Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053681102890X/ng5198sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053681102890X/ng5198Isup2.hkl |
CCDC reference: 842760
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.008 Å
- R factor = 0.041
- wR factor = 0.078
- Data-to-parameter ratio = 16.9
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O5
Alert level C PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Gd1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C23 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C26 PLAT910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 8 PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 10 PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 35
Alert level G PLAT005_ALERT_5_G No _iucr_refine_instructions_details in CIF .... ? PLAT153_ALERT_1_G The su's on the Cell Axes are Equal .......... 0.00300 Ang. PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature 293 K
0 ALERT level A = Most likely a serious problem - resolve or explain 1 ALERT level B = A potentially serious problem, consider carefully 8 ALERT level C = Check. Ensure it is not caused by an omission or oversight 4 ALERT level G = General information/check it is not something unexpected 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
The salen lignad was synthesized following the reference (Costes et al. 2000). To a 1:1 MeOH/CH2Cl2 solution (20 ml) of H2L (0.0748 g, 0.2 mmol) andGd(CH3COO)3˙4H2O (0.0813 g, 0.2 mmol) was added a MeOH solution (5 ml) ofZn(CH3COO)2˙2H2O (0.0438 g, 0.2 mmol) at the ambient temperature. The color of the solution immediately changed to yellow. After stirring for 8 h, the solution was filtered to remove the suspended particles. yellow single crystals suitable for X-ray diffraction were obtained by slow diffusion of diethylether into the filtrate in four days. ZnGd(C22H18N2O4)(CH3COO)3, Elemental Anal. Calc.: C, 43.44; H, 3.52; N, 3.62 wt%, Found: C, 43.38; H, 3.44; N, 3.27 wt%.
The anormal reflection data (-1 1 4) have been omitted during the refinement. H atoms bound to C atoms were placed in calculated positions and treated as riding on their parent atoms, with C—H = 0.93 Å (aromatic C) and Uiso(H) = 1.2Ueq(C), and with C—H = 0.96 Å (methyl C) and Uiso(H) = 1.5Ueq(C).
Data collection: RAPID-AUTO (Rigaku 1998); cell refinement: RAPID-AUTO (Rigaku 1998); data reduction: CrystalClear (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).
Fig. 1. The molecular structure of the title compound, showing 50% probability displacement ellipsoids. |
