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Acta Cryst. (2007). E63, m2277-m2278
https://doi.org/10.1107/S1600536807037737
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Retracted: {6,6′-Dimeth­oxy-2,2′-[ethane-1,2-diyl­bis(nitrilo­methyl­idyne)]­diphenolato}­methanol-μ-nitrato-dinitrato­lutetium(III)­zinc(II)

Y. Sui, Y.-H. Sui, Q.-Y. Luo and Y.-D. Wang
In the title heteronuclear ZnII–LuIII complex (systematic name: {6,6′-dimeth­oxy-2,2′-[ethane-1,2-diylbis(nitrilo­methyl­idyne)]diphenolato-1κ4O1,O1′,O6,O6′:2κ4O1,N,N′,O1′}(methanol-1κO)-μ-nitrato-1:2κ2O:O′-dinitrato-1κ4O,O′-lutetium(III)­zinc(II)), [LuZn(C18H18N2O4)(NO3)3(CH4O)], with the hexa­dentate Schiff base compartmental ligand N,N′-bis­(3-methoxy­salicyl­idene)ethyl­enediamine, the Lu and Zn atoms are triply bridged by two phenolate O atoms provided by the Schiff base ligand and one nitrate ion. The five-coordinated Zn is in a square-pyramidal geometry with the donor centers of two imine N atoms, two phenolate O atoms and one of the bridging nitrate O atoms. The LuIII center has a tenfold coordination environment of O atoms, involving the phenolate O atoms, two meth­oxy O atoms, one methanol O atom, and two O atoms from two nitrate ions and one from the bridging nitrate ion. Weak inter­molecular C—H...O inter­actions generate a two-dimensional layer structure.
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807037737/hg2271sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807037737/hg2271Isup2.hkl
Contains datablock I

CCDC reference: 1101491

checkCIF report

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.045
  • wR factor = 0.147
  • Data-to-parameter ratio = 17.3

checkCIF/PLATON results

No syntax errors found




Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.97
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.99
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       3.39 Ratio
PLAT230_ALERT_2_C Hirshfeld Test Diff for    O6     -   N4      ..       6.71 su
PLAT230_ALERT_2_C Hirshfeld Test Diff for    O7     -   N4      ..       5.38 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Lu1    -   O1      ..       6.39 su
PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ...          9
PLAT731_ALERT_1_C Bond    Calc     0.92(6), Rep     0.91(2) ......       3.00 su-Ra
              O1   -H1      1.555   1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      34.00 Deg.
              LU1  -O1   -H1      1.555   1.555   1.555


Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K
PLAT794_ALERT_5_G Check Predicted Bond Valency for Lu1         (3)       3.24
PLAT794_ALERT_5_G Check Predicted Bond Valency for Zn1         (2)       2.12
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......          1


   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   9 ALERT level C = Check and explain
   5 ALERT level G = General alerts; check

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   5 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
   1 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check
Comment top

The potential applications of trivalent lanthanide complexes as contrast agent for magnetic resonance imaging and stains for fluorescence imaging have prompted considerable interest in the preparation, magnetic and optical properties of 3 d-4f hetorometallic dinuclear complexes (Baggio et al., 2000; Caravan et al., 1999; Edder et al., 2000; Knoer et al., 2005). As part of our investigations into the structure and applications of 3 d-4f hetorometallic Schiff base complexes(Sui et al., 2006; Sui et al., 2007), we report here the synthesis and X-ray crystal structure analysis of the title complex, (I), a new ZnII—LuIII complex with salen-type Schiff base N,N'-bis(3-methoxysalicylidene) ethylenediamine(H2L).

Complex (I) crystallizes in the space group P21/n, with zinc and lutetium triply bridged by two phenolate O atoms provided by a salen-type Schiff base ligand and one nitrate. The inner salen-type cavity is occupied by zinc(II), while lutetium(III) is present in the open and larger portion of the dinucleating compartmental Schiff base ligand.

