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The crystal structure of [Cu(C12H8N2)3][C(CN)3]2 is composed of discrete [Cu(phen)3]2+ cations (phen is 1,10-phenanthroline) and [C(CN)3]- anions. The CuII atom is octahedrally coordinated by the three phen ligands. As a consequence of the Jahn-Teller effect, the two axial Cu-N bonds of 2.219 (3) and 2.238 (3) Å are longer than the equatorial Cu-N bonds, which are in trans positions, paired in two couples of almost equal distance [2.066 (3)/2.050 (3) and 2.121 (3)/2.121 (3) Å].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802017610/bt6193sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802017610/bt6193Isup2.hkl
Contains datablock I

CCDC reference: 198320

Key indicators

  • Single-crystal X-ray study
  • T = 220 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.044
  • wR factor = 0.152
  • Data-to-parameter ratio = 13.4

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
DIFF_020 Alert A _diffrn_standards_interval_count and _diffrn_standards_interval_time are missing. Number of measurements between standards or time (min) between standards.
Author response: At IPDS area detector systems no standard reflections are measured. The mean intensities of the records showed no significant decay.
DIFF_022  Alert A _diffrn_standards_decay_% is missing
          Percentage decrease in standards intensity.
Author response: See above.

Yellow Alert Alert Level C:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 26.00 From the CIF: _reflns_number_total 6872 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 7364 Completeness (_total/calc) 93.32% Alert C: < 95% complete PLAT_371 Alert C Long C(sp2)-C(sp1) Bond C(6) - C(8) = 1.42 Ang.
2 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check

Comment top

The structure of the five-coordinated CuII complex [Cu(L)2C(CN)3]C(CN)3 (L = 2,2'-bipyridine) is known (Potočňák et al., 1997). During an attempt to prepare the analogous complex with L = 1,10-phenanthroline (phen), the hexacoordinated CuII complex [Cu(phen)3][C(CN)3]2, (I), was isolated. We present here the structure of (I).

Experimental top

Crystals of (I) were prepared by mixing a 0.1 M aqueous solution of Cu(NO3)2 (5 ml) with 0.1 M ethanol solution of phen (10 ml). To the resulting blue solution, a 0.1 M aqueous ethanol solution of KC(CN)3 (5 ml) was added (all solutions were warmed up before mixing). Light-green dendritic crystals appeared within one week. The crystals were filtered off and dissolved in a warm mixture of ethanol and water (1:1). After one week, light-green prismatic crystals of (I) were filtered off and dried in air.