[GdZn(C22H18N2O4)(C2H3O2)3] | F(000) = 1532 |
Mr = 774.16 | Dx = 1.803 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 16409 reflections |
a = 14.012 (3) Å | θ = 3.0–27.5° |
b = 13.581 (3) Å | µ = 3.21 mm−1 |
c = 15.426 (3) Å | T = 293 K |
β = 103.65 (3)° | Block, yellow |
V = 2852.6 (10) Å3 | 0.15 × 0.14 × 0.13 mm |
Z = 4 |
Rigaku R-AXIS RAPID diffractometer | 6488 independent reflections |
Radiation source: fine-focus sealed tube | 4513 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.073 |
ω scan | θmax = 27.5°, θmin = 3.0° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −18→18 |
Tmin = 0.645, Tmax = 0.681 | k = −17→16 |
26483 measured reflections | l = −19→18 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.041 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.078 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0272P)2 + 1.1216P] where P = (Fo2 + 2Fc2)/3 |
6488 reflections | (Δ/σ)max < 0.001 |
384 parameters | Δρmax = 0.59 e Å−3 |
0 restraints | Δρmin = −0.82 e Å−3 |
[GdZn(C22H18N2O4)(C2H3O2)3] | V = 2852.6 (10) Å3 |
Mr = 774.16 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 14.012 (3) Å | µ = 3.21 mm−1 |
b = 13.581 (3) Å | T = 293 K |
c = 15.426 (3) Å | 0.15 × 0.14 × 0.13 mm |
β = 103.65 (3)° |
Rigaku R-AXIS RAPID diffractometer | 6488 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 4513 reflections with I > 2σ(I) |
Tmin = 0.645, Tmax = 0.681 | Rint = 0.073 |
26483 measured reflections |
R[F2 > 2σ(F2)] = 0.041 | 0 restraints |
wR(F2) = 0.078 | H-atom parameters constrained |
S = 1.01 | Δρmax = 0.59 e Å−3 |
6488 reflections | Δρmin = −0.82 e Å−3 |
384 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Gd1 | 0.298502 (17) | 0.880640 (16) | 0.188340 (16) | 0.03607 (7) | |
Zn1 | 0.05908 (4) | 0.84037 (4) | 0.19232 (4) | 0.03815 (14) | |
O1 | 0.4228 (3) | 0.9767 (3) | 0.2964 (3) | 0.0660 (12) | |
O2 | 0.4373 (3) | 0.8188 (3) | 0.3022 (3) | 0.0696 (12) | |
O3 | 0.1371 (2) | 0.9446 (2) | 0.1482 (2) | 0.0457 (8) | |
O4 | 0.2720 (3) | 1.0662 (2) | 0.1405 (2) | 0.0469 (8) | |
O5 | 0.2482 (3) | 0.8884 (4) | 0.3247 (3) | 0.0844 (14) | |
O6 | 0.1715 (2) | 0.7605 (2) | 0.1712 (2) | 0.0448 (9) | |
O7 | 0.3403 (2) | 0.6960 (2) | 0.1719 (2) | 0.0459 (9) | |
O8 | 0.2722 (3) | 0.8700 (3) | 0.0262 (2) | 0.0581 (10) | |
O9 | 0.4224 (3) | 0.8956 (3) | 0.1017 (3) | 0.0594 (10) | |
O10 | 0.0909 (3) | 0.8682 (2) | 0.3216 (2) | 0.0495 (9) | |
N1 | −0.0301 (3) | 0.7181 (3) | 0.1660 (3) | 0.0426 (10) | |
N2 | −0.0693 (3) | 0.9076 (3) | 0.1312 (3) | 0.0406 (9) | |