The LuIII center has a decacoordination environment of O atoms, involving the phenolate O atoms, two methoxy O atoms, one methanol O atom, two O atoms from two nitrates and one from the bridging nitrate. The five kinds of Lu—O bond distances are significantly different, the longest being the Lu—O(methoxy) separations and the shortest being the Lu—O(phenolate) and Lu—O6(bridging nitrate).

The ZnII is in a square-pyramidal geometry and is five-coordinated by two imine N atoms, two phenolate O atoms and one of the bridging nitrate O atoms. The Zn atom is 0.5813 (3)Å above the mean N2O2 plane with an average deviation from the plane of 0.0951 (4) Å, which construct the bottom of square-pyramid. The Zn—O7(bridging nitrate) separation is 2.001 (4)Å and the angles of this Zn—O vector with the Zn—N or Zn—O bonds lie between 103.1 (5)° and 115.7 (6)°, which suggesting that the ZnII is in a slightly distorted square-pyramidal conformation.

Adjacent molecules are held together by weak interactions (C10—H10···O12i=3.443 (7) and C12—H12···O9i=3.445 (8); symmetry codes: (i)1/2 + x, 1/2 - y, 1/2 + z). these link the molecules into a two-dimensional layer structure(Fig 2).

Related literature top

For related literature, see: Baggio et al. (2000); Caravan et al. (1999); Edder et al. (2000); Knoer et al. (2005); Sui et al. (2006, 2007).

Experimental top

H2L was prepared by the 2:1 condensation of 3-methoxysalicylaldehyde and ethylenediamine in methanol. Complex (I) was obtained by the treatment of zinc(II) acetate dihydrate (0.188 g, 1 mmol) with H2L(0.328 g, 1 mmol) in methanol solution (80 ml) under reflux for 3 h and then for another 3 h after the addition of lutetium(III) nitrate hexahydrate(0.469 g, 1 mmol). The reaction mixture was cooled and the resulting precipitate was filtered off, washed with diethyl ether and dried in vacuo. Single crystals of (I) suitable for X-ray analysis were obtained by slow evaporation at room temperature of a methanol solution. Analysis calculated for C19H22LuN5O14Zn: C 29.08, H 2.83, Lu 22.30, N 8.92,Zn 8.33%; found: C 30.01, H 2.85, Lu 22.39, N 8.98, Zn 8.38%. IR(KBr, cm-1): 1640(C=N), 1386,1490(nitrate).

Refinement top

The H atoms were positioned geometrically and treated as riding on their parent atoms, with C—H distances of 0.97Å (methylene) and 0.96Å (methyl), and with Uiso(H) = 1.5Ueq(C) for methyl H atoms and 1.2Ueq(C) for other H atoms. The methyl group of methanol was constrainted as idealized non-rotating CH3 group. The hydroxyl H atom, H1, was located in a difference Fourier map and refined with the O1—H1 distance restrained to 0.9 Å

Structure description top

The potential applications of trivalent lanthanide complexes as contrast agent for magnetic resonance imaging and stains for fluorescence imaging have prompted considerable interest in the preparation, magnetic and optical properties of 3 d-4f hetorometallic dinuclear complexes (Baggio et al., 2000; Caravan et al., 1999; Edder et al., 2000; Knoer et al., 2005). As part of our investigations into the structure and applications of 3 d-4f hetorometallic Schiff base complexes(Sui et al., 2006; Sui et al., 2007), we report here the synthesis and X-ray crystal structure analysis of the title complex, (I), a new ZnII—LuIII complex with salen-type Schiff base N,N'-bis(3-methoxysalicylidene) ethylenediamine(H2L).

Complex (I) crystallizes in the space group P21/n, with zinc and lutetium triply bridged by two phenolate O atoms provided by a salen-type Schiff base ligand and one nitrate. The inner salen-type cavity is occupied by zinc(II), while lutetium(III) is present in the open and larger portion of the dinucleating compartmental Schiff base ligand.

