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In the crystal structure of the dinuclear title compound, [CuZnBr2(C19H22N2O2)(C5H11N)], the CuII ion has a distorted square-pyramidal coordination involving two iminic N and two phenolic O atoms of the N,N′-bis­(salicyl­idene)-2,2′-di­methyl-1,3-propane­diaminate (SALPD2− or C17H16N2O22−) ligand and one N atom of the piperidine group. The coordination around the ZnII ion is distorted tetrahedral, with two O atoms of the SALPD2− ligand and two bromide ions. The Zn—Br bond lengths are 2.3309 (9) and 2.3508 (10) Å. The Cu...Zn distance is 3.0800 (9) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801019171/br6030sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801019171/br6030Isup2.hkl
Contains datablock I

CCDC reference: 177184

Key indicators

  • Single-crystal X-ray study
  • T = 301 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.038
  • wR factor = 0.095
  • Data-to-parameter ratio = 17.1

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_213 Alert C Atom C23 has ADP max/min Ratio ........... 4.00 prolate PLAT_420 Alert C D-H Without Acceptor N3 - H3A ? General Notes
ABSTY_01 Extra text has been found in the _exptl_absorpt_correction_type field, which should be only a single keyword. A literature citation should be included in the _exptl_absorpt_process_details field.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check

Computing details top

Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1993); cell refinement: SHELXL97 (Sheldrick, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97; molecular graphics: PLATON (Spek, 2000); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
[CuZnBr2(C17H16N2O2)(CH3)2(C5H11N)]Z = 4
Mr = 682.25Dx = 1.736 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 25 reflections
a = 10.659 (2) Åθ = 1.9–26.0°
b = 14.550 (1) ŵ = 4.82 mm1
c = 16.992 (3) ÅT = 301 K
β = 97.91 (2)°Prism, light green
V = 2610.2 (7) Å30.35 × 0.30 × 0.25 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer
Rint = 0.041
ω/2θ scansθmax = 26.0°
Absorption correction: empirical (using intensity measurements) via ψ scans
(Fair, 1990)
h = 136
Tmin = 0.202, Tmax = 0.300k = 170
8583 measured reflectionsl = 2020
5111 independent reflections3 standard reflections every 120 min
3403 reflections with I > 2σ(I) intensity decay: 1.2%
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)] = 0.038H-atom parameters constrained
wR(F2) = 0.095 w = 1/[σ2(Fo2) + (0.0506P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max = 0.0001
5111 reflectionsΔρmax = 0.82 e Å3
299 parametersΔρmin = 0.50 e Å3
2 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0028 (3)
Special details top