C1 | −0.2061 (4) | 0.6805 (5) | 0.1540 (4) | 0.0594 (15) | |
H1A | −0.1919 | 0.6148 | 0.1686 | 0.071* | |
C2 | −0.3228 (4) | 0.8097 (6) | 0.1166 (4) | 0.0722 (18) | |
H2A | −0.3877 | 0.8308 | 0.1047 | 0.087* | |
C3 | 0.1527 (5) | 1.1987 (3) | 0.0881 (3) | 0.0528 (14) | |
H3A | 0.2012 | 1.2443 | 0.0847 | 0.063* | |
C4 | −0.0760 (4) | 0.9959 (3) | 0.0987 (3) | 0.0441 (12) | |
H4A | −0.1388 | 1.0190 | 0.0729 | 0.053* | |
C5 | 0.4366 (4) | 0.6643 (4) | 0.1674 (5) | 0.0705 (18) | |
H5A | 0.4329 | 0.6302 | 0.1122 | 0.106* | |
H5B | 0.4626 | 0.6208 | 0.2164 | 0.106* | |
H5C | 0.4788 | 0.7205 | 0.1707 | 0.106* | |
C6 | 0.5288 (6) | 0.9052 (5) | 0.4231 (4) | 0.095 (3) | |
H6A | 0.5924 | 0.8835 | 0.4180 | 0.142* | |
H6B | 0.5060 | 0.8634 | 0.4642 | 0.142* | |
H6C | 0.5331 | 0.9718 | 0.4445 | 0.142* | |
C7 | −0.3015 (5) | 0.7124 (5) | 0.1369 (4) | 0.0728 (18) | |
H7A | −0.3517 | 0.6683 | 0.1390 | 0.087* | |
C8 | 0.2713 (4) | 0.6248 (3) | 0.1765 (3) | 0.0399 (11) | |
C9 | 0.0535 (5) | 1.2258 (4) | 0.0651 (4) | 0.0602 (16) | |
H9A | 0.0361 | 1.2898 | 0.0466 | 0.072* | |
C10 | 0.1059 (4) | 1.0339 (3) | 0.1223 (3) | 0.0373 (11) | |
C11 | −0.0183 (4) | 1.1587 (4) | 0.0697 (4) | 0.0550 (15) | |
H11A | −0.0838 | 1.1777 | 0.0532 | 0.066* | |
C12 | 0.1196 (5) | 0.4954 (3) | 0.1731 (4) | 0.0541 (14) | |
H12A | 0.0680 | 0.4512 | 0.1691 | 0.065* | |
C13 | 0.3513 (4) | 1.1311 (4) | 0.1360 (4) | 0.0594 (15) | |
H13A | 0.3416 | 1.1567 | 0.0765 | 0.089* | |
H13B | 0.4122 | 1.0956 | 0.1513 | 0.089* | |
H13C | 0.3531 | 1.1845 | 0.1771 | 0.089* | |
C14 | −0.1514 (4) | 0.8451 (4) | 0.1298 (3) | 0.0459 (12) | |
C15 | 0.0052 (4) | 1.0620 (3) | 0.0987 (3) | 0.0426 (12) | |
C16 | 0.2889 (4) | 0.5246 (3) | 0.1824 (3) | 0.0512 (13) | |
H16A | 0.3522 | 0.5005 | 0.1880 | 0.061* | |
C17 | −0.2486 (4) | 0.8776 (5) | 0.1134 (4) | 0.0600 (14) | |
H17A | −0.2638 | 0.9435 | 0.1005 | 0.072* | |
C18 | 0.1774 (4) | 1.1038 (3) | 0.1156 (3) | 0.0395 (11) | |
C19 | −0.1301 (4) | 0.7453 (4) | 0.1496 (3) | 0.0457 (12) | |
C20 | 0.0996 (4) | 0.5986 (3) | 0.1719 (3) | 0.0424 (12) | |
C21 | −0.0006 (4) | 0.6290 (4) | 0.1625 (3) | 0.0510 (13) | |
H21A | −0.0482 | 0.5798 | 0.1531 | 0.061* | |
C22 | 0.3616 (4) | 0.8806 (4) | 0.0284 (4) | 0.0524 (13) | |
C23 | 0.4599 (4) | 0.9003 (4) | 0.3355 (4) | 0.0498 (13) | |
C24 | 0.2012 (5) | 0.8960 (5) | 0.4602 (4) | 0.0749 (18) | |
H24A | 0.2498 | 0.9466 | 0.4778 | 0.112* | |
H24B | 0.2257 | 0.8352 | 0.4886 | 0.112* | |
H24C | 0.1423 | 0.9144 | 0.4777 | 0.112* | |
