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The title complex, [Cu(C32H28N2)2]I3, contains cations having CuI coordinated by four N atoms of two N,N′-bis­(3,3-diphenyl­prop-2-enyl­idene)ethane-1,2-diamine (Phca2en) ligands in a distorted tetra­hedral fashion and isolated linear I3 anions. The Phca2en ligand adopts a Z,Z conformation and acts as a bidentate ligand coordinating via two N atoms to the Cu atom. The Cu and central I atoms are located on twofold axes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806044916/ng2135sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806044916/ng2135Isup2.hkl
Contains datablock I

CCDC reference: 630180

Key indicators

  • Single-crystal X-ray study
  • T = 180 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.032
  • wR factor = 0.069
  • Data-to-parameter ratio = 28.7

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.61 Ratio
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.63 PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.09 Ratio
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 0.628 Tmax scaled 0.516 Tmin scaled 0.426 REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 32.01 From the CIF: _reflns_number_total 4735 Count of symmetry unique reflns 2686 Completeness (_total/calc) 176.28% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 2049 Fraction of Friedel pairs measured 0.763 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 3 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 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Bis[N,N'-bis(3,3-diphenylprop-2-enylidene)ethane-1,2-diamine-κ2N,N']copper(I) triiodide top
Crystal data top
[Cu(C32H28N2)2]I3Dx = 1.558 Mg m3
Mr = 1325.38Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4n2Cell parameters from 11035 reflections
Hall symbol: P -4 -2nθ = 2.7–32.0°
a = 17.1304 (7) ŵ = 2.07 mm1
c = 9.6273 (4) ÅT = 180 K
V = 2825.1 (2) Å3Prism, dark red
Z = 20.4 × 0.38 × 0.32 mm
F(000) = 1312
Data collection top
Oxford XCALIBUR
diffractometer
4735 independent reflections
Radiation source: fine-focus sealed tube3587 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
Detector resolution: 8.2632 pixels mm-1θmax = 32.0°, θmin = 2.7°
φ and ω scansh = 2425
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2006)
k = 2524
Tmin = 0.678, Tmax = 0.821l = 1313
29420 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.032H-atom parameters constrained
wR(F2) = 0.069 w = 1/[σ2(Fo2) + (0.0211P)2 + 1.9967P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max < 0.001
4735 reflectionsΔρmax = 1.04 e Å3
165 parametersΔρmin = 0.73 e Å3
0 restraintsAbsolute structure: Flack (1983) and Bernardinelli & Flack (1985), using 2109 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.031 (18)
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
C10.10339 (13)0.37530 (14)0.1759 (3)0.0367 (6)
H1A0.10950.31840.16160.044*
H1B0.13830.40280.11000.044*
C110.02211 (14)0.34988 (14)0.0877 (3)0.0271 (5)
H110.00260.29990.06280.033*
C120.10134 (13)0.37033 (13)0.0531 (2)0.0274 (5)
H120.11510.42400.05550.033*
C130.15754 (12)0.31876 (12)0.0176 (2)0.0236 (5)
C1310.14578 (14)0.23369 (14)0.0368 (3)0.0252 (5)
C1320.11750 (15)0.20465 (15)0.1617 (3)0.0319 (5)
H1320.10570.23970.23540.038*
C1330.10618 (18)0.12488 (16)0.1803 (3)0.0397 (7)
H1330.08680.10550.26620.048*
C1340.12333 (19)0.07372 (16)0.0727 (3)0.0432 (7)
H1340.11540.01920.08430.052*
C1350.15180 (19)0.10206 (17)0.0506 (3)0.0367 (7)
H1350.16350.06680.12380.044*
C1360.16364 (14)0.18091 (15)0.0697 (3)0.0289 (5)
H1360.18400.19950.15540.035*
C1410.23381 (15)0.34646 (15)0.0324 (3)0.0294 (5)
C1420.30174 (16)0.3029 (2)0.0094 (3)0.0423 (6)
H1420.29870.25280.03270.051*
C1430.3736 (2)0.3332 (3)0.0484 (5)0.0687 (15)
H1430.41950.30350.03230.082*
