.50
C40.4135 (8)0.6874 (2)0.4195 (3)0.050 (1)0.50
N1'0.5316 (8)0.5185 (2)0.4856 (3)0.051 (1)0.50
N2'1.0338 (8)0.5801 (2)0.3803 (3)0.044 (1)0.50
N3'1.4428 (7)0.5744 (2)0.2707 (3)0.045 (1)0.50
N4'0.4135 (8)0.6874 (2)0.4195 (3)0.050 (1)0.50
C50.2110 (8)0.7196 (2)0.2086 (3)0.049 (1)
C60.1585 (8)0.7309 (3)0.1324 (4)0.050 (2)
C70.1502 (8)0.7836 (3)0.1097 (3)0.047 (1)
C80.1911 (7)0.8258 (2)0.1627 (3)0.039 (1)
C90.1837 (8)0.8820 (3)0.1444 (3)0.047 (1)
C100.2175 (8)0.9205 (2)0.1970 (3)0.045 (1)
C110.2650 (7)0.9065 (2)0.2760 (3)0.041 (1)
C120.2992 (7)0.9450 (2)0.3337 (3)0.046 (1)
C130.3381 (8)0.9273 (2)0.4058 (4)0.047 (1)
C140.3467 (7)0.8716 (2)0.4210 (3)0.041 (1)
C150.2736 (7)0.8512 (2)0.2951 (3)0.035 (1)
C160.2376 (7)0.8105 (2)0.2380 (3)0.035 (1)
H50.21940.68350.22370.058*
H60.12980.70290.09790.060*
H70.11740.79190.05920.056*
H90.15470.89230.09440.056*
H100.21040.95680.18300.054*
H120.29540.98190.32290.055*
H130.35890.95220.44480.056*
H140.37660.86030.47050.050*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0497 (4)0.0384 (4)0.0460 (4)0.0011 (3)0.0138 (3)0.0002 (3)
Cu20.0466 (4)0.0517 (5)0.0516 (5)0.0013 (3)0.0183 (4)0.0004 (3)
Cu30.0483 (4)0.0442 (5)0.0503 (5)0.0038 (3)0.0082 (3)0.0130 (3)
N10.052 (3)0.031 (3)0.047 (3)0.006 (2)0.013 (3)0.002 (2)
N20.043 (3)0.032 (3)0.037 (3)0.000 (2)0.011 (2)0.004 (2)
C1'0.052 (3)0.031 (3)0.047 (3)0.006 (2)0.013 (3)0.002 (2)
C2'0.043 (3)0.032 (3)0.037 (3)0.000 (2)0.011 (2)0.004 (2)
N30.036 (2)0.042 (3)0.048 (3)0.000 (2)0.008 (2)0.001 (2)
N40.033 (2)0.044 (3)0.043 (3)0.003 (2)0.012 (2)0.002 (2)
C10.050 (3)0.040 (3)0.069 (4)0.009 (2)0.028 (3)0.008 (3)
C20.050 (3)0.043 (3)0.040 (3)0.003 (2)0.009 (2)0.003 (2)
C30.045 (3)0.048 (3)0.042 (3)0.004 (2)0.006 (2)0.001 (2)
C40.051 (3)0.058 (4)0.039 (3)0.011 (3)0.004 (2)0.001 (3)
N1'0.050 (3)0.040 (3)0.069 (4)0.009 (2)0.028 (3)0.008 (3)
N2'0.050 (3)0.043 (3)0.040 (3)0.003 (2)0.009 (2)0.003 (2)
N3'0.045 (3)0.048 (3)0.042 (3)0.004 (2)0.006 (2)0.001 (2)
N4'0.051 (3)0.058 (4)0.039 (3)0.011 (3)0.004 (2)0.001 (3)
C50.052 (3)0.037 (3)0.056 (4)0.000 (3)0.007 (3)0.005 (3)
C60.042 (3)0.048 (4)0.058 (4)0.000 (3)0.005 (3)0.016 (3)
C70.038 (3)0.064 (4)0.037 (3)0.010 (3)0.003 (2)0.005 (3)
C80.028 (2)0.052 (3)0.037 (3)0.003 (2)0.010 (2)0.002 (3)
C90.039 (3)0.055 (4)0.047 (3)0.001 (3)0.012 (2)0.013 (3)
C100.042 (3)0.041 (3)0.054 (4)0.004 (2)0.016 (3)0.011 (3)
C110.031 (3)0.038 (3)0.052 (3)0.004 (2)0.008 (2)0.009 (3)
C120.036 (3)0.040 (3)0.059 (4)0.002 (2)0.005 (3)0.003 (3)
C130.038 (3)0.048 (4)0.054 (4)0.002 (2)0.006 (3)0.014 (3)
C140.034 (3)0.047 (3)0.044 (3)0.002 (2)0.009 (2)0.005 (3)
C150.025 (2)0.041 (3)0.040 (3)0.007 (2)0.010 (2)0.005 (2)
