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The title compound, [CuI(dmtpy)(NCMe)](PF6) (dmtpy = 6,6''-dimesityl-2,2':6',2''-ter­pyridine) or [Cu(C2H3N)(C33H31N3)](PF6), displays a distorted square-planar coordination, with four N atoms from dmtpy and aceto­nitrile mol­ecules, as a result of the extremely bulky terpyridyl ligand.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803008249/ob6234sup1.cif
Contains datablocks General, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803008249/ob6234Isup2.hkl
Contains datablock I

CCDC reference: 214571

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.012 Å
  • R factor = 0.052
  • wR factor = 0.227
  • Data-to-parameter ratio = 17.2

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:
RINTA_01 Alert B The value of Rint is greater than 0.15 Rint given 0.150
Yellow Alert Alert Level C:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 7302 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 7890 Completeness (_total/calc) 92.55% Alert C: < 95% complete General Notes
ABSTM_02 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 0.863 Tmax scaled 0.861 Tmin scaled 0.727
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
1 Alert Level C = Please check

Comment top

Design of N-chelating ligands with various bulky substituents is essential approach in developing N-chelating metal catalysts for polymerization. For example, Johnson et al. (1995) have reported highly efficient Pd and Ni catalysts with α-diimino ligands for the polymerization of ethylene and α-olefin. It was also reported that the control of bulkiness in pyridine bisimino ligands (3 N coordination) contribute to polymerization by their Fe and Co catalysts (Small et al., 1998; Britovsek et al., 1998). Here, we determined the crystal structure of the title compound (I) to show the effect of the steric hindrance of the bulky terpyridine ligand 6,6''-dimesityl-2,2':6',2''-terpyridine (dmtpy), which perturbs the metal coordination geometry.

The Cu complex in (I) gives a distorted square planar coordination with four N atoms from dmtpy and acetonitrile molecules because of the extremely bulky terpyridyl ligand. The Cu1—N21 bond distance of 2.003 (5) Å for the central pyridine ring is shorter than those for the pyridine rings of the both side, 2.232 (5) Å and 2.244 (5) Å (Table 1). The Cu1 atom lies nearly on the plane of the central pyridine ring (C24···N21—Cu1, 176.8 (3)°). While, the Cu center aligned apart from the pyridine rings of the both side (C14···N11—Cu1, 155.7 (3)°, C34···N31—Cu1, 158.7 (3)°). The N21—Cu1—N1 bond angle is 152.8 (3)° and the Cu1 ion is located 0.625 (1) Å apart from the N11/N21/N31 plane. The bulkiness of dimesityl groups in the 6,6''- positions of terpyridine ligands distrupts the square planar coordination geometry forward to highly distorted tetrahedral one. Our ligand design of bulky derivatization in terpyridine ligands successfully induces a distortion in Cu(I) coordination geometry (Fig. 2).

Experimental top

To a solution of dmtpy (286 mg, 0.61 mmol) in tetrahydrofuran (12 ml) was added a solution of [Cu(NCMe)4](PF6) (226 mg, 0.61 mmol) in MeCN (5 ml) at room temperature. The reaction mixture was stirred for 10 min and dried in vacuo. The residue was recrystallized from MeCN/ether to give dark red crystals of (I). Yield: 26 mg (6.2%). Elemental analysis, calculated for C35H34CuF6N4P: C 58.45, H 4.77, N 7.79%; found: C 58.78, H 4.50, N 7.88%.