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
Cu0.26737 (5)0.24855 (3)0.38658 (3)0.03827 (17)
Zn0.01432 (5)0.33604 (4)0.31450 (4)0.04724 (18)
Br10.15362 (5)0.37698 (4)0.38186 (5)0.0752 (2)
Br20.00582 (7)0.36447 (4)0.17715 (4)0.0739 (2)
O10.0950 (3)0.2132 (2)0.3395 (2)0.0439 (8)
O20.1876 (3)0.36854 (19)0.3681 (2)0.0503 (9)
N10.3244 (3)0.1197 (2)0.3859 (2)0.0388 (9)
N20.4351 (3)0.3058 (2)0.4167 (2)0.0410 (9)
N30.2296 (4)0.2350 (3)0.5169 (2)0.0461 (10)
C10.0476 (4)0.1310 (3)0.3183 (3)0.0398 (10)
C20.0823 (4)0.1221 (3)0.2899 (3)0.0497 (12)
C30.1330 (5)0.0379 (4)0.2681 (3)0.0566 (14)
C40.0566 (5)0.0409 (4)0.2730 (3)0.0555 (13)
C50.0677 (5)0.0326 (3)0.3005 (3)0.0482 (12)
C60.1237 (4)0.0526 (3)0.3246 (3)0.0389 (10)
C70.2559 (4)0.0517 (3)0.3563 (3)0.0415 (11)
C80.4517 (4)0.0936 (3)0.4248 (3)0.0493 (12)
C90.5573 (4)0.1582 (3)0.4087 (3)0.0473 (12)
C100.5457 (4)0.2494 (3)0.4512 (3)0.0511 (12)
C110.5604 (5)0.1715 (4)0.3206 (3)0.0622 (15)
C120.6831 (5)0.1151 (4)0.4470 (4)0.0740 (18)
C130.4578 (4)0.3915 (3)0.4117 (3)0.0462 (11)
C140.3697 (4)0.4651 (3)0.3890 (3)0.0419 (11)
C150.4205 (5)0.5544 (3)0.3877 (3)0.0536 (13)
C160.3435 (6)0.6291 (3)0.3688 (4)0.0608 (15)
C170.2155 (6)0.6153 (3)0.3519 (4)0.0603 (15)
C180.1621 (5)0.5290 (3)0.3520 (4)0.0577 (14)
C190.2400 (4)0.4528 (3)0.3702 (3)0.0451 (11)
C200.2374 (6)0.3087 (5)0.5729 (4)0.0799 (19)
C210.1109 (7)0.3402 (6)0.5845 (5)0.110 (3)
C220.0399 (6)0.2659 (5)0.6135 (4)0.0709 (18)
C230.0281 (6)0.1957 (7)0.5528 (5)0.114 (3)
C240.1556 (6)0.1621 (4)0.5433 (4)0.0756 (17)
H20.13520.17490.28600.060*
H30.22090.03290.24930.068*
H3A0.30790.20940.53590.055*
H40.09180.09910.25730.067*
H50.11940.08600.30380.058*
H70.29780.00580.35530.050*
H8A0.47130.03120.40680.059*
H8B0.45030.09070.48280.059*
H10A0.53870.23700.50770.061*
H10B0.62400.28540.44930.061*
H11A0.62920.21380.31270.093*
H11B0.47950.19720.29600.093*
H11C0.57470.11210.29610.093*
H12A0.68090.10630.50400.111*
H12B0.75340.15610.43940.111*
H12C0.69500.05560.42210.111*
H130.54400.40910.42460.055*
H150.50940.56300.40010.064*
H160.37830.68910.36740.073*
H170.16180.66700.33990.072*
H180.07300.52160.33960.069*
H20A0.28530.36030.55350.096*
H20B0.28360.28770.62430.096*
H21A0.11820.39150.62310.131*
H21B0.06560.36310.53350.131*
H22A0.04490.28760.62290.085*
H22B0.08500.24150.66400.085*