C25 | 0.2112 (5) | 0.4601 (4) | 0.1798 (4) | 0.0632 (16) | |
H25A | 0.2223 | 0.3925 | 0.1827 | 0.076* | |
C26 | 0.1791 (4) | 0.8833 (4) | 0.3610 (3) | 0.0516 (13) | |
C27 | 0.1785 (4) | 0.6639 (3) | 0.1738 (3) | 0.0385 (11) | |
C28 | 0.3968 (5) | 0.8751 (5) | −0.0560 (4) | 0.084 (2) | |
H28A | 0.4423 | 0.9277 | −0.0570 | 0.125* | |
H28B | 0.3419 | 0.8811 | −0.1064 | 0.125* | |
H28C | 0.4289 | 0.8131 | −0.0586 | 0.125* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Gd1 | 0.02645 (12) | 0.03976 (12) | 0.04177 (14) | −0.00167 (10) | 0.00757 (9) | −0.00027 (11) |
Zn1 | 0.0263 (3) | 0.0438 (3) | 0.0441 (3) | 0.0004 (2) | 0.0079 (2) | −0.0002 (2) |
O1 | 0.071 (3) | 0.054 (2) | 0.065 (3) | −0.028 (2) | 0.000 (2) | 0.0017 (19) |
O2 | 0.068 (3) | 0.062 (2) | 0.064 (3) | 0.008 (2) | −0.014 (2) | −0.0066 (19) |
O3 | 0.030 (2) | 0.0417 (18) | 0.065 (2) | 0.0033 (14) | 0.0124 (17) | 0.0161 (15) |
O4 | 0.041 (2) | 0.0432 (18) | 0.057 (2) | −0.0066 (15) | 0.0117 (17) | 0.0041 (15) |
O5 | 0.045 (3) | 0.166 (4) | 0.044 (2) | −0.021 (3) | 0.014 (2) | −0.010 (3) |
O6 | 0.034 (2) | 0.0337 (18) | 0.070 (3) | −0.0015 (14) | 0.0186 (18) | −0.0013 (15) |
O7 | 0.0256 (19) | 0.0440 (18) | 0.066 (2) | 0.0072 (14) | 0.0074 (16) | −0.0030 (15) |
O8 | 0.041 (2) | 0.090 (3) | 0.044 (2) | 0.004 (2) | 0.0114 (17) | −0.0026 (18) |
O9 | 0.036 (2) | 0.087 (3) | 0.057 (3) | −0.0017 (19) | 0.0137 (19) | 0.001 (2) |
O10 | 0.036 (2) | 0.070 (2) | 0.043 (2) | 0.0000 (17) | 0.0112 (16) | 0.0014 (16) |
N1 | 0.031 (2) | 0.054 (2) | 0.044 (3) | −0.0075 (18) | 0.0116 (19) | −0.0008 (18) |
N2 | 0.033 (2) | 0.051 (2) | 0.037 (2) | 0.0069 (17) | 0.0061 (18) | −0.0012 (17) |
C1 | 0.041 (4) | 0.088 (4) | 0.051 (4) | −0.013 (3) | 0.016 (3) | 0.000 (3) |
C2 | 0.022 (3) | 0.134 (6) | 0.061 (4) | −0.009 (3) | 0.010 (3) | −0.007 (4) |
C3 | 0.070 (4) | 0.039 (3) | 0.047 (3) | 0.000 (3) | 0.008 (3) | 0.002 (2) |
C4 | 0.034 (3) | 0.062 (3) | 0.036 (3) | 0.017 (2) | 0.008 (2) | −0.005 (2) |
C5 | 0.028 (3) | 0.069 (4) | 0.112 (6) | 0.011 (3) | 0.014 (3) | −0.010 (3) |
C6 | 0.096 (6) | 0.110 (5) | 0.064 (5) | −0.045 (5) | −0.008 (4) | −0.005 (4) |
C7 | 0.040 (4) | 0.110 (5) | 0.068 (5) | −0.022 (3) | 0.012 (3) | 0.000 (4) |
C8 | 0.046 (3) | 0.036 (2) | 0.036 (3) | 0.001 (2) | 0.007 (2) | −0.0035 (19) |
C9 | 0.078 (5) | 0.038 (3) | 0.060 (4) | 0.014 (3) | 0.008 (3) | 0.001 (2) |
C10 | 0.040 (3) | 0.038 (2) | 0.032 (3) | 0.006 (2) | 0.007 (2) | −0.0005 (18) |
C11 | 0.050 (4) | 0.050 (3) | 0.058 (4) | 0.017 (3) | 0.000 (3) | −0.002 (2) |
