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The crystal structure of the centrosymmetric title compound, fully described by the name catena-poly[[(1,10-phenanthroline-κ
2N,
N′)cupriocyano]copper(I)]-μ-cyano-[[(1,10-phenanthroline-κ
2N,
N′)cupriocyano]copper(I)]-μ-cyano-copper(I)-μ-cyano-copper(II)-μ-cyano], [Cu
3(CN)
3(C
12H
8N
2)]
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
CCDC reference: 620744
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (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
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 = 448.88 | Dx = 1.992 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 9184 reflections |
a = 6.790 (1) Å | θ = 3.2–27.5° |
b = 24.642 (5) Å | µ = 4.23 mm−1 |
c = 18.136 (4) Å | T = 295 K |
β = 99.43 (3)° | Block, brown |
V = 2993.5 (10) Å3 | 0.22 × 0.18 × 0.16 mm |
Z = 8 | |
Data collection top
Rigaku R-AXIS RAPID IP diffractometer | 3430 independent reflections |
Radiation source: fine-focus sealed tube | 2232 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.111 |
ω scans | θmax = 27.5°, θmin = 3.2° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −8→8 |
Tmin = 0.441, Tmax = 0.551 | k = −32→31 |
14429 measured reflections | l = −23→23 |
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)] = 0.060 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.171 | H-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 parameters | Δρmax = 0.67 e Å−3 |
0 restraints | Δρmin = −0.85 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
Cu1 | 0.63781 (10) | 0.57896 (3) | 0.44086 (4) | 0.0441 (2) | |
Cu2 | 1.25966 (10) | 0.57965 (3) | 0.33521 (4) | 0.0488 (3) | |
Cu3 | 0.32909 (11) | 0.75378 (3) | 0.37598 (4) | 0.0476 (3) | |
N1 | 0.8872 (8) | 0.5811 (2) | 0.4048 (3) | 0.043 (1) | 0.50 |
N2 | 0.4894 (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 |
N3 | 0.2494 (6) | 0.7579 (2) | 0.2603 (3) | 0.042 (1) | |
N4 | 0.3139 (6) | 0.8342 (2) | 0.3678 (2) | 0.039 (1) | |
C1 | 0.5316 (8) | 0.5185 (2) | 0.4856 (3) | 0.051 (1) | 0.50 |
C2 | 1.0338 (8) | 0.5801 (2) | 0.3803 (3) | 0.044 (1) | 0.50 |
C3 | 1.4428 (7) | 0.5744 (2) | 0.2707 (3) | 0.045 (1) | 0.50 |
C4 | 0.4135 (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 |
C5 | 0.2110 (8) | 0.7196 (2) | 0.2086 (3) | 0.049 (1) | |
C6 | 0.1585 (8) | 0.7309 (3) | 0.1324 (4) | 0.050 (2) | |
C7 | 0.1502 (8) | 0.7836 (3) | 0.1097 (3) | 0.047 (1) | |
C8 | 0.1911 (7) | 0.8258 (2) | 0.1627 (3) | 0.039 (1) | |
C9 | 0.1837 (8) | 0.8820 (3) | 0.1444 (3) | 0.047 (1) | |
C10 | 0.2175 (8) | 0.9205 (2) | 0.1970 (3) | 0.045 (1) | |
C11 | 0.2650 (7) | 0.9065 (2) | 0.2760 (3) | 0.041 (1) | |
C12 | 0.2992 (7) | 0.9450 (2) | 0.3337 (3) | 0.046 (1) | |
C13 | 0.3381 (8) | 0.9273 (2) | 0.4058 (4) | 0.047 (1) | |
C14 | 0.3467 (7) | 0.8716 (2) | 0.4210 (3) | 0.041 (1) | |