C1440.3795 (3)0.4043 (3)0.1091 (5)0.0850 (18)
H1440.42930.42490.13260.102*
C1450.3133 (3)0.4465 (2)0.1362 (4)0.0736 (14)
H1450.31740.49590.18040.088*
C1460.2405 (2)0.41798 (18)0.0998 (3)0.0466 (8)
H1460.19500.44730.12090.056*
N10.02260 (11)0.39815 (11)0.1515 (2)0.0246 (4)
Cu10.00000.50000.25000.02255 (9)
I10.00000.50000.75000.04172 (8)
I20.120456 (12)0.379544 (12)0.75000.06406 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0203 (11)0.0235 (12)0.0664 (16)0.0043 (10)0.0029 (10)0.0112 (11)
C110.0256 (11)0.0177 (10)0.0380 (13)0.0004 (8)0.0015 (9)0.0054 (9)
C120.0292 (11)0.0202 (10)0.0327 (11)0.0004 (9)0.0030 (9)0.0029 (9)
C130.0256 (10)0.0221 (10)0.0231 (10)0.0006 (9)0.0010 (8)0.0030 (8)
C1310.0217 (10)0.0240 (11)0.0298 (11)0.0057 (9)0.0036 (9)0.0026 (9)
C1320.0380 (14)0.0307 (12)0.0271 (12)0.0040 (11)0.0018 (11)0.0007 (10)
C1330.0483 (17)0.0347 (14)0.0362 (14)0.0007 (12)0.0022 (12)0.0127 (11)
C1340.0538 (18)0.0224 (12)0.0534 (18)0.0035 (12)0.0163 (15)0.0073 (12)
C1350.0412 (16)0.0259 (13)0.0431 (16)0.0102 (13)0.0096 (13)0.0082 (12)
C1360.0272 (12)0.0280 (12)0.0315 (12)0.0067 (10)0.0015 (10)0.0027 (10)
C1410.0298 (12)0.0323 (12)0.0262 (11)0.0042 (10)0.0041 (10)0.0101 (10)
C1420.0287 (14)0.063 (2)0.0355 (13)0.0025 (12)0.0010 (12)0.0163 (14)
C1430.0289 (17)0.123 (4)0.055 (2)0.016 (2)0.0049 (15)0.047 (3)
C1440.059 (3)0.122 (4)0.075 (3)0.058 (3)0.038 (2)0.059 (3)
C1450.095 (3)0.059 (2)0.067 (2)0.046 (2)0.049 (2)0.0301 (19)
C1460.061 (2)0.0331 (15)0.0451 (16)0.0114 (14)0.0251 (15)0.0098 (12)
N10.0206 (9)0.0205 (9)0.0326 (10)0.0005 (7)0.0008 (8)0.0021 (8)
Cu10.01616 (12)0.01616 (12)0.0353 (2)0.00021 (17)0.0000.000
I10.04703 (12)0.04703 (12)0.03111 (14)0.00530 (14)0.0000.000
I20.07092 (13)0.07092 (13)0.05035 (15)0.01943 (15)0.00613 (19)0.00613 (19)
Geometric parameters (Å, º) top
C1—N11.457 (3)C134—H1340.9500
C1—C1i1.518 (6)C135—C1361.378 (4)
C1—H1A0.9900C135—H1350.9500
C1—H1B0.9900C136—H1360.9500
C11—N11.284 (3)C141—C1461.391 (4)
C11—C121.441 (3)C141—C1421.400 (4)
C11—H110.9500C142—C1431.388 (5)
C12—C131.351 (3)C142—H1420.9500
C12—H120.9500C143—C1441.355 (8)
C13—C1411.471 (3)C143—H1430.9500
C13—C1311.483 (3)C144—C1451.369 (7)
C131—C1321.389 (4)C144—H1440.9500
C131—C1361.401 (3)C145—C1461.385 (5)
C132—C1331.392 (4)C145—H1450.9500
C132—H1320.9500C146—H1460.9500
C133—C1341.389 (4)N1—Cu12.0232 (19)
C133—H1330.9500Cu1—N1ii2.0232 (19)
C134—C1351.371 (5)I1—I22.9182 (3)
N1—C1—C1i108.37 (18)C131—C136—H136119.9
N1—C1—H1A110.0C146—C141—C142118.3 (3)
N1—C1—H1B110.0C146—C141—C13120.7 (3)
H1A—C1—H1B108.4C142—C141—C13121.0 (2)
N1—C11—C12121.1 (2)C143—C142—C141119.7 (4)
N1—C11—H11119.5C143—C142—H142120.2
C12—C11—H11119.5C141—C142—H142120.2
C13—C12—C11124.8 (2)C144—C143—C142121.3 (4)
C13—C12—H12117.6C144—C143—H143119.4
C11—C12—H12117.6C142—C143—H143119.4
C12—C13—C141120.3 (2)C143—C144—C145119.6 (3)
C12—C13—C131121.0 (2)C143—C144—H144120.2
C141—C13—C131118.6 (2)C145—C144—H144120.2
C132—C131—C136118.6 (2)C144—C145—C146120.8 (4)
C132—C131—C13120.5 (2)C144—C145—H145119.6
C136—C131—C13120.9 (2)C146—C145—H145119.6
C131—C132—C133120.8 (3)C145—C146—C141120.2 (4)
C131—C132—H132119.6C145—C146—H146119.9
C133—C132—H132119.6C141—C146—H146119.9
C134—C133—C132119.6 (3)C11—N1—C1118.1 (2)
C134—C133—H133120.2C11—N1—Cu1131.74 (17)
C132—C133—H133120.2C1—N1—Cu1109.75 (14)
C135—C134—C133119.8 (3)N1—Cu1—N1ii123.35 (11)
C135—C134—H134120.1N1—Cu1—N1i83.67 (11)
C133—C134—H134120.1N1ii—Cu1—N1i124.09 (12)
C134—C135—C136121.0 (3)N1—Cu1—N1iii124.09 (12)
C134—C135—H135119.5N1ii—Cu1—N1iii83.67 (11)
C136—C135—H135119.5N1i—Cu1—N1iii123.35 (11)
C135—C136—C131120.2 (3)I2iii—I1—I2180.0
C135—C136—H136119.9
Symmetry codes: (i) y1/2, x+1/2, z+1/2; (ii) y+1/2, x+1/2, z+1/2; (iii) x, y+1, z.
 

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