C12 | 0.067 (4) | 0.041 (3) | 0.057 (4) | −0.011 (3) | 0.020 (3) | 0.001 (2) |
C13 | 0.051 (4) | 0.063 (3) | 0.063 (4) | −0.017 (3) | 0.010 (3) | 0.012 (3) |
C14 | 0.028 (3) | 0.069 (3) | 0.039 (3) | −0.001 (2) | 0.005 (2) | −0.005 (2) |
C15 | 0.042 (3) | 0.048 (3) | 0.036 (3) | 0.011 (2) | 0.005 (2) | −0.002 (2) |
C16 | 0.058 (4) | 0.046 (3) | 0.050 (3) | 0.015 (3) | 0.014 (3) | 0.006 (2) |
C17 | 0.038 (3) | 0.090 (4) | 0.050 (3) | 0.007 (3) | 0.007 (3) | −0.002 (3) |
C18 | 0.045 (3) | 0.040 (3) | 0.031 (3) | 0.004 (2) | 0.006 (2) | −0.0037 (18) |
C19 | 0.029 (3) | 0.066 (3) | 0.041 (3) | −0.010 (2) | 0.007 (2) | −0.004 (2) |
C20 | 0.050 (3) | 0.041 (3) | 0.038 (3) | −0.005 (2) | 0.016 (2) | 0.0008 (19) |
C21 | 0.054 (4) | 0.051 (3) | 0.051 (3) | −0.017 (3) | 0.018 (3) | 0.000 (2) |
C22 | 0.046 (3) | 0.059 (3) | 0.056 (4) | 0.009 (3) | 0.020 (3) | 0.002 (3) |
C23 | 0.036 (3) | 0.066 (4) | 0.047 (3) | −0.015 (3) | 0.008 (2) | 0.002 (3) |
C24 | 0.067 (5) | 0.114 (5) | 0.043 (4) | −0.003 (4) | 0.011 (3) | −0.002 (3) |
C25 | 0.079 (5) | 0.041 (3) | 0.071 (4) | 0.004 (3) | 0.019 (4) | 0.006 (3) |
C26 | 0.049 (4) | 0.066 (3) | 0.038 (3) | 0.001 (3) | 0.006 (3) | −0.001 (2) |
C27 | 0.044 (3) | 0.035 (2) | 0.038 (3) | −0.001 (2) | 0.013 (2) | 0.0001 (19) |
C28 | 0.078 (5) | 0.120 (5) | 0.061 (4) | 0.023 (4) | 0.032 (4) | −0.006 (4) |
Gd1—O3 | 2.365 (3) | C4—C15 | 1.449 (7) |
Gd1—O5 | 2.373 (4) | C4—H4A | 0.9300 |
Gd1—O6 | 2.382 (3) | C5—H5A | 0.9600 |
Gd1—O9 | 2.436 (4) | C5—H5B | 0.9600 |
Gd1—O2 | 2.441 (4) | C5—H5C | 0.9600 |
Gd1—O8 | 2.445 (4) | C6—C23 | 1.465 (8) |
Gd1—O1 | 2.479 (4) | C6—H6A | 0.9600 |
Gd1—O7 | 2.601 (3) | C6—H6B | 0.9600 |
Gd1—O4 | 2.627 (3) | C6—H6C | 0.9600 |
Gd1—C22 | 2.810 (6) | C7—H7A | 0.9300 |
Gd1—C23 | 2.814 (5) | C8—C16 | 1.382 (6) |
Gd1—Zn1 | 3.4139 (9) | C8—C27 | 1.395 (6) |
Zn1—O10 | 1.975 (3) | C9—C11 | 1.371 (8) |
Zn1—O6 | 2.002 (3) | C9—H9A | 0.9300 |
Zn1—O3 | 2.003 (3) | C10—C18 | 1.402 (6) |
Zn1—N2 | 2.039 (4) | C10—C15 | 1.425 (6) |
Zn1—N1 | 2.060 (4) | C11—C15 | 1.401 (6) |
O1—C23 | 1.250 (6) | C11—H11A | 0.9300 |
O2—C23 | 1.230 (6) | C12—C25 | 1.351 (8) |
O3—C10 | 1.319 (5) | C12—C20 | 1.429 (6) |
O4—C18 | 1.387 (6) | C12—H12A | 0.9300 |
O4—C13 | 1.434 (6) | C13—H13A | 0.9600 |
O5—C26 | 1.230 (7) | C13—H13B | 0.9600 |
O6—C27 | 1.315 (5) | C13—H13C | 0.9600 |
O7—C8 | 1.382 (5) | C14—C17 | 1.397 (7) |
O7—C5 | 1.433 (6) | C14—C19 | 1.406 (7) |
O8—C22 | 1.253 (6) | C16—C25 | 1.390 (8) |
O9—C22 | 1.261 (6) | C16—H16A | 0.9300 |
O10—C26 | 1.259 (6) | C17—H17A | 0.9300 |
