supplementary materials
Bis{6,6'-dimethoxy-2,2'-[ethane-1,2-diylbis(iminomethylene)]diphenolato(1.5-)-
4O,N,N',O'}erbium(III)
A solution of 6,6'-dimethoxy-2,2'-(ethane-1,2-diyldiiminodimethylene) diphenol
(0.328 g, 2 mmol) in ethanol (20 ml), and then a solution of
Er(NO3)3.6H2O (0.461 g, 1 mmol) in ethanol (10 ml) was added. The
reaction mixture was stirred for 3 h in the air and then filtered. X-ray
quality crystals of (I) were obtained by evaporation of an ethanol solution.
The space group was uniquely assigned from the systematic absences. All H atoms
were located in difference Fourier maps. H atoms bonded to C, O and N atoms
were treated as riding atoms, with C—H distances of 0.93 Å (aryl), 0.96 Å (methyl), 0.97Å (methylene) and N—H distances of 0.90 Å (amino),
Uiso(H) = 1.2Ueq(aryl, methylene, NH) or 1.5Ueq(C)
(methyl or OH). The H1 bonded to O1 is disordered and were refined with the
occupancies ties to 0.5.
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT (Siemens, 1996); 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: SHELXTL (Sheldrick, 2008).
Bis{6,6'-dimethoxy-2,2'-[ethane-1,2-diylbis(iminomethylene)]diphenolato(1.5-)-
κ4O,
N,
N',
O'}erbium(III)
top
Crystal data top
| [Er(C18H22.5N2O4)2] | F(000) = 1684 |
| Mr = 829.02 | Dx = 1.586 Mg m−3 |
| Orthorhombic, Iba2 | Mo Kα radiation, λ = 0.71073 Å |
| Hall symbol: I 2 -2c | Cell parameters from 4129 reflections |
| a = 11.1542 (10) Å | θ = 2.9–25.7° |
| b = 21.958 (2) Å | µ = 2.48 mm−1 |
| c = 14.1751 (15) Å | T = 298 K |
| V = 3471.8 (6) Å3 | Block, brown |
| Z = 4 | 0.20 × 0.15 × 0.14 mm |
Data collection top
Siemens SMART 1000 CCD area-detector diffractometer | 3007 independent reflections |
| Radiation source: fine-focus sealed tube | 2199 reflections with I > 2σ(I) |
| graphite | Rint = 0.031 |
| φ and ω scans | θmax = 25.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→10 |
| Tmin = 0.637, Tmax = 0.723 | k = −20→26 |
| 7986 measured reflections | l = −16→16 |
Refinement top
| Refinement on F2 | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
| R[F2 > 2σ(F2)] = 0.044 | H-atom parameters constrained |
| wR(F2) = 0.162 | w = 1/[σ2(Fo2) + (0.1143P)2 + 1.9553P] where P = (Fo2 + 2Fc2)/3 |
| S = 1.06 | (Δ/σ)max = 0.001 |
| 3007 reflections | Δρmax = 0.75 e Å−3 |
| 224 parameters | Δρmin = −1.42 e Å−3 |
| 1 restraint | Absolute structure: Flack (1983), 1400 Freidel pairs |
| Primary atom site location: structure-invariant direct methods | Flack parameter: 0.02 (5) |
Crystal data top
| [Er(C18H22.5N2O4)2] | V = 3471.8 (6) Å3 |
| Mr = 829.02 | Z = 4 |
| Orthorhombic, Iba2 | Mo Kα radiation |
| a = 11.1542 (10) Å | µ = 2.48 mm−1 |
| b = 21.958 (2) Å | T = 298 K |
| c = 14.1751 (15) Å | 0.20 × 0.15 × 0.14 mm |
Data collection top
Siemens SMART 1000 CCD area-detector diffractometer | 3007 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 2199 reflections with I > 2σ(I) |
| Tmin = 0.637, Tmax = 0.723 | Rint = 0.031 |
| 7986 measured reflections | θmax = 25.0° |
Refinement top