Computing details top

Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1991); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLEASE PROVIDE; software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The structure of the complex cation in (I), showing the labeling and 25% propability ellipsoids for non-H atoms.
[Figure 2] Fig. 2. CPK drawing of cation part structure of (I). Brown (Cu), purple (N) and black (C).
(I) top
Crystal data top
[Cu(C2H3N)(C33H31N3)](PF6)F(000) = 1480
Mr = 719.17Dx = 1.391 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71069 Å
a = 11.317 (3) ÅCell parameters from 25 reflections
b = 23.592 (4) Åθ = 29.2–30.0°
c = 12.873 (2) ŵ = 0.75 mm1
β = 92.450 (16)°T = 296 K
V = 3433.7 (11) Å3Block, dark red
Z = 40.50 × 0.30 × 0.20 mm
Data collection top
Rigaku AFC-5R
diffractometer
2104 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.150
Graphite monochromatorθmax = 27.5°, θmin = 2.5°
ω–2θ scansh = 013
Absorption correction: Ψ scan
(North, 1968)
k = 030
Tmin = 0.842, Tmax = 0.998l = 1616
7686 measured reflections3 standard reflections every 150 reflections
7302 independent reflections intensity decay: 0.2%
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) = 0.227H-atom parameters constrained
S = 0.91 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
7302 reflections(Δ/σ)max < 0.001
425 parametersΔρmax = 0.50 e Å3
0 restraintsΔρmin = 0.58 e Å3
Crystal data top
[Cu(C2H3N)(C33H31N3)](PF6)V = 3433.7 (11) Å3
Mr = 719.17Z = 4
Monoclinic, P21/nMo Kα radiation
a = 11.317 (3) ŵ = 0.75 mm1
b = 23.592 (4) ÅT = 296 K
c = 12.873 (2) Å0.50 × 0.30 × 0.20 mm
β = 92.450 (16)°
Data collection top
Rigaku AFC-5R
diffractometer
2104 reflections with I > 2σ(I)
Absorption correction: Ψ scan
(North, 1968)
Rint = 0.150
Tmin = 0.842, Tmax = 0.9983 standard reflections every 150 reflections
7686 measured reflections intensity decay: 0.2%
7302 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0520 restraints
wR(F2) = 0.227H-atom parameters constrained
S = 0.91Δρmax = 0.50 e Å3
7302 reflectionsΔρmin = 0.58 e Å3
425 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
Cu10.05468 (7)0.10159 (4)0.17286 (6)0.0525 (3)
P10.0440 (2)0.42579 (10)0.19005 (16)0.0636 (6)
F10.0048 (6)0.4646 (4)0.2806 (4)0.165 (3)
F20.0705 (7)0.3931 (5)0.1877 (6)0.227 (5)
F30.1021 (9)0.3872 (3)0.2710 (5)0.182 (4)
F40.0829 (6)0.3895 (2)0.0968 (4)0.121 (2)
F50.1619 (7)0.4580 (5)0.1919 (6)0.204 (4)
F60.0092 (8)0.4681 (3)0.1096 (5)0.179 (4)
N10.1947 (5)0.0958 (3)0.2571 (4)0.0665 (18)
N110.1095 (5)0.1199 (2)0.0108 (4)0.0430 (14)
N210.0775 (5)0.0687 (2)0.0837 (4)0.0448 (14)
N310.0997 (5)0.1041 (3)0.2751 (4)0.0522 (14)
C10.2767 (7)0.1005 (4)0.3073 (6)0.066 (2)
C20.3835 (8)0.1043 (4)0.3752 (7)0.100 (3)
H2A0.44840.08680.34160.120*
H2B0.37050.08500.43940.120*
H2C0.40160.14340.38900.120*
C120.0470 (6)0.0852 (3)0.0564 (5)0.0449 (17)
C130.0867 (6)0.0718 (3)0.1553 (5)0.0487 (18)
H130.04220.04870.20060.058*
C140.1931 (7)0.0937 (3)0.1829 (5)0.062 (2)
H140.22240.08450.24720.075*
C150.2573 (7)0.1291 (3)0.1164 (6)0.057 (2)