The LuIII center has a decacoordination environment of O atoms, involving the phenolate O atoms, two methoxy O atoms, one methanol O atom, two O atoms from two nitrates and one from the bridging nitrate. The five kinds of Lu—O bond distances are significantly different, the longest being the Lu—O(methoxy) separations and the shortest being the Lu—O(phenolate) and Lu—O6(bridging nitrate).

The ZnII is in a square-pyramidal geometry and is five-coordinated by two imine N atoms, two phenolate O atoms and one of the bridging nitrate O atoms. The Zn atom is 0.5813 (3)Å above the mean N2O2 plane with an average deviation from the plane of 0.0951 (4) Å, which construct the bottom of square-pyramid. The Zn—O7(bridging nitrate) separation is 2.001 (4)Å and the angles of this Zn—O vector with the Zn—N or Zn—O bonds lie between 103.1 (5)° and 115.7 (6)°, which suggesting that the ZnII is in a slightly distorted square-pyramidal conformation.

Adjacent molecules are held together by weak interactions (C10—H10···O12i=3.443 (7) and C12—H12···O9i=3.445 (8); symmetry codes: (i)1/2 + x, 1/2 - y, 1/2 + z). these link the molecules into a two-dimensional layer structure(Fig 2).

For related literature, see: Baggio et al. (2000); Caravan et al. (1999); Edder et al. (2000); Knoer et al. (2005); Sui et al. (2006, 2007).