Refinement top

The H-atom positions were placed in calculated positions and refined riding on their parent C atoms, with C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: EXPOSE in IPDS (Stoe & Cie, 1999); cell refinement: CELL in IPDS; data reduction: INTEGRATE in IPDS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Crystal Impact, 1999); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The structure of (I) with the atom-labelling scheme. Displacement ellipsoids are drawn at the 40% probability level. H atoms have ben omitted for clarity.
Tris(2,2'-bipyridine)copper(II) tricyanomethanide top
Crystal data top
[Cu(C12H8N2)3](C4N3)2F(000) = 1604
Mr = 784.29Dx = 1.391 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 9.3854 (12) ÅCell parameters from 8000 reflections
b = 31.179 (5) Åθ = 1.7–26.0°
c = 12.7972 (18) ŵ = 0.63 mm1
β = 91.084 (16)°T = 220 K
V = 3744.2 (9) Å3Prism, light green
Z = 40.30 × 0.21 × 0.09 mm
Data collection top
Stoe IPDS
diffractometer
6872 independent reflections
Radiation source: fine-focus sealed tube4834 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.050
D = 70mm, Φ 0–199.5°, ΔΦ 1.5°, 7 min/rec scansθmax = 26.0°, θmin = 2.5°
Absorption correction: numerical
(FACE in IPDS; Stoe & Cie, 1999)
h = 1110
Tmin = 0.885, Tmax = 0.949k = 3838
19431 measured reflectionsl = 1515
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)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.152H-atom parameters constrained
S = 0.82 w = 1/[σ2(Fo2) + (0.113P)2 + 2.769P]
where P = (Fo2 + 2Fc2)/3
6872 reflections(Δ/σ)max < 0.001
514 parametersΔρmax = 0.31 e Å3
0 restraintsΔρmin = 0.62 e Å3
Crystal data top
[Cu(C12H8N2)3](C4N3)2V = 3744.2 (9) Å3
Mr = 784.29Z = 4
Monoclinic, P21/nMo Kα radiation
a = 9.3854 (12) ŵ = 0.63 mm1
b = 31.179 (5) ÅT = 220 K
c = 12.7972 (18) Å0.30 × 0.21 × 0.09 mm
β = 91.084 (16)°
Data collection top
Stoe IPDS
diffractometer
6872 independent reflections
Absorption correction: numerical
(FACE in IPDS; Stoe & Cie, 1999)
4834 reflections with I > 2σ(I)
Tmin = 0.885, Tmax = 0.949Rint = 0.050
19431 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0440 restraints
wR(F2) = 0.152H-atom parameters constrained
S = 0.82Δρmax = 0.31 e Å3
6872 reflectionsΔρmin = 0.62 e Å3
514 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R- factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu10.44541 (4)0.119748 (12)0.76875 (3)0.03013 (14)
N100.3267 (3)0.10209 (9)0.6235 (2)0.0361 (7)
C110.3361 (4)0.05927 (10)0.6026 (2)0.0324 (7)
C120.2512 (4)0.12650 (11)0.5574 (3)0.0440 (9)
H120.24360.15570.57150.053*
C130.1833 (5)0.11039 (13)0.4682 (3)0.0483 (9)
H130.13280.12860.42340.058*
C140.1915 (5)0.06733 (13)0.4471 (3)0.0487 (9)
H140.14620.05610.38780.058*