N1—C21 | 1.284 (6) | C20—C27 | 1.413 (6) |
N1—C19 | 1.413 (6) | C20—C21 | 1.438 (7) |
N2—C4 | 1.295 (6) | C21—H21A | 0.9300 |
N2—C14 | 1.427 (6) | C22—C28 | 1.499 (8) |
C1—C7 | 1.370 (8) | C24—C26 | 1.498 (7) |
C1—C19 | 1.396 (7) | C24—H24A | 0.9600 |
C1—H1A | 0.9300 | C24—H24B | 0.9600 |
C2—C7 | 1.375 (8) | C24—H24C | 0.9600 |
C2—C17 | 1.398 (8) | C25—H25A | 0.9300 |
C2—H2A | 0.9300 | C28—H28A | 0.9600 |
C3—C18 | 1.376 (6) | C28—H28B | 0.9600 |
C3—C9 | 1.400 (8) | C28—H28C | 0.9600 |
C3—H3A | 0.9300 | ||
O3—Gd1—O5 | 75.50 (14) | C7—C1—C19 | 120.8 (6) |
O3—Gd1—O6 | 65.12 (10) | C7—C1—H1A | 119.6 |
O5—Gd1—O6 | 76.04 (13) | C19—C1—H1A | 119.6 |
O3—Gd1—O9 | 125.94 (12) | C7—C2—C17 | 121.3 (6) |
O5—Gd1—O9 | 151.85 (14) | C7—C2—H2A | 119.4 |
O6—Gd1—O9 | 127.31 (12) | C17—C2—H2A | 119.4 |
O3—Gd1—O2 | 149.88 (14) | C18—C3—C9 | 119.1 (5) |
O5—Gd1—O2 | 74.38 (16) | C18—C3—H3A | 120.4 |
O6—Gd1—O2 | 106.97 (12) | C9—C3—H3A | 120.4 |
O9—Gd1—O2 | 82.74 (14) | N2—C4—C15 | 126.0 (4) |
O3—Gd1—O8 | 81.38 (13) | N2—C4—H4A | 117.0 |
O5—Gd1—O8 | 154.78 (14) | C15—C4—H4A | 117.0 |
O6—Gd1—O8 | 85.25 (12) | O7—C5—H5A | 109.5 |
O9—Gd1—O8 | 53.03 (13) | O7—C5—H5B | 109.5 |
O2—Gd1—O8 | 128.15 (14) | H5A—C5—H5B | 109.5 |
O3—Gd1—O1 | 117.37 (13) | O7—C5—H5C | 109.5 |
O5—Gd1—O1 | 71.90 (14) | H5A—C5—H5C | 109.5 |
O6—Gd1—O1 | 145.40 (12) | H5B—C5—H5C | 109.5 |
O9—Gd1—O1 | 81.16 (13) | C23—C6—H6A | 109.5 |
O2—Gd1—O1 | 51.91 (13) | C23—C6—H6B | 109.5 |
O8—Gd1—O1 | 129.16 (13) | H6A—C6—H6B | 109.5 |
O3—Gd1—O7 | 123.52 (10) | C23—C6—H6C | 109.5 |
O5—Gd1—O7 | 104.50 (14) | H6A—C6—H6C | 109.5 |
O6—Gd1—O7 | 60.56 (10) | H6B—C6—H6C | 109.5 |
O9—Gd1—O7 | 79.67 (12) | C1—C7—C2 | 119.8 (6) |
O2—Gd1—O7 | 65.11 (11) | C1—C7—H7A | 120.1 |
O8—Gd1—O7 | 79.98 (11) | C2—C7—H7A | 120.1 |
O1—Gd1—O7 | 115.73 (12) | O7—C8—C16 | 125.2 (5) |
O3—Gd1—O4 | 60.72 (10) | O7—C8—C27 | 113.0 (4) |
O5—Gd1—O4 | 98.87 (14) | C16—C8—C27 | 121.8 (5) |
O6—Gd1—O4 | 124.96 (11) | C11—C9—C3 | 120.6 (5) |
O9—Gd1—O4 | 80.67 (12) | C11—C9—H9A | 119.7 |
O2—Gd1—O4 | 124.60 (12) | C3—C9—H9A | 119.7 |
O8—Gd1—O4 | 78.02 (11) | O3—C10—C18 | 117.0 (4) |
O1—Gd1—O4 | 73.41 (12) | O3—C10—C15 | 124.1 (4) |
O7—Gd1—O4 | 156.55 (11) | C18—C10—C15 | 118.8 (4) |
O3—Gd1—C22 | 104.47 (14) | C9—C11—C15 | 121.3 (5) |
O5—Gd1—C22 | 177.28 (16) | C9—C11—H11A | 119.3 |
O6—Gd1—C22 | 106.46 (15) | C15—C11—H11A | 119.3 |
O9—Gd1—C22 | 26.62 (14) | C25—C12—C20 | 121.9 (5) |
O2—Gd1—C22 | 105.62 (16) | C25—C12—H12A | 119.0 |
O8—Gd1—C22 | 26.43 (14) | C20—C12—H12A | 119.0 |
O1—Gd1—C22 | 105.89 (16) | O4—C13—H13A | 109.5 |