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: APEX2; software used to prepare material for publication: APEX2 and publCIF (Westrip, 2007).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), showing 30% probability displacement ellipsoids.
[Figure 2] Fig. 2. The packing diagram of (I), viewed along the c axis; hydrogen bonds are shown as dashed lines.
{6,6'-dimethoxy-2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato-\1κ4O1,O1',O6,O6':2κ4O1,\<i>N,N',O1'}(methanol-1κO)-µ-nitrato-1:\2κ2O:O'-dinitrato-1κ4O,O'-lutetium(III)ζinc(II) top
Crystal data top
[LuZn(C18H18N2O4)(NO3)3(CH4O)]F(000) = 1536
Mr = 784.76Dx = 1.992 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 6963 reflections
a = 9.6105 (11) Åθ = 2.1–28.3°
b = 13.7179 (16) ŵ = 4.75 mm−1
c = 19.851 (2) ÅT = 293 K
β = 91.559 (2)°Block, yellow
V = 2616.2 (5) Å30.22 × 0.11 × 0.06 mm
Z = 4
Data collection top
Bruker APEX II area-detector
diffractometer		6348 independent reflections
Radiation source: fine-focus sealed tube4676 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.036
φ and ω scansθmax = 28.3°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2004)		h = −12→12
Tmin = 0.422, Tmax = 0.764k = −16→18
18694 measured reflectionsl = −26→26
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)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.147H atoms treated by a mixture of independent and constrained refinement
S = 1.01 w = 1/[σ2(Fo2) + (0.1008P)2]
where P = (Fo2 + 2Fc2)/3
6348 reflections(Δ/σ)max = 0.001
367 parametersΔρmax = 1.89 e Å−3
1 restraintΔρmin = −1.24 e Å−3
Crystal data top
[LuZn(C18H18N2O4)(NO3)3(CH4O)]V = 2616.2 (5) Å3
Mr = 784.76Z = 4
Monoclinic, P21/nMo Kα radiation
a = 9.6105 (11) ŵ = 4.75 mm−1
b = 13.7179 (16) ÅT = 293 K
c = 19.851 (2) Å0.22 × 0.11 × 0.06 mm
β = 91.559 (2)°
Data collection top
Bruker APEX II area-detector
diffractometer		6348 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2004)		4676 reflections with I > 2σ(I)
Tmin = 0.422, Tmax = 0.764Rint = 0.036
18694 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0451 restraint
wR(F2) = 0.147H atoms treated by a mixture of independent and constrained refinement
S = 1.01Δρmax = 1.89 e Å−3
6348 reflectionsΔρmin = −1.24 e Å−3
367 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
Lu10.71866 (3)0.27793 (2)0.115439 (12)0.03144 (12)
Zn10.68616 (7)0.37139 (5)0.27269 (3)0.02574 (17)
O90.7326 (5)0.3589 (3)0.0042 (2)0.0345 (10)
C160.9327 (6)0.2406 (4)0.2552 (3)0.0233 (11)
N30.7914 (6)0.3541 (4)0.3614 (3)0.0358 (12)
C10.4254 (6)0.3545 (4)0.1936 (3)0.0269 (12)