C150.2683 (4)0.04015 (11)0.5152 (3)0.0401 (8)
C160.2802 (5)0.00561 (12)0.5009 (3)0.0471 (9)
H160.23470.01840.44370.057*
C210.4175 (4)0.03290 (10)0.6752 (2)0.0329 (7)
C220.5561 (4)0.02874 (12)0.8261 (3)0.0466 (9)
H220.59830.04190.88420.056*
C230.5736 (5)0.01566 (14)0.8137 (3)0.0578 (11)
H230.62760.03130.86200.069*
C240.5105 (5)0.03578 (12)0.7297 (3)0.0507 (10)
H240.52150.06520.72040.061*
C250.4285 (4)0.01157 (11)0.6573 (3)0.0385 (8)
C260.3559 (4)0.03020 (11)0.5685 (3)0.0449 (9)
H260.36120.05960.55750.054*
N200.4824 (3)0.05278 (9)0.7591 (2)0.0363 (7)
N300.5430 (4)0.13074 (9)0.9274 (2)0.0437 (7)
C310.4416 (4)0.12791 (10)1.0028 (3)0.0363 (8)
C320.6729 (5)0.14309 (14)0.9570 (3)0.0543 (10)
H320.74250.14550.90660.065*
C330.7091 (5)0.15262 (15)1.0605 (4)0.0616 (12)
H330.80140.16131.07770.074*
C340.6099 (5)0.14928 (13)1.1369 (3)0.0570 (11)
H340.63410.15511.20630.068*
C350.4708 (4)0.13682 (11)1.1085 (3)0.0420 (9)
C360.3569 (5)0.13166 (12)1.1831 (3)0.0454 (9)
H360.37440.13811.25310.055*
C410.3006 (4)0.11503 (9)0.9697 (3)0.0344 (7)
C420.1457 (4)0.09612 (12)0.8347 (3)0.0415 (8)
H420.12760.09200.76380.050*
C430.0358 (4)0.08816 (13)0.9047 (3)0.0493 (10)
H430.05250.07850.88040.059*
C440.0595 (4)0.09474 (12)1.0087 (3)0.0479 (10)
H440.01290.08981.05590.057*
C450.1934 (4)0.10891 (11)1.0443 (3)0.0385 (8)
C460.2269 (5)0.11779 (11)1.1528 (3)0.0438 (9)
H460.15720.11381.20260.053*
N400.2747 (3)0.10927 (9)0.8651 (2)0.0371 (7)
N500.4161 (3)0.18702 (10)0.7561 (2)0.0436 (7)
C510.5298 (4)0.20586 (11)0.7088 (3)0.0403 (8)
C520.3156 (5)0.21187 (15)0.7938 (4)0.0623 (12)
H520.23860.19910.82630.075*
C530.3200 (7)0.25641 (18)0.7872 (4)0.0780 (15)
H530.24760.27280.81550.094*
C540.4306 (7)0.27568 (15)0.7391 (4)0.0760 (16)
H540.43360.30540.73430.091*
C550.5418 (5)0.25079 (12)0.6960 (4)0.0552 (11)
C560.6618 (6)0.26739 (14)0.6414 (5)0.0755 (15)
H560.66920.29680.63130.091*
C610.6402 (4)0.17860 (10)0.6713 (3)0.0379 (8)
C620.7279 (4)0.10951 (12)0.6566 (3)0.0431 (9)
H620.71910.08030.66970.052*
C630.8470 (5)0.12363 (14)0.6023 (4)0.0581 (11)
H630.91540.10430.58000.070*
C640.8606 (5)0.16669 (16)0.5827 (4)0.0650 (12)
H640.93800.17670.54550.078*
C650.7568 (5)0.19587 (13)0.6189 (3)0.0515 (10)
C660.7638 (6)0.24151 (15)0.6045 (4)0.0740 (15)
H660.84000.25330.56910.089*
N600.6265 (3)0.13556 (9)0.6904 (2)0.0355 (6)
C10.4404 (6)0.27457 (19)0.4003 (6)0.093 (2)
N10.4885 (7)0.30702 (18)0.3790 (8)0.165 (4)
C20.4598 (6)0.19691 (18)0.4206 (3)0.0613 (12)
N20.5258 (5)0.16503 (17)0.4164 (3)0.0770 (12)
C30.2365 (6)0.23314 (16)0.4546 (4)0.0694 (13)
N30.1188 (6)0.23246 (18)0.4802 (5)0.112 (2)
C40.3799 (5)0.23502 (15)0.4247 (3)0.0596 (11)
C50.1150 (4)0.07402 (15)0.7441 (3)0.0519 (10)
N50.1147 (5)0.10879 (14)0.7113 (3)0.0671 (10)
C60.1870 (5)0.02272 (17)0.8810 (3)0.0641 (12)