C15 | 0.2736 (7) | 0.8512 (2) | 0.2951 (3) | 0.035 (1) | |
C16 | 0.2376 (7) | 0.8105 (2) | 0.2380 (3) | 0.035 (1) | |
H5 | 0.2194 | 0.6835 | 0.2237 | 0.058* | |
H6 | 0.1298 | 0.7029 | 0.0979 | 0.060* | |
H7 | 0.1174 | 0.7919 | 0.0592 | 0.056* | |
H9 | 0.1547 | 0.8923 | 0.0944 | 0.056* | |
H10 | 0.2104 | 0.9568 | 0.1830 | 0.054* | |
H12 | 0.2954 | 0.9819 | 0.3229 | 0.055* | |
H13 | 0.3589 | 0.9522 | 0.4448 | 0.056* | |
H14 | 0.3766 | 0.8603 | 0.4705 | 0.050* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0497 (4) | 0.0384 (4) | 0.0460 (4) | −0.0011 (3) | 0.0138 (3) | 0.0002 (3) |
Cu2 | 0.0466 (4) | 0.0517 (5) | 0.0516 (5) | −0.0013 (3) | 0.0183 (4) | −0.0004 (3) |
Cu3 | 0.0483 (4) | 0.0442 (5) | 0.0503 (5) | 0.0038 (3) | 0.0082 (3) | 0.0130 (3) |
N1 | 0.052 (3) | 0.031 (3) | 0.047 (3) | −0.006 (2) | 0.013 (3) | −0.002 (2) |
N2 | 0.043 (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) |
N3 | 0.036 (2) | 0.042 (3) | 0.048 (3) | 0.000 (2) | 0.008 (2) | −0.001 (2) |
N4 | 0.033 (2) | 0.044 (3) | 0.043 (3) | 0.003 (2) | 0.012 (2) | 0.002 (2) |
C1 | 0.050 (3) | 0.040 (3) | 0.069 (4) | 0.009 (2) | 0.028 (3) | 0.008 (3) |
C2 | 0.050 (3) | 0.043 (3) | 0.040 (3) | −0.003 (2) | 0.009 (2) | −0.003 (2) |
C3 | 0.045 (3) | 0.048 (3) | 0.042 (3) | −0.004 (2) | 0.006 (2) | 0.001 (2) |
C4 | 0.051 (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) |
C5 | 0.052 (3) | 0.037 (3) | 0.056 (4) | 0.000 (3) | 0.007 (3) | −0.005 (3) |
C6 | 0.042 (3) | 0.048 (4) | 0.058 (4) | 0.000 (3) | 0.005 (3) | −0.016 (3) |
C7 | 0.038 (3) | 0.064 (4) | 0.037 (3) | 0.010 (3) | 0.003 (2) | −0.005 (3) |
C8 | 0.028 (2) | 0.052 (3) | 0.037 (3) | 0.003 (2) | 0.010 (2) | 0.002 (3) |
C9 | 0.039 (3) | 0.055 (4) | 0.047 (3) | 0.001 (3) | 0.012 (2) | 0.013 (3) |
C10 | 0.042 (3) | 0.041 (3) | 0.054 (4) | 0.004 (2) | 0.016 (3) | 0.011 (3) |
C11 | 0.031 (3) | 0.038 (3) | 0.052 (3) | 0.004 (2) | 0.008 (2) | 0.009 (3) |
C12 | 0.036 (3) | 0.040 (3) | 0.059 (4) | 0.002 (2) | 0.005 (3) | −0.003 (3) |
C13 | 0.038 (3) | 0.048 (4) | 0.054 (4) | −0.002 (2) | 0.006 (3) | −0.014 (3) |
C14 | 0.034 (3) | 0.047 (3) | 0.044 (3) | 0.002 (2) | 0.009 (2) | −0.005 (3) |
C15 | 0.025 (2) | 0.041 (3) | 0.040 (3) | 0.007 (2) | 0.010 (2) | 0.005 (2) |
C16 | 0.029 (2) | 0.039 (3) | 0.041 (3) | 0.004 (2) | 0.015 (2) | 0.003 (2) |
Geometric parameters (Å, º) top
Cu1—C1 | 1.895 (5) | C8—C16 | 1.402 (7) |
Cu1—N1 | 1.913 (6) | C8—C9 | 1.425 (8) |
Cu1—N2 | 1.935 (5) | C9—C10 | 1.338 (8) |
Cu1—Cu2i | 2.941 (1) | C10—C11 | 1.456 (8) |
Cu2—C2 | 1.852 (6) | C11—C12 | 1.403 (8) |
Cu2—C3 | 1.846 (5) | C11—C15 | 1.404 (7) |
Cu3—C4 | 1.864 (6) | C12—C13 | 1.362 (8) |
Cu3—N3 | 2.081 (5) | C13—C14 | 1.400 (8) |
Cu3—N4 | 1.989 (5) | C15—C16 | 1.434 (7) |
N1—C2 | 1.155 (7) | C5—H5 | 0.93 |
N2—C4 | 1.152 (7) | C6—H6 | 0.93 |
N3—C5 | 1.328 (7) | C7—H7 | 0.93 |
N3—C16 | 1.356 (7) | C9—H9 | 0.93 |