C151.0143 (6)0.1820 (5)0.2139 (3)0.0278 (12)
O100.9304 (4)0.3295 (4)0.0530 (2)0.0362 (10)
N10.8632 (7)0.3645 (4)0.0027 (3)0.0417 (14)
O40.4598 (4)0.3571 (4)0.0784 (2)0.0382 (11)
N20.5204 (6)0.3680 (4)0.3370 (2)0.0347 (12)
C20.3668 (6)0.3698 (5)0.1290 (3)0.0302 (13)
C121.0935 (7)0.1994 (6)0.3476 (4)0.0429 (18)
H121.12020.20440.39280.051*
C60.3432 (6)0.3723 (5)0.2495 (4)0.0338 (14)
C110.9745 (7)0.2492 (5)0.3237 (3)0.0316 (13)
C30.2275 (6)0.3960 (6)0.1195 (4)0.0422 (17)
H30.19020.40590.07630.051*
C141.1308 (7)0.1341 (5)0.2382 (3)0.0372 (15)
H141.18250.09540.20970.045*
O110.9235 (7)0.3988 (6)−0.0447 (3)0.081 (2)
C50.2012 (7)0.3978 (5)0.2378 (4)0.0437 (18)
H50.14510.40820.27450.052*
C100.8999 (7)0.3033 (5)0.3734 (3)0.0341 (14)
H100.93370.30070.41770.041*
C70.3935 (7)0.3673 (5)0.3192 (3)0.0382 (15)
H70.32800.36340.35270.046*
C131.1710 (7)0.1434 (6)0.3053 (4)0.0457 (18)
H131.25050.11180.32170.055*
C171.0623 (7)0.1394 (6)0.1013 (3)0.0463 (18)
H17A1.15240.16770.11010.069*
H17B1.03120.15530.05630.069*
H17C1.06820.06990.10610.069*
C180.4098 (8)0.3814 (7)0.0115 (4)0.053 (2)
H18A0.32710.34460.00100.080*
H18B0.47990.3661−0.02030.080*
H18C0.38880.44980.00920.080*
C40.1453 (7)0.4072 (5)0.1753 (4)0.0483 (19)
H40.05100.42130.16950.058*
O30.8215 (4)0.2822 (3)0.22720 (19)0.0252 (9)
O20.5557 (4)0.3227 (3)0.1980 (2)0.0277 (9)
O70.7422 (4)0.5038 (3)0.24088 (19)0.0299 (9)
O50.9661 (4)0.1771 (3)0.1480 (2)0.0305 (9)
O10.6452 (4)0.1208 (3)0.1631 (2)0.0312 (9)
O60.7588 (5)0.4461 (3)0.1366 (2)0.0372 (10)
O120.5672 (5)0.1831 (4)0.0287 (2)0.0362 (10)
O130.7842 (5)0.1475 (3)0.0300 (2)0.0366 (10)
N50.6642 (6)0.1335 (4)0.0041 (2)0.0341 (12)
N40.7731 (6)0.5131 (4)0.1793 (3)0.0411 (13)
C90.7120 (8)0.3983 (5)0.4171 (3)0.0416 (16)
H9A0.71510.46890.41440.050*
H9B0.75090.37820.46050.050*
C80.5620 (8)0.3619 (6)0.4081 (3)0.0459 (18)
H8A0.55560.29490.42340.055*
H8B0.50050.40140.43470.055*
C190.5051 (8)0.0893 (6)0.1656 (4)0.052 (2)
H19A0.45830.12480.19990.079*
H19B0.50280.02090.17560.079*
H19C0.45930.10080.12270.079*
O140.6430 (6)0.0768 (4)−0.0412 (3)0.0619 (16)
O80.8349 (9)0.6088 (5)0.1561 (4)0.086 (2)
H10.699 (6)0.151 (5)0.132 (3)0.037 (19)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Lu10.03498 (17)0.03647 (19)0.02275 (15)−0.00013 (11)−0.00161 (11)−0.00127 (10)
Zn10.0316 (4)0.0291 (4)0.0166 (3)−0.0008 (3)0.0017 (3)−0.0009 (3)
O90.034 (2)0.049 (3)0.020 (2)0.003 (2)−0.0042 (17)0.0029 (18)
C160.024 (3)0.027 (3)0.019 (3)−0.003 (2)−0.009 (2)0.006 (2)
N30.051 (3)0.039 (3)0.017 (2)−0.005 (3)−0.002 (2)−0.007 (2)
C10.018 (3)0.027 (3)0.036 (3)−0.001 (2)0.001 (2)−0.006 (2)