N60.2477 (6)0.01587 (19)0.9576 (4)0.1031 (18)
C70.0299 (5)0.00017 (14)0.7358 (3)0.0573 (12)
N70.0344 (5)0.02602 (13)0.6935 (3)0.0804 (14)
C80.1117 (4)0.03234 (14)0.7865 (3)0.0507 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0301 (3)0.0296 (2)0.0309 (2)0.00178 (16)0.00420 (15)0.00165 (15)
N100.0397 (19)0.0326 (14)0.0361 (15)0.0019 (13)0.0085 (12)0.0007 (11)
C110.032 (2)0.0324 (16)0.0333 (16)0.0035 (14)0.0076 (13)0.0027 (13)
C120.050 (3)0.0362 (18)0.046 (2)0.0025 (16)0.0122 (17)0.0036 (15)
C130.048 (3)0.053 (2)0.044 (2)0.0067 (18)0.0005 (17)0.0077 (16)
C140.049 (3)0.056 (2)0.041 (2)0.0022 (19)0.0058 (17)0.0000 (16)
C150.046 (2)0.0417 (18)0.0325 (17)0.0013 (16)0.0041 (15)0.0042 (14)
C160.062 (3)0.0424 (19)0.0373 (19)0.0062 (18)0.0029 (17)0.0117 (15)
C210.032 (2)0.0363 (16)0.0309 (16)0.0043 (14)0.0062 (13)0.0023 (13)
C220.054 (3)0.052 (2)0.0334 (18)0.0021 (18)0.0045 (16)0.0018 (15)
C230.070 (3)0.062 (2)0.042 (2)0.013 (2)0.0096 (19)0.0076 (18)
C240.063 (3)0.040 (2)0.049 (2)0.0092 (18)0.0022 (19)0.0055 (16)
C250.039 (2)0.0379 (17)0.0388 (18)0.0021 (15)0.0029 (15)0.0002 (14)
C260.056 (3)0.0345 (18)0.044 (2)0.0043 (17)0.0018 (17)0.0081 (15)
N200.0356 (18)0.0420 (16)0.0314 (14)0.0076 (13)0.0014 (12)0.0028 (11)
N300.041 (2)0.0384 (15)0.0519 (18)0.0016 (13)0.0101 (14)0.0069 (13)
C310.038 (2)0.0297 (16)0.0415 (18)0.0043 (14)0.0032 (15)0.0010 (13)
C320.038 (3)0.058 (2)0.067 (3)0.0035 (19)0.0095 (19)0.006 (2)
C330.039 (3)0.069 (3)0.077 (3)0.004 (2)0.007 (2)0.008 (2)
C340.056 (3)0.057 (2)0.058 (3)0.007 (2)0.011 (2)0.0080 (19)
C350.049 (3)0.0351 (17)0.0416 (19)0.0093 (16)0.0047 (16)0.0026 (14)
C360.059 (3)0.0432 (19)0.0346 (18)0.0141 (18)0.0005 (16)0.0006 (14)
C410.038 (2)0.0274 (16)0.0376 (17)0.0044 (14)0.0053 (14)0.0002 (13)
C420.035 (2)0.048 (2)0.0412 (19)0.0079 (16)0.0005 (15)0.0049 (15)
C430.037 (3)0.059 (2)0.053 (2)0.0117 (18)0.0078 (17)0.0028 (18)
C440.044 (3)0.054 (2)0.047 (2)0.0061 (18)0.0170 (17)0.0035 (17)
C450.044 (2)0.0344 (17)0.0372 (18)0.0042 (15)0.0086 (15)0.0043 (13)
C460.051 (3)0.0445 (19)0.0360 (18)0.0082 (18)0.0091 (16)0.0051 (15)
N400.045 (2)0.0350 (14)0.0320 (14)0.0012 (13)0.0071 (12)0.0014 (11)
N500.039 (2)0.0506 (17)0.0408 (17)0.0037 (14)0.0009 (13)0.0098 (13)
C510.045 (2)0.0356 (17)0.0406 (19)0.0034 (15)0.0076 (16)0.0057 (14)
C520.051 (3)0.072 (3)0.064 (3)0.018 (2)0.008 (2)0.009 (2)
C530.076 (4)0.075 (3)0.082 (4)0.032 (3)0.001 (3)0.017 (3)
C540.091 (5)0.043 (2)0.093 (4)0.021 (3)0.026 (3)0.010 (2)
C550.058 (3)0.0369 (19)0.070 (3)0.0032 (18)0.016 (2)0.0022 (18)
C560.085 (4)0.032 (2)0.108 (4)0.014 (2)0.007 (3)0.012 (2)
C610.042 (2)0.0343 (17)0.0368 (17)0.0075 (15)0.0006 (15)0.0033 (13)
C620.039 (2)0.0408 (19)0.050 (2)0.0050 (16)0.0063 (16)0.0056 (15)