H23A0.01370.22140.50190.137*
H23B0.02420.14440.56830.137*
H24A0.19790.13800.59470.091*
H24B0.14860.11140.50420.091*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu0.0297 (3)0.0407 (3)0.0443 (4)0.0001 (2)0.0046 (2)0.0009 (2)
Zn0.0340 (3)0.0443 (3)0.0619 (4)0.0070 (3)0.0013 (2)0.0004 (2)
Br10.0455 (3)0.0798 (4)0.1035 (6)0.0111 (3)0.0218 (3)0.0125 (3)
Br20.0931 (5)0.0632 (4)0.0622 (5)0.0123 (3)0.0005 (3)0.0106 (3)
O10.0313 (15)0.0399 (15)0.059 (2)0.0017 (14)0.0007 (14)0.0028 (13)
O20.0344 (16)0.0371 (16)0.078 (3)0.0007 (15)0.0019 (16)0.0028 (13)
N10.0310 (18)0.043 (2)0.042 (2)0.0041 (17)0.0059 (16)0.0032 (15)
N20.0322 (18)0.048 (2)0.043 (3)0.0035 (17)0.0057 (17)0.0022 (15)
N30.048 (2)0.058 (2)0.036 (2)0.0090 (18)0.0206 (19)0.0080 (18)
C10.038 (2)0.046 (2)0.036 (3)0.0027 (19)0.007 (2)0.0064 (19)
C20.033 (2)0.055 (3)0.060 (4)0.001 (2)0.005 (2)0.004 (2)
C30.042 (3)0.063 (3)0.065 (4)0.002 (3)0.008 (2)0.015 (2)
C40.057 (3)0.050 (3)0.059 (4)0.004 (2)0.009 (3)0.017 (2)
C50.056 (3)0.044 (2)0.045 (3)0.003 (2)0.009 (2)0.004 (2)
C60.041 (2)0.043 (2)0.033 (3)0.0041 (19)0.006 (2)0.0019 (19)
C70.047 (2)0.040 (2)0.038 (3)0.0016 (19)0.006 (2)0.003 (2)
C80.041 (3)0.055 (3)0.049 (3)0.003 (2)0.003 (2)0.008 (2)
C90.031 (2)0.062 (3)0.048 (3)0.001 (2)0.001 (2)0.008 (2)
C100.034 (2)0.065 (3)0.052 (3)0.001 (2)0.005 (2)0.004 (2)
C110.044 (3)0.088 (4)0.057 (4)0.003 (3)0.014 (3)0.011 (3)
C120.039 (3)0.087 (4)0.093 (5)0.006 (3)0.001 (3)0.016 (3)
C130.033 (2)0.062 (3)0.044 (3)0.006 (2)0.007 (2)0.009 (2)
C140.042 (2)0.047 (2)0.038 (3)0.005 (2)0.011 (2)0.010 (2)
C150.058 (3)0.060 (3)0.043 (3)0.004 (2)0.007 (2)0.016 (3)
C160.085 (4)0.044 (3)0.053 (4)0.008 (2)0.009 (3)0.015 (3)
C170.073 (4)0.042 (3)0.066 (4)0.005 (2)0.008 (3)0.002 (2)
C180.055 (3)0.042 (3)0.076 (4)0.005 (2)0.009 (3)0.002 (2)
C190.046 (3)0.041 (2)0.049 (3)0.003 (2)0.008 (2)0.003 (2)
C200.078 (4)0.099 (5)0.062 (5)0.020 (4)0.008 (3)0.004 (4)
C210.099 (6)0.126 (7)0.100 (7)0.043 (5)0.001 (5)0.053 (5)
C220.053 (3)0.113 (5)0.055 (4)0.014 (4)0.034 (3)0.032 (3)
C230.055 (4)0.186 (9)0.102 (7)0.081 (7)0.012 (4)0.012 (5)
C240.085 (4)0.090 (4)0.055 (4)0.006 (3)0.022 (3)0.011 (4)
Geometric parameters (Å, º) top
Cu—Zn3.0800 (9)C11—H11B0.98
Cu—O11.969 (3)C11—H11C0.98
Cu—O21.948 (3)C12—H12A0.98
Cu—N11.972 (3)C12—H12B0.98
Cu—N21.975 (3)C12—H12C0.98