C150.028 (3)0.030 (3)0.025 (3)−0.001 (2)−0.004 (2)0.003 (2)
O100.026 (2)0.046 (3)0.037 (2)−0.0026 (19)−0.0018 (18)0.005 (2)
N10.052 (4)0.045 (4)0.028 (3)0.001 (3)0.009 (3)0.002 (2)
O40.031 (2)0.056 (3)0.028 (2)0.009 (2)−0.0102 (18)−0.008 (2)
N20.045 (3)0.041 (3)0.018 (2)−0.001 (2)0.009 (2)−0.001 (2)
C20.021 (3)0.027 (3)0.042 (3)0.003 (2)0.000 (2)−0.009 (3)
C120.040 (4)0.058 (5)0.030 (3)−0.006 (3)−0.017 (3)0.014 (3)
C60.027 (3)0.025 (3)0.050 (4)−0.001 (2)0.013 (3)−0.001 (3)
C110.034 (3)0.041 (4)0.020 (3)−0.006 (3)−0.011 (2)0.005 (3)
C30.022 (3)0.040 (4)0.064 (5)0.005 (3)−0.010 (3)−0.008 (3)
C140.031 (3)0.039 (4)0.041 (4)0.008 (3)−0.008 (3)0.004 (3)
O110.074 (4)0.112 (6)0.059 (4)−0.004 (4)0.030 (3)0.041 (4)
C50.029 (3)0.032 (4)0.070 (5)0.002 (3)0.018 (3)−0.007 (4)
C100.039 (4)0.046 (4)0.016 (3)−0.012 (3)−0.007 (2)0.002 (3)
C70.043 (4)0.034 (4)0.039 (3)0.004 (3)0.019 (3)0.000 (3)
C130.034 (4)0.054 (5)0.048 (4)0.012 (3)−0.012 (3)0.016 (4)
C170.043 (4)0.061 (5)0.034 (4)0.017 (3)0.003 (3)−0.005 (3)
C180.049 (4)0.073 (6)0.038 (4)0.013 (4)−0.011 (3)−0.002 (4)
C40.020 (3)0.042 (4)0.083 (6)0.005 (3)0.007 (3)−0.003 (4)
O30.024 (2)0.036 (2)0.0158 (18)0.0032 (16)−0.0046 (15)−0.0008 (15)
O20.0231 (19)0.035 (2)0.025 (2)0.0036 (17)−0.0015 (16)−0.0048 (18)
O70.044 (2)0.023 (2)0.023 (2)0.0001 (17)0.0051 (18)−0.0026 (16)
O50.029 (2)0.039 (3)0.023 (2)0.0060 (18)−0.0043 (16)−0.0035 (18)
O10.031 (2)0.027 (2)0.036 (2)−0.0040 (17)−0.0015 (18)0.0063 (19)
O60.059 (3)0.029 (3)0.023 (2)−0.005 (2)0.004 (2)−0.0032 (18)
O120.038 (2)0.041 (3)0.028 (2)0.000 (2)−0.0088 (19)−0.003 (2)
O130.035 (2)0.045 (3)0.030 (2)0.001 (2)−0.0026 (19)−0.007 (2)
N50.051 (3)0.029 (3)0.021 (2)−0.002 (2)−0.005 (2)0.000 (2)
N40.041 (3)0.039 (3)0.044 (3)0.005 (3)0.002 (3)0.008 (3)
C90.067 (5)0.040 (4)0.018 (3)0.005 (3)0.006 (3)−0.003 (3)
C80.069 (5)0.045 (4)0.025 (3)0.010 (4)0.021 (3)0.008 (3)
C190.039 (4)0.061 (5)0.057 (5)−0.017 (4)0.006 (3)0.014 (4)
O140.083 (4)0.058 (4)0.043 (3)0.002 (3)−0.022 (3)−0.030 (3)
O80.116 (6)0.060 (4)0.083 (5)−0.010 (4)0.030 (4)0.003 (4)
Geometric parameters (Å, º) top
Lu1—O12.465 (4)C6—C51.421 (9)
Lu1—O22.378 (4)C6—C71.456 (10)
Lu1—O32.405 (4)C11—C101.442 (10)
Lu1—O42.794 (4)C3—C41.387 (10)
Lu1—O52.812 (4)C3—H30.9300
Lu1—O62.374 (5)C14—C131.382 (10)
Lu1—O92.479 (4)C14—H140.9300
Lu1—O102.513 (4)C5—C41.344 (11)
Lu1—O122.577 (4)C5—H50.9300
Lu1—O132.556 (4)C10—H100.9300
Zn1—O22.029 (4)C7—H70.9300
Zn1—O32.017 (4)C13—H130.9300
Zn1—O72.001 (4)C17—O51.424 (8)
Zn1—N22.069 (5)C17—H17A0.9600
Zn1—N32.021 (5)C17—H17B0.9600
Lu1—H11.79 (6)C17—H17C0.9600
O9—N11.259 (7)C18—H18A0.9600
C16—O31.321 (6)C18—H18B0.9600