C160.029 (2)0.039 (3)0.041 (3)0.004 (2)0.015 (2)0.003 (2)
Geometric parameters (Å, º) top
Cu1—C11.895 (5)C8—C161.402 (7)
Cu1—N11.913 (6)C8—C91.425 (8)
Cu1—N21.935 (5)C9—C101.338 (8)
Cu1—Cu2i2.941 (1)C10—C111.456 (8)
Cu2—C21.852 (6)C11—C121.403 (8)
Cu2—C31.846 (5)C11—C151.404 (7)
Cu3—C41.864 (6)C12—C131.362 (8)
Cu3—N32.081 (5)C13—C141.400 (8)
Cu3—N41.989 (5)C15—C161.434 (7)
N1—C21.155 (7)C5—H50.93
N2—C41.152 (7)C6—H60.93
N3—C51.328 (7)C7—H70.93
N3—C161.356 (7)C9—H90.93
N4—C141.327 (7)C10—H100.93
N4—C151.367 (7)C12—H120.93
C5—C61.396 (8)C13—H130.93
C6—C71.361 (9)C14—H140.93
C7—C81.412 (8)
C1—Cu1—N1126.0 (2)C15—C11—C10117.7 (5)
C1—Cu1—N2117.7 (2)C13—C12—C11118.8 (6)
N1—Cu1—N2116.2 (2)C12—C13—C14119.9 (6)
C2—Cu2—C3166.5 (2)N4—C14—C13122.7 (5)
C4—Cu3—N3118.7 (2)N4—C15—C11121.9 (5)
C4—Cu3—N4156.1 (2)N4—C15—C16117.7 (5)
N3—Cu3—N482.8 (2)C11—C15—C16120.4 (5)
C2—N1—Cu1176.2 (5)N3—C16—C8122.7 (5)
C4—N2—Cu1167.5 (4)N3—C16—C15117.3 (5)
C5—N3—C16118.3 (5)C8—C16—C15120.0 (5)
C5—N3—Cu3131.8 (4)N3—C5—H5118.5
C16—N3—Cu3109.9 (4)C6—C5—H5118.5
C14—N4—C15118.2 (5)C7—C6—H6120.6
C14—N4—Cu3129.6 (4)C5—C6—H6120.6
C15—N4—Cu3112.2 (4)C6—C7—H7119.9
N1—C2—Cu2176.4 (5)C8—C7—H7119.9
N2—C4—Cu3166.0 (5)C10—C9—H9119.1
N3—C5—C6123.1 (6)C8—C9—H9119.1
C7—C6—C5118.8 (6)C9—C10—H10119.4
C6—C7—C8120.2 (5)C11—C10—H10119.4
C16—C8—C7116.9 (5)C13—C12—H12120.6
C16—C8—C9118.9 (5)C11—C12—H12120.6
C7—C8—C9124.2 (5)C12—C13—H13120.1
C10—C9—C8121.7 (6)C14—C13—H13120.1
C9—C10—C11121.3 (5)N4—C14—H14118.6
C12—C11—C15118.4 (5)C13—C14—H14118.6
C12—C11—C10123.8 (5)
Cu2i—Cu1—N2—C475 (2)C11—C12—C13—C141.1 (8)
C4—Cu3—N3—C514.1 (6)C15—N4—C14—C131.1 (7)
N4—Cu3—N3—C5177.1 (5)Cu3—N4—C14—C13177.2 (4)
C4—Cu3—N3—C16165.9 (3)C12—C13—C14—N41.5 (8)
N4—Cu3—N3—C163.0 (3)C14—N4—C15—C110.4 (7)
C4—Cu3—N4—C1424.4 (7)Cu3—N4—C15—C11177.1 (4)
N3—Cu3—N4—C14179.7 (4)C14—N4—C15—C16179.8 (4)
C4—Cu3—N4—C15151.8 (5)Cu3—N4—C15—C163.6 (5)
N3—Cu3—N4—C153.5 (3)C12—C11—C15—N40.0 (7)
N4—Cu3—C4—N2105 (2)C10—C11—C15—N4178.9 (4)
N3—Cu3—C4—N247 (2)C12—C11—C15—C16179.4 (4)
C16—N3—C5—C60.2 (8)C10—C11—C15—C160.4 (7)
Cu3—N3—C5—C6179.8 (4)C5—N3—C16—C81.4 (7)
N3—C5—C6—C71.4 (9)Cu3—N3—C16—C8178.5 (4)
C5—C6—C7—C81.0 (8)C5—N3—C16—C15178.1 (4)
C6—C7—C8—C160.6 (7)Cu3—N3—C16—C151.9 (5)
C6—C7—C8—C9179.2 (5)C7—C8—C16—N31.8 (7)
C16—C8—C9—C100.9 (8)C9—C8—C16—N3179.5 (4)
C7—C8—C9—C10177.7 (5)C7—C8—C16—C15177.7 (4)
C8—C9—C10—C110.5 (8)C9—C8—C16—C151.0 (7)
C9—C10—C11—C12179.1 (5)N4—C15—C16—N31.0 (6)
C9—C10—C11—C150.2 (8)C11—C15—C16—N3179.6 (4)
C15—C11—C12—C130.4 (8)N4—C15—C16—C8178.5 (4)
C10—C11—C12—C13178.5 (5)C11—C15—C16—C80.8 (7)
Symmetry code: (i) x1, y, z.
 

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