Cu—N32.312 (4)C13—N21.274 (6)
Zn—Br12.3309 (9)C13—C141.442 (6)
Zn—Br22.3508 (10)C13—H130.95
Zn—O12.003 (3)C14—C191.388 (6)
Zn—O22.001 (3)C14—C151.409 (6)
N3—H3A0.9375C15—C161.373 (7)
C1—O11.328 (5)C15—H150.95
C1—C21.409 (6)C16—C171.370 (8)
C1—C61.395 (6)C16—H160.95
C2—C31.369 (7)C17—C181.379 (7)
C2—H20.95C17—H170.95
C3—C41.402 (7)C18—C191.394 (6)
C3—H30.95C18—H180.95
C4—C51.348 (7)C19—O21.346 (5)
C4—H40.95C20—N31.428 (7)
C5—C61.411 (6)C20—C211.463 (9)
C5—H50.95C20—H20A0.99
C6—C71.438 (6)C20—H20B0.99
C7—N11.290 (5)C21—C221.445 (9)
C7—H70.95C21—H21A0.99
C8—N11.475 (5)C21—H21B0.99
C8—C91.520 (7)C22—C231.444 (10)
C8—H8A0.99C22—H22A0.99
C8—H8B0.99C22—H22B0.99
C9—C111.514 (8)C23—C241.474 (10)
C9—C101.524 (7)C23—H23A0.99
C9—C121.541 (6)C23—H23B0.99
C10—N21.488 (6)C24—N31.431 (7)
C10—H10A0.99C24—H24A0.99
C10—H10B0.99C24—H24B0.99
C11—H11A0.98
O2—Cu—O178.84 (12)C11—C9—C10111.8 (4)
O2—Cu—N1168.33 (15)C8—C9—C10110.0 (4)
O1—Cu—N191.17 (13)C11—C9—C12109.5 (4)
O2—Cu—N291.32 (14)C8—C9—C12107.2 (4)
O1—Cu—N2167.54 (15)C10—C9—C12106.1 (4)
N1—Cu—N297.70 (15)N2—C10—C9113.9 (4)
O2—Cu—N395.80 (15)N2—C13—C14128.5 (4)
O1—Cu—N395.22 (14)C19—C14—C15119.2 (4)
N1—Cu—N391.07 (15)C19—C14—C13123.9 (4)
N2—Cu—N393.34 (15)C15—C14—C13116.9 (4)
O2—Cu—Zn39.37 (9)C16—C15—C14121.0 (5)
O1—Cu—Zn39.55 (9)C17—C16—C15118.7 (5)
N1—Cu—Zn130.12 (10)C16—C17—C18122.2 (5)
N2—Cu—Zn129.85 (11)C17—C18—C19119.4 (5)
Cu—O2—Zn102.50 (13)O2—C19—C14121.3 (4)
O2—Zn—O176.80 (12)O2—C19—C18119.2 (4)
O2—Zn—Br1116.05 (11)C14—C19—C18119.5 (4)
O1—Zn—Br1117.39 (10)N3—C20—C21110.8 (5)
O2—Zn—Br2111.29 (12)C22—C21—C20110.3 (6)
O1—Zn—Br2110.22 (10)C21—C22—C23106.5 (6)
Br1—Zn—Br2118.11 (4)C22—C23—C24108.8 (6)
O2—Zn—Cu38.13 (8)N3—C24—C23110.2 (5)
O1—Zn—Cu38.75 (8)N3—Cu—Zn99.08 (10)
Br1—Zn—Cu126.87 (3)C7—N1—C8114.4 (4)
Br2—Zn—Cu115.01 (3)C7—N1—Cu125.0 (3)
O1—C1—C2119.7 (4)C8—N1—Cu120.5 (3)
O1—C1—C6121.4 (4)C13—N2—C10114.7 (4)
C2—C1—C6118.9 (4)C13—N2—Cu124.6 (3)
C3—C2—C1120.6 (4)C10—N2—Cu120.6 (3)
C2—C3—C4120.7 (4)C24—N3—C20109.3 (5)
C5—C4—C3118.9 (5)C24—N3—Cu122.7 (3)
C4—C5—C6122.3 (5)C20—N3—Cu124.9 (4)
C1—C6—C5118.6 (4)C1—O1—Cu130.1 (3)
C1—C6—C7124.4 (4)C1—O1—Zn127.6 (3)
C5—C6—C7117.0 (4)Cu—O1—Zn101.70 (13)
N1—C7—C6127.7 (4)C19—O2—Cu130.0 (3)
N1—C8—C9114.8 (4)C19—O2—Zn125.5 (3)
C11—C9—C8112.0 (4)
 

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