C16—C151.403 (8)C18—H18C0.9600
C16—C111.412 (7)C4—H40.9300
N3—C101.271 (9)O7—N41.272 (7)
N3—C91.489 (8)O1—C191.416 (8)
C1—O21.327 (7)O1—H10.91 (2)
C1—C61.400 (8)O6—N41.257 (7)
C1—C21.402 (9)O12—N51.264 (7)
C15—C141.375 (8)O13—N51.264 (7)
C15—O51.376 (7)N5—O141.202 (7)
O10—N11.269 (7)N4—O81.517 (9)
N1—O111.213 (7)C9—C81.531 (11)
O4—C21.374 (8)C9—H9A0.9700
O4—C181.440 (8)C9—H9B0.9700
N2—C71.260 (9)C8—H8A0.9700
N2—C81.459 (8)C8—H8B0.9700
C2—C31.394 (8)C19—H19A0.9600
C12—C131.372 (11)C19—H19B0.9600
C12—C111.404 (9)C19—H19C0.9600
C12—H120.9300
O6—Lu1—O274.58 (15)C8—N2—Zn1113.7 (4)
O6—Lu1—O375.68 (14)O4—C2—C3125.1 (6)
O2—Lu1—O367.64 (13)O4—C2—C1113.4 (5)
O6—Lu1—O1145.94 (14)C3—C2—C1121.5 (6)
O2—Lu1—O176.13 (15)C13—C12—C11121.1 (6)
O3—Lu1—O177.39 (14)C13—C12—H12119.5
O6—Lu1—O973.13 (15)C11—C12—H12119.5
O2—Lu1—O9123.42 (15)C1—C6—C5118.2 (7)
O3—Lu1—O9141.30 (14)C1—C6—C7124.4 (6)
O1—Lu1—O9139.19 (14)C5—C6—C7117.4 (6)
O6—Lu1—O1071.59 (16)C12—C11—C16119.5 (6)
O2—Lu1—O10145.56 (16)C12—C11—C10115.7 (6)
O3—Lu1—O1097.50 (14)C16—C11—C10124.7 (6)
O1—Lu1—O10132.82 (15)C4—C3—C2119.1 (7)
O9—Lu1—O1050.98 (14)C4—C3—H3120.5
O6—Lu1—O13139.06 (15)C2—C3—H3120.5
O2—Lu1—O13144.78 (15)C15—C14—C13119.9 (6)
O3—Lu1—O13121.81 (14)C15—C14—H14120.1
O1—Lu1—O1373.83 (15)C13—C14—H14120.1
O9—Lu1—O1372.64 (15)C4—C5—C6122.2 (7)
O10—Lu1—O1369.62 (16)C4—C5—H5118.9
O6—Lu1—O12133.99 (16)C6—C5—H5118.9
O2—Lu1—O12102.71 (14)N3—C10—C11125.0 (5)
O3—Lu1—O12147.06 (14)N3—C10—H10117.5
O1—Lu1—O1269.69 (15)C11—C10—H10117.5
O9—Lu1—O1270.97 (15)N2—C7—C6124.0 (6)
O10—Lu1—O12105.23 (15)N2—C7—H7118.0
O13—Lu1—O1249.32 (14)C6—C7—H7118.0
O6—Lu1—O478.92 (16)C12—C13—C14119.9 (6)
O2—Lu1—O458.84 (13)C12—C13—H13120.0
O3—Lu1—O4125.00 (13)C14—C13—H13120.0
O1—Lu1—O4100.30 (15)O5—C17—H17A109.5
O9—Lu1—O470.16 (14)O5—C17—H17B109.5
O10—Lu1—O4119.20 (15)H17A—C17—H17B109.5
O13—Lu1—O4109.33 (13)O5—C17—H17C109.5
O12—Lu1—O462.46 (14)H17A—C17—H17C109.5
O6—Lu1—O5107.77 (15)H17B—C17—H17C109.5
O2—Lu1—O5122.51 (12)O4—C18—H18A109.5
O3—Lu1—O558.40 (12)O4—C18—H18B109.5
O1—Lu1—O574.38 (14)H18A—C18—H18B109.5
O9—Lu1—O5111.08 (13)O4—C18—H18C109.5
O10—Lu1—O563.94 (14)H18A—C18—H18C109.5
O13—Lu1—O565.56 (13)H18B—C18—H18C109.5
O12—Lu1—O5111.37 (14)C5—C4—C3120.3 (6)
O4—Lu1—O5173.31 (13)C5—C4—H4119.9
O6—Lu1—H1159 (2)C3—C4—H4119.9
O2—Lu1—H192.7 (16)C16—O3—Zn1126.7 (3)
O3—Lu1—H184 (2)C16—O3—Lu1133.2 (3)
O1—Lu1—H116.5 (16)Zn1—O3—Lu1100.03 (15)
O9—Lu1—H1127.8 (19)C1—O2—Zn1120.2 (4)
O10—Lu1—H1117.4 (17)C1—O2—Lu1132.7 (4)
O13—Lu1—H158.1 (17)Zn1—O2—Lu1100.56 (15)
O12—Lu1—H165 (2)N4—O7—Zn1117.8 (4)
O4—Lu1—H1109 (2)C15—O5—C17115.4 (5)