C630.041 (3)0.059 (2)0.075 (3)0.000 (2)0.021 (2)0.001 (2)
C640.043 (3)0.073 (3)0.079 (3)0.014 (2)0.023 (2)0.007 (2)
C650.042 (3)0.049 (2)0.064 (3)0.0108 (18)0.0032 (19)0.0055 (18)
C660.064 (4)0.051 (3)0.107 (4)0.023 (2)0.006 (3)0.018 (3)
N600.0369 (18)0.0345 (14)0.0352 (15)0.0074 (12)0.0061 (12)0.0049 (11)
C10.056 (4)0.072 (3)0.154 (6)0.009 (3)0.042 (4)0.004 (3)
N10.097 (5)0.075 (3)0.326 (11)0.012 (3)0.111 (6)0.012 (5)
C20.055 (3)0.081 (3)0.048 (2)0.021 (3)0.006 (2)0.006 (2)
N20.068 (3)0.095 (3)0.068 (3)0.005 (3)0.004 (2)0.010 (2)
C30.050 (3)0.071 (3)0.087 (4)0.011 (2)0.006 (2)0.026 (3)
N30.059 (4)0.105 (4)0.174 (6)0.014 (3)0.026 (3)0.050 (4)
C40.048 (3)0.071 (3)0.059 (3)0.014 (2)0.009 (2)0.003 (2)
C50.033 (2)0.070 (3)0.052 (2)0.000 (2)0.0007 (17)0.021 (2)
N50.062 (3)0.067 (3)0.072 (3)0.010 (2)0.002 (2)0.008 (2)
C60.047 (3)0.089 (3)0.056 (3)0.015 (2)0.013 (2)0.017 (2)
N60.105 (4)0.135 (5)0.068 (3)0.014 (3)0.043 (3)0.011 (3)
C70.070 (3)0.050 (2)0.051 (2)0.014 (2)0.018 (2)0.0059 (19)
N70.105 (4)0.053 (2)0.081 (3)0.002 (2)0.049 (3)0.005 (2)
C80.041 (3)0.065 (3)0.045 (2)0.0111 (19)0.0082 (17)0.0127 (18)
Geometric parameters (Å, º) top
Cu1—N602.050 (3)C42—N401.330 (5)
Cu1—N402.066 (3)C42—C431.401 (5)
Cu1—N502.121 (3)C42—H420.9300
Cu1—N202.121 (3)C43—C441.360 (6)
Cu1—N102.219 (3)C43—H430.9300
Cu1—N302.238 (3)C44—C451.401 (6)
N10—C121.332 (5)C44—H440.9300
N10—C111.364 (4)C45—C461.444 (5)
C11—C151.409 (5)C46—H460.9300
C11—C211.448 (5)N50—C521.319 (5)
C12—C131.391 (6)N50—C511.370 (5)
C12—H120.9300C51—C551.415 (5)
C13—C141.372 (6)C51—C611.430 (5)
C13—H130.9300C52—C531.392 (7)
C14—C151.405 (5)C52—H520.9300
C14—H140.9300C53—C541.356 (8)
C15—C161.443 (5)C53—H530.9300
C16—C261.348 (5)C54—C551.421 (7)
C16—H160.9300C54—H540.9300
C21—N201.373 (4)C55—C561.433 (7)
C21—C251.409 (5)C56—C661.345 (7)
C22—N201.324 (5)C56—H560.9300
C22—C231.403 (6)C61—N601.370 (4)
C22—H220.9300C61—C651.402 (5)
C23—C241.370 (6)C62—N601.330 (5)
C23—H230.9300C62—C631.398 (6)
C24—C251.411 (5)C62—H620.9300
C24—H240.9300C63—C641.372 (6)
C25—C261.437 (5)C63—H630.9300
C26—H260.9300C64—C651.418 (6)
N30—C321.326 (5)C64—H640.9300
N30—C311.371 (5)C65—C661.437 (6)
C31—C351.403 (5)C66—H660.9300
C31—C411.439 (5)C1—N11.143 (7)
C32—C331.393 (6)C1—C41.395 (7)
C32—H320.9300C2—N21.173 (6)
C33—C341.367 (6)C2—C41.406 (7)
C33—H330.9300C3—N31.158 (7)
C34—C351.403 (6)C3—C41.408 (7)
C34—H340.9300C5—N51.162 (6)
C35—C361.455 (5)C5—C81.409 (6)
C36—C461.345 (6)C6—N61.144 (6)
C36—H360.9300C6—C81.421 (6)
C41—N401.367 (4)C7—N71.146 (6)
C41—C451.413 (5)C7—C81.413 (6)
N60—Cu1—N40171.67 (11)C35—C36—H36119.3
N60—Cu1—N5080.36 (12)N40—C41—C45121.9 (3)
N40—Cu1—N5095.79 (11)N40—C41—C31118.1 (3)
N60—Cu1—N2094.03 (11)C45—C41—C31120.1 (3)
N40—Cu1—N2090.50 (11)N40—C42—C43123.0 (3)