| R[F2 > 2σ(F2)] = 0.044 | H-atom parameters constrained |
| wR(F2) = 0.162 | Δρmax = 0.75 e Å−3 |
| S = 1.06 | Δρmin = −1.42 e Å−3 |
| 3007 reflections | Absolute structure: Flack (1983), 1400 Freidel pairs |
| 224 parameters | Flack parameter: 0.02 (5) |
| 1 restraint | |
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| | x | y | z | Uiso*/Ueq | Occ. (<1) |
| Er1 | 1.0000 | 1.0000 | 0.0158 (2) | 0.0342 (2) | |
| O1 | 0.9418 (5) | 1.0681 (3) | 0.1202 (4) | 0.0297 (13) | |
| H1 | 0.9919 | 1.0955 | 0.1209 | 0.045* | 0.50 |
| O2 | 0.9141 (6) | 1.1865 (3) | 0.0933 (5) | 0.0479 (18) | |
| O3 | 1.1356 (6) | 0.9653 (3) | −0.0834 (5) | 0.0389 (16) | |
| O4 | 1.3687 (7) | 0.9386 (4) | −0.0660 (7) | 0.065 (3) | |
| N1 | 0.7906 (7) | 0.9657 (4) | 0.0823 (6) | 0.040 (2) | |
| H1C | 0.7358 | 0.9838 | 0.0439 | 0.048* | |
| N2 | 0.9283 (8) | 0.8957 (4) | −0.0492 (6) | 0.043 (2) | |
| H2 | 0.9673 | 0.8670 | −0.0146 | 0.052* | |
| C1 | 0.7624 (12) | 0.9901 (6) | 0.1789 (10) | 0.049 (3) | |
| H1A | 0.6906 | 0.9706 | 0.2029 | 0.058* | |
| H1B | 0.8279 | 0.9809 | 0.2216 | 0.058* | |
| C2 | 0.7440 (9) | 1.0568 (5) | 0.1748 (7) | 0.042 (3) | |
| C3 | 0.8366 (9) | 1.0926 (5) | 0.1404 (7) | 0.039 (3) | |
| C4 | 0.8159 (9) | 1.1552 (5) | 0.1290 (7) | 0.041 (2) | |
| C5 | 0.7089 (10) | 1.1808 (6) | 0.1508 (8) | 0.051 (3) | |
| H5 | 0.6957 | 1.2223 | 0.1429 | 0.061* | |
| C6 | 0.6169 (10) | 1.1415 (7) | 0.1866 (9) | 0.056 (3) | |
| H6 | 0.5428 | 1.1582 | 0.2021 | 0.067* | |
| C7 | 0.6330 (9) | 1.0854 (7) | 0.1977 (9) | 0.057 (3) | |
| H7 | 0.5708 | 1.0618 | 0.2216 | 0.068* | |
| C8 | 0.8935 (13) | 1.2474 (5) | 0.0637 (10) | 0.064 (3) | |
| H8A | 0.8112 | 1.2519 | 0.0451 | 0.095* | |
| H8B | 0.9447 | 1.2567 | 0.0112 | 0.095* | |
| H8C | 0.9107 | 1.2747 | 0.1149 | 0.095* | |
| C9 | 0.9606 (16) | 0.8829 (7) | −0.1469 (9) | 0.061 (4) | |
| H9A | 0.9455 | 0.9184 | −0.1860 | 0.073* | |
| H9B | 0.9135 | 0.8492 | −0.1709 | 0.073* | |
| C10 | 1.0949 (14) | 0.8668 (6) | −0.1482 (8) | 0.054 (3) | |
| C11 | 1.1731 (11) | 0.9109 (5) | −0.1134 (7) | 0.043 (3) | |
| C12 | 1.2992 (13) | 0.8958 (6) | −0.1052 (8) | 0.056 (3) | |
| C13 | 1.3345 (14) | 0.8375 (6) | −0.1369 (9) | 0.063 (4) | |
| H13 | 1.4149 | 0.8264 | −0.1333 | 0.076* | |
| C14 | 1.2544 (16) | 0.7976 (7) | −0.1721 (10) | 0.070 (4) | |
| H14 | 1.2804 | 0.7590 | −0.1897 | 0.084* | |
| C15 | 1.1369 (14) | 0.8120 (6) | −0.1826 (9) | 0.066 (4) | |
| H15 | 1.0850 | 0.7852 | −0.2128 | 0.079* | |
| C16 | 1.4901 (11) | 0.9202 (11) | −0.0443 (19) | 0.092 (7) | |
| H16A | 1.5326 | 0.9538 | −0.0167 | 0.139* | |
| H16B | 1.5298 | 0.9078 | −0.1013 | 0.139* | |
| H16C | 1.4885 | 0.8868 | −0.0007 | 0.139* | |
| C17 | 0.7704 (9) | 0.9017 (5) | 0.0703 (9) | 0.051 (3) | |
| H17A | 0.6876 | 0.8920 | 0.0849 | 0.061* | |
| H17B | 0.8216 | 0.8789 | 0.1127 | 0.061* | |
| C18 | 0.7979 (11) | 0.8845 (5) | −0.0316 (10) | 0.052 (3) | |
| H18A | 0.7792 | 0.8419 | −0.0422 | 0.063* | |
| H18B | 0.7498 | 0.9089 | −0.0743 | 0.063* | |