O5—Lu1—H165 (2)C15—O5—Lu1117.0 (3)
O7—Zn1—O3103.10 (17)C17—O5—Lu1126.1 (4)
O7—Zn1—N3104.4 (2)C19—O1—Lu1124.2 (4)
O3—Zn1—N390.3 (2)C19—O1—H1136 (4)
O7—Zn1—O2103.56 (17)Lu1—O1—H134 (5)
O3—Zn1—O282.30 (16)N4—O6—Lu1147.7 (4)
N3—Zn1—O2152.0 (2)N5—O12—Lu196.9 (3)
O7—Zn1—N2115.71 (19)N5—O13—Lu197.9 (3)
O3—Zn1—N2141.2 (2)O14—N5—O12121.7 (6)
N3—Zn1—N280.5 (2)O14—N5—O13122.4 (6)
O2—Zn1—N288.42 (19)O12—N5—O13115.8 (5)
N1—O9—Lu197.3 (3)O6—N4—O7123.4 (5)
O3—C16—C15117.4 (5)O6—N4—O8117.7 (5)
O3—C16—C11125.1 (6)O7—N4—O8118.8 (6)
C15—C16—C11117.5 (5)N3—C9—C8106.3 (5)
C10—N3—C9121.3 (5)N3—C9—H9A110.5
C10—N3—Zn1128.0 (4)C8—C9—H9A110.5
C9—N3—Zn1110.1 (4)N3—C9—H9B110.5
O2—C1—C6123.9 (6)C8—C9—H9B110.5
O2—C1—C2117.6 (5)H9A—C9—H9B108.7
C6—C1—C2118.5 (5)N2—C8—C9109.1 (5)
C14—C15—O5124.1 (6)N2—C8—H8A109.9
C14—C15—C16122.1 (6)C9—C8—H8A109.9
O5—C15—C16113.9 (5)N2—C8—H8B109.9
N1—O10—Lu195.3 (3)C9—C8—H8B109.9
O11—N1—O9122.7 (6)H8A—C8—H8B108.3
O11—N1—O10120.9 (6)O1—C19—H19A109.5
O9—N1—O10116.4 (5)O1—C19—H19B109.5
C2—O4—C18115.9 (5)H19A—C19—H19B109.5
C2—O4—Lu1116.7 (3)O1—C19—H19C109.5
C18—O4—Lu1127.3 (4)H19A—C19—H19C109.5
C7—N2—C8120.5 (6)H19B—C19—H19C109.5
C7—N2—Zn1125.7 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C10—H10···O12i0.932.533.443 (7)168
C12—H12···O9i0.932.583.445 (8)154
C17—H17B···O100.962.583.043 (9)110
C17—H17B···O130.962.422.993 (8)118
C18—H18B···O90.962.473.125 (9)126
C19—H19C···O120.962.443.079 (9)124
Symmetry code: (i) x+1/2, −y+1/2, z+1/2.

Experimental details

Crystal data
Chemical formula[LuZn(C18H18N2O4)(NO3)3(CH4O)]
Mr784.76
Crystal system, space groupMonoclinic, P21/n
Temperature (K)293
a, b, c (Å)9.6105 (11), 13.7179 (16), 19.851 (2)
β (°) 91.559 (2)
V (Å3)2616.2 (5)
Z4
Radiation typeMo Kα
µ (mm−1)4.75
Crystal size (mm)0.22 × 0.11 × 0.06
Data collection
DiffractometerBruker APEX II area-detector
Absorption correctionMulti-scan
(SADABS; Bruker, 2004)
Tmin, Tmax0.422, 0.764
No. of measured, independent and
observed [I > 2σ(I)] reflections		18694, 6348, 4676
Rint0.036
(sin θ/λ)max (Å−1)0.668
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.045, 0.147, 1.01
No. of reflections6348
No. of parameters367
No. of restraints1
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)1.89, −1.24

Computer programs: APEX2 (Bruker, 2004), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), APEX2 and publCIF (Westrip, 2007).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C10—H10···O12i0.932.533.443 (7)167.6
C12—H12···O9i0.932.583.445 (8)154.1
Symmetry code: (i) x+1/2, −y+1/2, z+1/2.
 

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