H150.32910.14430.13530.069*
C160.2114 (6)0.1416 (3)0.0200 (5)0.0459 (17)
C220.0676 (6)0.0652 (3)0.0190 (5)0.0434 (17)
C230.1594 (7)0.0453 (3)0.0831 (6)0.058 (2)
H230.15080.04260.15440.070*
C240.2635 (7)0.0295 (3)0.0404 (7)0.069 (2)
H240.32570.01550.08250.083*
C250.2751 (6)0.0345 (3)0.0657 (6)0.057 (2)
H250.34440.02350.09630.068*
C260.1806 (6)0.0564 (3)0.1253 (6)0.0502 (19)
C320.1853 (6)0.0693 (3)0.2398 (6)0.0521 (18)
C330.2717 (7)0.0479 (4)0.3003 (7)0.076 (2)
H330.32900.02300.27350.091*
C340.2692 (8)0.0653 (4)0.4045 (7)0.095 (3)
H340.32540.05160.44860.113*
C350.1872 (8)0.1013 (4)0.4405 (7)0.084 (3)
H350.18800.11380.50900.101*
C360.0989 (7)0.1205 (3)0.3752 (6)0.064 (2)
C410.2746 (6)0.1814 (3)0.0541 (5)0.0564 (19)
C420.3887 (7)0.1693 (4)0.0936 (6)0.066 (2)
C430.4444 (7)0.2095 (4)0.1593 (7)0.076 (3)
H430.52100.20240.18520.091*
C440.3908 (9)0.2583 (4)0.1866 (6)0.079 (3)
C450.2799 (8)0.2677 (4)0.1469 (7)0.077 (2)
H450.24200.30090.16560.093*
C460.2201 (7)0.2312 (3)0.0809 (6)0.062 (2)
C470.4515 (8)0.1136 (4)0.0687 (8)0.105 (3)
H47A0.52840.11310.10320.126*
H47B0.45960.11070.00500.126*
H47C0.40580.08230.09240.126*
C480.4586 (10)0.3010 (5)0.2525 (8)0.123 (4)
H48A0.40880.33290.26530.147*
H48B0.52670.31330.21680.147*
H48C0.48350.28380.31750.147*
C490.0995 (8)0.2489 (4)0.0354 (9)0.117 (4)
H49A0.06830.21940.00930.141*
H49B0.10730.28320.00400.141*
H49C0.04680.25530.09070.141*
C510.0073 (7)0.1608 (4)0.4120 (5)0.059 (2)
C520.0810 (8)0.1451 (4)0.4845 (6)0.079 (3)
C530.1665 (9)0.1871 (6)0.5163 (7)0.103 (4)
H530.22500.17750.56620.123*
C540.1652 (9)0.2405 (6)0.4760 (8)0.095 (3)
C550.0800 (9)0.2548 (4)0.4041 (7)0.086 (3)
H550.07900.29120.37630.103*
C560.0070 (7)0.2158 (4)0.3706 (6)0.069 (2)
C570.0887 (11)0.0851 (5)0.5281 (8)0.129 (4)
H57A0.15500.08240.57690.155*
H57B0.09860.05870.47230.155*
H57C0.01730.07640.56250.155*
C580.2561 (10)0.2856 (6)0.5135 (9)0.151 (5)
H58A0.31080.26910.56400.181*
H58B0.21570.31670.54460.181*
H58C0.29850.29910.45540.181*
C590.1021 (9)0.2362 (4)0.2920 (7)0.105 (3)
H59A0.08680.27480.27360.126*
H59B0.17820.23360.32200.126*
H59C0.10130.21290.23080.126*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0464 (5)0.0594 (6)0.0510 (5)0.0025 (5)0.0062 (4)0.0069 (5)
P10.0659 (15)0.0672 (14)0.0580 (14)0.0154 (12)0.0076 (11)0.0014 (12)
F10.171 (6)0.230 (8)0.090 (4)0.121 (6)0.035 (4)0.077 (5)
F20.154 (7)0.362 (13)0.171 (7)0.152 (8)0.079 (6)0.080 (8)
F30.283 (10)0.143 (6)0.119 (5)0.092 (7)0.027 (6)0.025 (5)
F40.155 (5)0.104 (4)0.109 (4)0.037 (4)0.048 (4)0.024 (3)
F50.146 (7)0.294 (11)0.171 (7)0.114 (7)0.003 (6)0.006 (8)
F60.289 (10)0.147 (6)0.096 (4)0.115 (7)0.051 (5)0.006 (4)
N10.049 (4)0.099 (5)0.051 (4)0.010 (4)0.002 (3)0.006 (4)
N110.044 (3)0.038 (3)0.047 (3)0.002 (3)0.002 (3)0.002 (3)
N210.040 (3)0.041 (3)0.054 (4)0.003 (3)0.002 (3)0.010 (3)
N310.057 (4)0.054 (4)0.046 (3)0.001 (3)0.005 (3)0.014 (3)
C10.052 (5)0.083 (6)0.063 (5)0.005 (5)0.002 (4)0.002 (5)
C20.084 (6)0.100 (7)0.111 (7)0.001 (6)0.040 (6)0.004 (6)
C120.052 (4)0.039 (4)0.043 (4)0.007 (3)0.002 (3)0.005 (3)
C130.067 (5)0.040 (4)0.038 (4)0.007 (4)0.007 (4)0.004 (3)