O7—Gd1—C22 | 77.82 (13) | O4—C13—H13B | 109.5 |
O4—Gd1—C22 | 78.86 (13) | H13A—C13—H13B | 109.5 |
O3—Gd1—C23 | 135.50 (14) | O4—C13—H13C | 109.5 |
O5—Gd1—C23 | 68.36 (15) | H13A—C13—H13C | 109.5 |
O6—Gd1—C23 | 126.30 (13) | H13B—C13—H13C | 109.5 |
O9—Gd1—C23 | 83.90 (14) | C17—C14—C19 | 119.5 (5) |
O2—Gd1—C23 | 25.85 (13) | C17—C14—N2 | 124.3 (5) |
O8—Gd1—C23 | 136.84 (14) | C19—C14—N2 | 116.2 (4) |
O1—Gd1—C23 | 26.35 (12) | C11—C15—C10 | 118.4 (5) |
O7—Gd1—C23 | 90.78 (13) | C11—C15—C4 | 117.1 (5) |
O4—Gd1—C23 | 99.73 (13) | C10—C15—C4 | 124.4 (4) |
C22—Gd1—C23 | 110.42 (16) | C8—C16—C25 | 119.5 (5) |
O3—Gd1—Zn1 | 34.95 (7) | C8—C16—H16A | 120.3 |
O5—Gd1—Zn1 | 59.49 (10) | C25—C16—H16A | 120.3 |
O6—Gd1—Zn1 | 35.01 (7) | C14—C17—C2 | 119.1 (6) |
O9—Gd1—Zn1 | 148.60 (9) | C14—C17—H17A | 120.5 |
O2—Gd1—Zn1 | 123.47 (11) | C2—C17—H17A | 120.5 |
O8—Gd1—Zn1 | 95.59 (10) | C3—C18—O4 | 125.9 (5) |
O1—Gd1—Zn1 | 127.58 (10) | C3—C18—C10 | 121.7 (5) |
O7—Gd1—Zn1 | 95.30 (7) | O4—C18—C10 | 112.5 (4) |
O4—Gd1—Zn1 | 94.82 (8) | C1—C19—C14 | 119.5 (5) |
C22—Gd1—Zn1 | 121.98 (13) | C1—C19—N1 | 124.2 (5) |
C23—Gd1—Zn1 | 127.37 (11) | C14—C19—N1 | 116.2 (4) |
O10—Zn1—O6 | 105.65 (14) | C27—C20—C12 | 117.8 (5) |
O10—Zn1—O3 | 101.36 (14) | C27—C20—C21 | 124.3 (4) |
O6—Zn1—O3 | 79.28 (13) | C12—C20—C21 | 117.8 (5) |
O10—Zn1—N2 | 110.22 (15) | N1—C21—C20 | 125.6 (5) |
O6—Zn1—N2 | 144.04 (15) | N1—C21—H21A | 117.2 |
O3—Zn1—N2 | 91.09 (15) | C20—C21—H21A | 117.2 |
O10—Zn1—N1 | 109.55 (15) | O8—C22—O9 | 120.1 (5) |
O6—Zn1—N1 | 89.71 (14) | O8—C22—C28 | 120.2 (5) |
O3—Zn1—N1 | 148.98 (15) | O9—C22—C28 | 119.7 (5) |
N2—Zn1—N1 | 80.92 (16) | O8—C22—Gd1 | 60.3 (3) |
O10—Zn1—Gd1 | 89.96 (10) | O9—C22—Gd1 | 59.9 (3) |
O6—Zn1—Gd1 | 43.06 (9) | C28—C22—Gd1 | 177.1 (4) |
O3—Zn1—Gd1 | 42.55 (9) | O2—C23—O1 | 120.5 (5) |
N2—Zn1—Gd1 | 133.10 (12) | O2—C23—C6 | 118.3 (5) |
N1—Zn1—Gd1 | 132.72 (12) | O1—C23—C6 | 121.1 (5) |
C23—O1—Gd1 | 92.0 (3) | O2—C23—Gd1 | 59.9 (3) |
C23—O2—Gd1 | 94.3 (3) | O1—C23—Gd1 | 61.7 (3) |
C10—O3—Zn1 | 125.8 (3) | C6—C23—Gd1 | 167.8 (5) |
C10—O3—Gd1 | 130.2 (3) | C26—C24—H24A | 109.5 |
Zn1—O3—Gd1 | 102.50 (12) | C26—C24—H24B | 109.5 |
C18—O4—C13 | 117.4 (4) | H24A—C24—H24B | 109.5 |
C18—O4—Gd1 | 119.6 (3) | C26—C24—H24C | 109.5 |
C13—O4—Gd1 | 122.9 (3) | H24A—C24—H24C | 109.5 |
C26—O5—Gd1 | 146.3 (4) | H24B—C24—H24C | 109.5 |
C27—O6—Zn1 | 126.2 (3) | C12—C25—C16 | 120.1 (5) |
C27—O6—Gd1 | 129.1 (3) | C12—C25—H25A | 119.9 |
Zn1—O6—Gd1 | 101.93 (12) | C16—C25—H25A | 119.9 |