N50—Cu1—N20172.01 (11)N40—C42—H42118.5
N60—Cu1—N1093.31 (11)C43—C42—H42118.5
N40—Cu1—N1094.49 (11)C44—C43—C42119.3 (4)
N50—Cu1—N1096.84 (11)C44—C43—H43120.3
N20—Cu1—N1077.71 (10)C42—C43—H43120.3
N60—Cu1—N3094.49 (11)C43—C44—C45119.7 (3)
N40—Cu1—N3077.94 (12)C43—C44—H44120.2
N50—Cu1—N3088.17 (11)C45—C44—H44120.2
N20—Cu1—N3097.98 (11)C44—C45—C41118.0 (3)
N10—Cu1—N30171.35 (11)C44—C45—C46123.4 (3)
C12—N10—C11118.1 (3)C41—C45—C46118.6 (4)
C12—N10—Cu1130.0 (2)C36—C46—C45121.2 (3)
C11—N10—Cu1111.9 (2)C36—C46—H46119.4
N10—C11—C15122.6 (3)C45—C46—H46119.4
N10—C11—C21117.8 (3)C42—N40—C41118.1 (3)
C15—C11—C21119.6 (3)C42—N40—Cu1125.9 (2)
N10—C12—C13123.0 (3)C41—N40—Cu1116.0 (2)
N10—C12—H12118.5C52—N50—C51118.6 (4)
C13—C12—H12118.5C52—N50—Cu1130.2 (3)
C14—C13—C12119.3 (4)C51—N50—Cu1110.9 (2)
C14—C13—H13120.4N50—C51—C55122.7 (4)
C12—C13—H13120.4N50—C51—C61118.0 (3)
C13—C14—C15119.9 (4)C55—C51—C61119.3 (4)
C13—C14—H14120.1N50—C52—C53122.8 (5)
C15—C14—H14120.1N50—C52—H52118.6
C11—C15—C14117.1 (3)C53—C52—H52118.6
C11—C15—C16119.0 (3)C54—C53—C52119.6 (5)
C14—C15—C16123.9 (3)C54—C53—H53120.2
C26—C16—C15121.4 (3)C52—C53—H53120.2
C26—C16—H16119.3C53—C54—C55120.5 (4)
C15—C16—H16119.3C53—C54—H54119.7
N20—C21—C25122.6 (3)C55—C54—H54119.7
N20—C21—C11117.8 (3)C51—C55—C56118.6 (4)
C25—C21—C11119.6 (3)C51—C55—C54115.8 (4)
N20—C22—C23123.1 (3)C56—C55—C54125.6 (4)
N20—C22—H22118.5C66—C56—C55121.7 (4)
C23—C22—H22118.5C66—C56—H56119.1
C24—C23—C22119.4 (4)C55—C56—H56119.1
C24—C23—H23120.3N60—C61—C65122.6 (3)
C22—C23—H23120.3N60—C61—C51116.8 (3)
C23—C24—C25119.5 (4)C65—C61—C51120.6 (3)
C23—C24—H24120.3N60—C62—C63123.6 (3)
C25—C24—H24120.3N60—C62—H62118.2
C21—C25—C24117.4 (3)C63—C62—H62118.2
C21—C25—C26119.4 (3)C64—C63—C62118.5 (4)
C24—C25—C26123.2 (3)C64—C63—H63120.7
C16—C26—C25120.9 (3)C62—C63—H63120.7
C16—C26—H26119.5C63—C64—C65120.1 (4)
C25—C26—H26119.5C63—C64—H64120.0
C22—N20—C21118.0 (3)C65—C64—H64120.0
C22—N20—Cu1127.2 (2)C61—C65—C64117.2 (4)
C21—N20—Cu1114.8 (2)C61—C65—C66118.7 (4)
C32—N30—C31117.7 (3)C64—C65—C66124.1 (4)
C32—N30—Cu1131.4 (3)C56—C66—C65120.9 (4)
C31—N30—Cu1110.5 (3)C56—C66—H66119.5
N30—C31—C35122.7 (4)C65—C66—H66119.5
N30—C31—C41117.2 (3)C62—N60—C61118.0 (3)
C35—C31—C41120.1 (3)C62—N60—Cu1128.1 (2)
N30—C32—C33122.6 (4)C61—N60—Cu1113.9 (2)
N30—C32—H32118.7N1—C1—C4178.9 (10)
C33—C32—H32118.7N2—C2—C4179.5 (6)
C34—C33—C32120.4 (4)N3—C3—C4178.5 (7)
C34—C33—H33119.8C1—C4—C3119.5 (5)
C32—C33—H33119.8C1—C4—C2121.2 (5)
C33—C34—C35118.6 (4)C3—C4—C2119.2 (4)
C33—C34—H34120.7N5—C5—C8177.9 (5)
C35—C34—H34120.7N6—C6—C8178.6 (6)
C34—C35—C31117.9 (4)N7—C7—C8178.7 (6)
C34—C35—C36123.5 (3)C7—C8—C5119.6 (4)
C31—C35—C36118.5 (4)C7—C8—C6119.9 (4)
C46—C36—C35121.4 (3)C5—C8—C6120.5 (4)
C46—C36—H36119.3