C140.083 (6)0.064 (6)0.042 (4)0.002 (5)0.022 (4)0.005 (4)
C150.067 (5)0.048 (5)0.059 (5)0.002 (4)0.020 (4)0.003 (4)
C160.048 (4)0.039 (4)0.051 (4)0.002 (3)0.003 (3)0.001 (3)
C220.043 (4)0.034 (4)0.053 (4)0.004 (3)0.005 (3)0.006 (3)
C230.057 (5)0.056 (5)0.060 (5)0.004 (4)0.015 (4)0.006 (4)
C240.056 (5)0.074 (6)0.076 (6)0.011 (4)0.015 (5)0.014 (5)
C250.038 (4)0.051 (5)0.080 (6)0.001 (3)0.008 (4)0.005 (4)
C260.045 (4)0.036 (4)0.070 (5)0.004 (3)0.006 (4)0.008 (3)
C320.043 (4)0.055 (5)0.059 (5)0.003 (4)0.012 (4)0.008 (4)
C330.061 (5)0.079 (6)0.089 (6)0.019 (5)0.023 (5)0.017 (5)
C340.086 (7)0.118 (8)0.083 (7)0.038 (6)0.048 (6)0.022 (6)
C350.091 (7)0.096 (7)0.069 (5)0.028 (6)0.033 (5)0.018 (5)
C360.061 (5)0.070 (6)0.063 (5)0.001 (4)0.015 (4)0.008 (4)
C410.056 (5)0.061 (5)0.053 (4)0.007 (4)0.015 (4)0.004 (4)
C420.049 (5)0.072 (6)0.076 (5)0.003 (4)0.000 (4)0.001 (5)
C430.047 (5)0.095 (7)0.084 (6)0.012 (5)0.010 (4)0.024 (6)
C440.094 (7)0.079 (7)0.065 (5)0.021 (6)0.004 (5)0.014 (5)
C450.076 (6)0.073 (6)0.084 (6)0.009 (5)0.008 (5)0.008 (5)
C460.056 (5)0.051 (5)0.080 (5)0.008 (4)0.001 (4)0.017 (4)
C470.072 (6)0.109 (9)0.134 (9)0.005 (6)0.001 (6)0.002 (7)
C480.151 (10)0.117 (9)0.098 (8)0.058 (8)0.018 (7)0.023 (7)
C490.090 (7)0.083 (7)0.176 (11)0.034 (6)0.028 (7)0.052 (7)
C510.067 (5)0.073 (6)0.039 (4)0.007 (5)0.012 (4)0.010 (4)
C520.100 (7)0.099 (8)0.038 (5)0.013 (6)0.003 (5)0.002 (5)
C530.082 (7)0.178 (12)0.046 (6)0.003 (8)0.017 (5)0.023 (7)
C540.083 (7)0.136 (11)0.066 (7)0.025 (7)0.007 (5)0.019 (7)
C550.091 (7)0.089 (7)0.077 (6)0.012 (6)0.005 (5)0.020 (5)
C560.070 (5)0.084 (7)0.052 (5)0.004 (5)0.003 (4)0.029 (5)
C570.148 (11)0.164 (13)0.074 (7)0.008 (9)0.013 (7)0.019 (7)
C580.107 (9)0.217 (15)0.128 (10)0.062 (9)0.005 (7)0.066 (10)
C590.120 (8)0.084 (7)0.108 (7)0.004 (6)0.039 (7)0.027 (6)
Geometric parameters (Å, º) top
Cu1—N11.886 (6)C35—C361.408 (11)
Cu1—N212.003 (5)C35—H350.9300
Cu1—N312.232 (5)C36—C511.471 (10)
Cu1—N112.244 (5)C41—C461.378 (10)
P1—F21.507 (7)C41—C421.396 (10)
P1—F31.512 (6)C42—C431.403 (11)
P1—F51.535 (7)C42—C471.534 (12)
P1—F61.542 (6)C43—C441.355 (12)
P1—F41.554 (5)C43—H430.9300
P1—F11.561 (5)C44—C451.353 (11)
N1—C11.114 (8)C44—C481.505 (11)
N11—C161.338 (8)C45—C461.369 (10)
N11—C121.367 (8)C45—H450.9300
N21—C221.333 (8)C46—C491.521 (11)
N21—C261.336 (8)C47—H47A0.9600
N31—C321.336 (8)C47—H47B0.9600
N31—C361.346 (9)C47—H47C0.9600
C1—C21.463 (10)C48—H48A0.9600
C2—H2A0.9600C48—H48B0.9600
C2—H2B0.9600C48—H48C0.9600
C2—H2C0.9600C49—H49A0.9600
C12—C131.403 (9)C49—H49B0.9600
C12—C221.480 (9)C49—H49C0.9600
C13—C141.372 (10)C51—C521.388 (11)
C13—H130.9300C51—C561.402 (11)
C14—C151.381 (10)C52—C531.433 (13)
C14—H140.9300C52—C571.524 (13)
C15—C161.397 (9)C53—C541.364 (15)
C15—H150.9300C53—H530.9300
C16—C411.497 (9)C54—C551.350 (12)
C22—C231.381 (9)C54—C581.543 (14)
C23—C241.372 (10)C55—C561.403 (11)
C23—H230.9300C55—H550.9300
C24—C251.383 (10)C56—C591.523 (11)
C24—H240.9300C57—H57A0.9600
C25—C261.389 (9)C57—H57B0.9600
C25—H250.9300C57—H57C0.9600
C26—C321.508 (10)C58—H58A0.9600