C8—O7—C5 | 118.1 (4) | O5—C26—O10 | 125.3 (5) |
C8—O7—Gd1 | 119.5 (3) | O5—C26—C24 | 117.6 (5) |
C5—O7—Gd1 | 122.1 (3) | O10—C26—C24 | 117.0 (5) |
C22—O8—Gd1 | 93.3 (3) | O6—C27—C8 | 116.3 (4) |
C22—O9—Gd1 | 93.5 (3) | O6—C27—C20 | 125.0 (4) |
C26—O10—Zn1 | 118.7 (3) | C8—C27—C20 | 118.7 (4) |
C21—N1—C19 | 123.6 (4) | C22—C28—H28A | 109.5 |
C21—N1—Zn1 | 125.6 (4) | C22—C28—H28B | 109.5 |
C19—N1—Zn1 | 110.7 (3) | H28A—C28—H28B | 109.5 |
C4—N2—C14 | 124.1 (4) | C22—C28—H28C | 109.5 |
C4—N2—Zn1 | 124.7 (3) | H28A—C28—H28C | 109.5 |
C14—N2—Zn1 | 111.2 (3) | H28B—C28—H28C | 109.5 |
Experimental details
Crystal data | |
Chemical formula | [GdZn(C22H18N2O4)(C2H3O2)3] |
Mr | 774.16 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 14.012 (3), 13.581 (3), 15.426 (3) |
β (°) | 103.65 (3) |
V (Å3) | 2852.6 (10) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 3.21 |
Crystal size (mm) | 0.15 × 0.14 × 0.13 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID diffractometer |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.645, 0.681 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 26483, 6488, 4513 |
Rint | 0.073 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.078, 1.01 |
No. of reflections | 6488 |
No. of parameters | 384 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.59, −0.82 |
Computer programs: RAPID-AUTO (Rigaku 1998), CrystalClear (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
Lanthanide complexes with spectroscopic and magnetic properties are currently of considerable interest. In continuation of our studies of salen-type lanthanide complexes (Bao et al., 2010, Xu et al., 2011), we present here the synthesis and the crystal structure of the title compound.
In the title compound,the Zn(II) ion is five-coordinated by two imino nitrogen atoms and two phenolate oxygen atoms from the ligand, and one oxygen from the bridging acetate group to form the pyramid coordination geometry. The Zn—N bond distances are in the range of 2.042 (4) Å—2.062 (4) Å, and the Zn—O bond distances are in the range of 1.974 (3) Å—2.004 (3) Å, which in accordance with the reported values (Liao et al. 2010). The Gd(III) ion is ligated to five oxygen atoms of three acetate groups, and four oxygen atoms from the ligand. The Gd—O bond distances are in the range of 2.365 (3)—2.626 (3) Å (Fig.1, Table 1). The Gd—Zn distance is 3.414 (1) Å. The positive charge of the Gd(III) and Zn(II) ions are balanced by the ligand L2- and three acetate groups (L = N,N'-bis(2-oxy-3-methoxybenzylidene)- 1,2-diaminobenzene).