N4—C14 | 1.327 (7) | C10—H10 | 0.93 |
N4—C15 | 1.367 (7) | C12—H12 | 0.93 |
C5—C6 | 1.396 (8) | C13—H13 | 0.93 |
C6—C7 | 1.361 (9) | C14—H14 | 0.93 |
C7—C8 | 1.412 (8) | | |
| | | |
C1—Cu1—N1 | 126.0 (2) | C15—C11—C10 | 117.7 (5) |
C1—Cu1—N2 | 117.7 (2) | C13—C12—C11 | 118.8 (6) |
N1—Cu1—N2 | 116.2 (2) | C12—C13—C14 | 119.9 (6) |
C2—Cu2—C3 | 166.5 (2) | N4—C14—C13 | 122.7 (5) |
C4—Cu3—N3 | 118.7 (2) | N4—C15—C11 | 121.9 (5) |
C4—Cu3—N4 | 156.1 (2) | N4—C15—C16 | 117.7 (5) |
N3—Cu3—N4 | 82.8 (2) | C11—C15—C16 | 120.4 (5) |
C2—N1—Cu1 | 176.2 (5) | N3—C16—C8 | 122.7 (5) |
C4—N2—Cu1 | 167.5 (4) | N3—C16—C15 | 117.3 (5) |
C5—N3—C16 | 118.3 (5) | C8—C16—C15 | 120.0 (5) |
C5—N3—Cu3 | 131.8 (4) | N3—C5—H5 | 118.5 |
C16—N3—Cu3 | 109.9 (4) | C6—C5—H5 | 118.5 |
C14—N4—C15 | 118.2 (5) | C7—C6—H6 | 120.6 |
C14—N4—Cu3 | 129.6 (4) | C5—C6—H6 | 120.6 |
C15—N4—Cu3 | 112.2 (4) | C6—C7—H7 | 119.9 |
N1—C2—Cu2 | 176.4 (5) | C8—C7—H7 | 119.9 |
N2—C4—Cu3 | 166.0 (5) | C10—C9—H9 | 119.1 |
N3—C5—C6 | 123.1 (6) | C8—C9—H9 | 119.1 |
C7—C6—C5 | 118.8 (6) | C9—C10—H10 | 119.4 |
C6—C7—C8 | 120.2 (5) | C11—C10—H10 | 119.4 |
C16—C8—C7 | 116.9 (5) | C13—C12—H12 | 120.6 |
C16—C8—C9 | 118.9 (5) | C11—C12—H12 | 120.6 |
C7—C8—C9 | 124.2 (5) | C12—C13—H13 | 120.1 |
C10—C9—C8 | 121.7 (6) | C14—C13—H13 | 120.1 |
C9—C10—C11 | 121.3 (5) | N4—C14—H14 | 118.6 |
C12—C11—C15 | 118.4 (5) | C13—C14—H14 | 118.6 |
C12—C11—C10 | 123.8 (5) | | |
| | | |
Cu2i—Cu1—N2—C4 | −75 (2) | C11—C12—C13—C14 | 1.1 (8) |
C4—Cu3—N3—C5 | 14.1 (6) | C15—N4—C14—C13 | 1.1 (7) |
N4—Cu3—N3—C5 | −177.1 (5) | Cu3—N4—C14—C13 | 177.2 (4) |
C4—Cu3—N3—C16 | −165.9 (3) | C12—C13—C14—N4 | −1.5 (8) |
N4—Cu3—N3—C16 | 3.0 (3) | C14—N4—C15—C11 | −0.4 (7) |
C4—Cu3—N4—C14 | −24.4 (7) | Cu3—N4—C15—C11 | −177.1 (4) |
N3—Cu3—N4—C14 | −179.7 (4) | C14—N4—C15—C16 | −179.8 (4) |
C4—Cu3—N4—C15 | 151.8 (5) | Cu3—N4—C15—C16 | 3.6 (5) |
N3—Cu3—N4—C15 | −3.5 (3) | C12—C11—C15—N4 | 0.0 (7) |
N4—Cu3—C4—N2 | −105 (2) | C10—C11—C15—N4 | −178.9 (4) |
N3—Cu3—C4—N2 | 47 (2) | C12—C11—C15—C16 | 179.4 (4) |
C16—N3—C5—C6 | −0.2 (8) | C10—C11—C15—C16 | 0.4 (7) |
Cu3—N3—C5—C6 | 179.8 (4) | C5—N3—C16—C8 | −1.4 (7) |
N3—C5—C6—C7 | 1.4 (9) | Cu3—N3—C16—C8 | 178.5 (4) |
C5—C6—C7—C8 | −1.0 (8) | C5—N3—C16—C15 | 178.1 (4) |
C6—C7—C8—C16 | −0.6 (7) | Cu3—N3—C16—C15 | −1.9 (5) |
C6—C7—C8—C9 | −179.2 (5) | C7—C8—C16—N3 | 1.8 (7) |
C16—C8—C9—C10 | −0.9 (8) | C9—C8—C16—N3 | −179.5 (4) |
C7—C8—C9—C10 | 177.7 (5) | C7—C8—C16—C15 | −177.7 (4) |
C8—C9—C10—C11 | 0.5 (8) | C9—C8—C16—C15 | 1.0 (7) |
C9—C10—C11—C12 | −179.1 (5) | N4—C15—C16—N3 | −1.0 (6) |
C9—C10—C11—C15 | −0.2 (8) | C11—C15—C16—N3 | 179.6 (4) |
C15—C11—C12—C13 | −0.4 (8) | N4—C15—C16—C8 | 178.5 (4) |
C10—C11—C12—C13 | 178.5 (5) | C11—C15—C16—C8 | −0.8 (7) |
Symmetry code: (i) x−1, y, z. |
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