C32—C331.372 (10)C58—H58B0.9600
C33—C341.402 (11)C58—H58C0.9600
C33—H330.9300C59—H59A0.9600
C34—C351.327 (11)C59—H59B0.9600
C34—H340.9300C59—H59C0.9600
N1—Cu1—N21152.8 (3)C34—C35—H35120.0
N1—Cu1—N31108.8 (2)C36—C35—H35120.0
N21—Cu1—N3176.3 (2)N31—C36—C35120.2 (7)
N1—Cu1—N11106.8 (2)N31—C36—C51118.0 (7)
N21—Cu1—N1176.8 (2)C35—C36—C51121.7 (7)
N31—Cu1—N11142.9 (2)C46—C41—C42120.0 (7)
F2—P1—F393.1 (6)C46—C41—C16119.1 (7)
F2—P1—F5178.9 (7)C42—C41—C16120.9 (7)
F3—P1—F586.3 (5)C41—C42—C43117.8 (8)
F2—P1—F690.4 (6)C41—C42—C47121.9 (8)
F3—P1—F6176.2 (5)C43—C42—C47120.3 (8)
F5—P1—F690.2 (5)C44—C43—C42122.4 (8)
F2—P1—F488.5 (4)C44—C43—H43118.8
F3—P1—F494.1 (4)C42—C43—H43118.8
F5—P1—F490.6 (5)C45—C44—C43117.4 (8)
F6—P1—F487.3 (3)C45—C44—C48123.1 (10)
F2—P1—F192.5 (5)C43—C44—C48119.4 (10)
F3—P1—F188.2 (4)C44—C45—C46123.9 (9)
F5—P1—F188.4 (5)C44—C45—H45118.1
F6—P1—F190.4 (4)C46—C45—H45118.1
F4—P1—F1177.5 (4)C45—C46—C41118.5 (8)
C1—N1—Cu1170.2 (8)C45—C46—C49118.5 (8)
C16—N11—C12118.2 (6)C41—C46—C49122.8 (7)
C16—N11—Cu1128.7 (4)C42—C47—H47A109.5
C12—N11—Cu1108.5 (4)C42—C47—H47B109.5
C22—N21—C26119.7 (6)H47A—C47—H47B109.5
C22—N21—Cu1120.0 (4)C42—C47—H47C109.5
C26—N21—Cu1119.9 (5)H47A—C47—H47C109.5
C32—N31—C36118.5 (6)H47B—C47—H47C109.5
C32—N31—Cu1111.0 (4)C44—C48—H48A109.5
C36—N31—Cu1126.8 (5)C44—C48—H48B109.5
N1—C1—C2177.6 (10)H48A—C48—H48B109.5
C1—C2—H2A109.5C44—C48—H48C109.5
C1—C2—H2B109.5H48A—C48—H48C109.5
H2A—C2—H2B109.5H48B—C48—H48C109.5
C1—C2—H2C109.5C46—C49—H49A109.5
H2A—C2—H2C109.5C46—C49—H49B109.5
H2B—C2—H2C109.5H49A—C49—H49B109.5
N11—C12—C13122.1 (6)C46—C49—H49C109.5
N11—C12—C22114.9 (6)H49A—C49—H49C109.5
C13—C12—C22122.9 (6)H49B—C49—H49C109.5
C14—C13—C12118.0 (7)C52—C51—C56119.4 (8)
C14—C13—H13121.0C52—C51—C36121.3 (8)
C12—C13—H13121.0C56—C51—C36119.3 (7)
C13—C14—C15120.8 (7)C51—C52—C53117.7 (9)
C13—C14—H14119.6C51—C52—C57121.7 (9)
C15—C14—H14119.6C53—C52—C57120.6 (9)
C14—C15—C16118.3 (7)C54—C53—C52122.3 (9)
C14—C15—H15120.9C54—C53—H53118.8
C16—C15—H15120.9C52—C53—H53118.8
N11—C16—C15122.6 (6)C55—C54—C53119.2 (10)
N11—C16—C41116.5 (6)C55—C54—C58119.3 (12)
C15—C16—C41120.8 (6)C53—C54—C58121.5 (11)
N21—C22—C23121.4 (6)C54—C55—C56121.2 (10)
N21—C22—C12114.5 (5)C54—C55—H55119.4
C23—C22—C12124.1 (7)C56—C55—H55119.4
C24—C23—C22119.3 (7)C51—C56—C55120.2 (8)
C24—C23—H23120.3C51—C56—C59122.1 (8)
C22—C23—H23120.3C55—C56—C59117.7 (9)
C23—C24—C25119.4 (7)C52—C57—H57A109.5
C23—C24—H24120.3C52—C57—H57B109.5
C25—C24—H24120.3H57A—C57—H57B109.5
C24—C25—C26118.3 (7)C52—C57—H57C109.5
C24—C25—H25120.8H57A—C57—H57C109.5
C26—C25—H25120.8H57B—C57—H57C109.5
N21—C26—C25121.6 (7)C54—C58—H58A109.5
N21—C26—C32114.6 (6)C54—C58—H58B109.5
C25—C26—C32123.8 (7)H58A—C58—H58B109.5
N31—C32—C33123.9 (7)C54—C58—H58C109.5
N31—C32—C26113.6 (6)H58A—C58—H58C109.5
C33—C32—C26122.4 (7)H58B—C58—H58C109.5
C32—C33—C34116.7 (8)C56—C59—H59A109.5
C32—C33—H33121.7C56—C59—H59B109.5
C34—C33—H33121.7H59A—C59—H59B109.5
C35—C34—C33120.5 (8)C56—C59—H59C109.5
C35—C34—H34119.7H59A—C59—H59C109.5
C33—C34—H34119.7H59B—C59—H59C109.5
C34—C35—C36120.1 (8)