Experimental details

Crystal data
Chemical formula[Cu(C12H8N2)3](C4N3)2
Mr784.29
Crystal system, space groupMonoclinic, P21/n
Temperature (K)220
a, b, c (Å)9.3854 (12), 31.179 (5), 12.7972 (18)
β (°) 91.084 (16)
V3)3744.2 (9)
Z4
Radiation typeMo Kα
µ (mm1)0.63
Crystal size (mm)0.30 × 0.21 × 0.09
Data collection
DiffractometerStoe IPDS
diffractometer
Absorption correctionNumerical
(FACE in IPDS; Stoe & Cie, 1999)
Tmin, Tmax0.885, 0.949
No. of measured, independent and
observed [I > 2σ(I)] reflections
19431, 6872, 4834
Rint0.050
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.044, 0.152, 0.82
No. of reflections6872
No. of parameters514
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.31, 0.62

Computer programs: EXPOSE in IPDS (Stoe & Cie, 1999), CELL in IPDS, INTEGRATE in IPDS, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), DIAMOND (Crystal Impact, 1999), SHELXL97.

Selected geometric parameters (Å, º) top
Cu1—N602.050 (3)C2—C41.406 (7)
Cu1—N402.066 (3)C3—N31.158 (7)
Cu1—N502.121 (3)C3—C41.408 (7)
Cu1—N202.121 (3)C5—N51.162 (6)
Cu1—N102.219 (3)C5—C81.409 (6)
Cu1—N302.238 (3)C6—N61.144 (6)
C1—N11.143 (7)C6—C81.421 (6)
C1—C41.395 (7)C7—N71.146 (6)
C2—N21.173 (6)C7—C81.413 (6)
N60—Cu1—N40171.67 (11)N10—Cu1—N30171.35 (11)
N60—Cu1—N5080.36 (12)N1—C1—C4178.9 (10)
N40—Cu1—N5095.79 (11)N2—C2—C4179.5 (6)
N60—Cu1—N2094.03 (11)N3—C3—C4178.5 (7)
N40—Cu1—N2090.50 (11)C1—C4—C3119.5 (5)
N50—Cu1—N20172.01 (11)C1—C4—C2121.2 (5)
N60—Cu1—N1093.31 (11)C3—C4—C2119.2 (4)
N40—Cu1—N1094.49 (11)N5—C5—C8177.9 (5)
N50—Cu1—N1096.84 (11)N6—C6—C8178.6 (6)
N20—Cu1—N1077.71 (10)N7—C7—C8178.7 (6)
N60—Cu1—N3094.49 (11)C7—C8—C5119.6 (4)
N40—Cu1—N3077.94 (12)C7—C8—C6119.9 (4)
N50—Cu1—N3088.17 (11)C5—C8—C6120.5 (4)
N20—Cu1—N3097.98 (11)
 

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