Experimental details

Crystal data
Chemical formula[Cu(C2H3N)(C33H31N3)](PF6)
Mr719.17
Crystal system, space groupMonoclinic, P21/n
Temperature (K)296
a, b, c (Å)11.317 (3), 23.592 (4), 12.873 (2)
β (°) 92.450 (16)
V3)3433.7 (11)
Z4
Radiation typeMo Kα
µ (mm1)0.75
Crystal size (mm)0.50 × 0.30 × 0.20
Data collection
DiffractometerRigaku AFC-5R
diffractometer
Absorption correctionΨ scan
(North, 1968)
Tmin, Tmax0.842, 0.998
No. of measured, independent and
observed [I > 2σ(I)] reflections
7686, 7302, 2104
Rint0.150
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.052, 0.227, 0.91
No. of reflections7302
No. of parameters425
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.50, 0.58

Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1991), MSC/AFC Diffractometer Control Software, TEXSAN (Molecular Structure Corporation, 1999), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), PLEASE PROVIDE, SHELXL97.

Selected geometric parameters (Å, º) top
Cu1—N11.886 (6)Cu1—N312.232 (5)
Cu1—N212.003 (5)Cu1—N112.244 (5)
N1—Cu1—N21152.8 (3)N1—Cu1—N11106.8 (2)
N1—Cu1—N31108.8 (2)N21—Cu1—N1176.8 (2)
N21—Cu1—N3176.3 (2)N31—Cu1—N11142.9 (2)
 

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