Atomic displacement parameters (Å2) top| | U11 | U22 | U33 | U12 | U13 | U23 |
| Er1 | 0.0382 (3) | 0.0267 (3) | 0.0377 (3) | 0.0000 (2) | 0.000 | 0.000 |
| O1 | 0.018 (3) | 0.033 (4) | 0.038 (3) | 0.003 (3) | 0.005 (3) | −0.004 (3) |
| O2 | 0.053 (4) | 0.035 (4) | 0.055 (4) | 0.009 (3) | 0.001 (3) | −0.007 (3) |
| O3 | 0.056 (4) | 0.026 (4) | 0.034 (4) | 0.014 (3) | 0.011 (3) | −0.001 (3) |
| O4 | 0.055 (5) | 0.055 (6) | 0.085 (7) | 0.019 (4) | 0.031 (4) | 0.023 (5) |
| N1 | 0.031 (4) | 0.038 (5) | 0.052 (5) | −0.009 (4) | −0.007 (4) | 0.012 (4) |
| N2 | 0.051 (6) | 0.026 (4) | 0.052 (5) | −0.003 (4) | −0.024 (4) | 0.003 (4) |
| C1 | 0.041 (6) | 0.055 (8) | 0.050 (7) | −0.002 (5) | 0.001 (5) | 0.017 (5) |
| C2 | 0.032 (5) | 0.048 (7) | 0.046 (6) | 0.008 (5) | 0.005 (4) | 0.005 (5) |
| C3 | 0.036 (6) | 0.045 (7) | 0.036 (6) | 0.005 (5) | −0.009 (4) | −0.003 (5) |
| C4 | 0.043 (6) | 0.041 (6) | 0.040 (5) | 0.010 (5) | −0.008 (5) | −0.004 (5) |
| C5 | 0.046 (6) | 0.051 (7) | 0.055 (7) | 0.018 (6) | −0.003 (5) | −0.006 (5) |
| C6 | 0.042 (7) | 0.066 (9) | 0.060 (8) | 0.019 (6) | 0.007 (5) | 0.007 (6) |
| C7 | 0.036 (6) | 0.071 (10) | 0.063 (8) | 0.006 (6) | 0.015 (5) | 0.010 (7) |
| C8 | 0.079 (9) | 0.025 (6) | 0.087 (9) | −0.003 (6) | 0.010 (7) | 0.008 (6) |
| C9 | 0.086 (9) | 0.045 (8) | 0.052 (8) | −0.001 (7) | −0.019 (7) | −0.007 (6) |
| C10 | 0.084 (9) | 0.036 (6) | 0.043 (6) | 0.015 (6) | −0.005 (6) | −0.003 (5) |
| C11 | 0.063 (8) | 0.041 (7) | 0.024 (6) | 0.021 (6) | 0.007 (5) | 0.010 (5) |
| C12 | 0.076 (9) | 0.047 (7) | 0.045 (6) | 0.029 (7) | 0.021 (6) | 0.011 (6) |
| C13 | 0.084 (10) | 0.051 (9) | 0.056 (8) | 0.034 (8) | 0.022 (7) | 0.011 (6) |
| C14 | 0.104 (12) | 0.049 (8) | 0.057 (8) | 0.024 (8) | 0.011 (7) | −0.003 (7) |
| C15 | 0.105 (12) | 0.045 (8) | 0.047 (7) | 0.019 (7) | −0.005 (7) | −0.011 (6) |
| C16 | 0.060 (10) | 0.089 (15) | 0.128 (17) | 0.026 (7) | 0.030 (8) | 0.031 (13) |
| C17 | 0.037 (6) | 0.040 (7) | 0.075 (10) | −0.011 (5) | −0.017 (6) | 0.013 (6) |
| C18 | 0.057 (7) | 0.023 (6) | 0.076 (8) | −0.016 (5) | −0.029 (6) | 0.011 (5) |
Geometric parameters (Å, °) top
| Er1—O3i | 2.202 (6) | C5—C6 | 1.433 (19) |
| Er1—O3 | 2.202 (6) | C5—H5 | 0.9300 |
| Er1—O1 | 2.203 (6) | C6—C7 | 1.254 (19) |
| Er1—O1i | 2.203 (6) | C6—H6 | 0.9300 |
| Er1—N2 | 2.595 (8) | C7—H7 | 0.9300 |
| Er1—N2i | 2.595 (8) | C8—H8A | 0.9600 |
| Er1—N1i | 2.628 (8) | C8—H8B | 0.9600 |
| Er1—N1 | 2.628 (8) | C8—H8C | 0.9600 |
| O1—C3 | 1.321 (12) | C9—C10 | 1.54 (2) |
| O1—H1 | 0.8200 | C9—H9A | 0.9700 |
| O2—C4 | 1.389 (13) | C9—H9B | 0.9700 |
| O2—C8 | 1.419 (14) | C10—C15 | 1.379 (17) |
| O3—C11 | 1.334 (13) | C10—C11 | 1.394 (19) |
| O4—C12 | 1.340 (16) | C11—C12 | 1.450 (17) |
| O4—C16 | 1.446 (16) | C12—C13 | 1.412 (17) |
| N1—C17 | 1.433 (14) | C13—C14 | 1.35 (2) |
| N1—C1 | 1.504 (16) | C13—H13 | 0.9300 |
| N1—H1C | 0.9094 | C14—C15 | 1.36 (2) |
| N2—C9 | 1.458 (16) | C14—H14 | 0.9300 |
| N2—C18 | 1.495 (15) | C15—H15 | 0.9300 |
| N2—H2 | 0.9105 | C16—H16A | 0.9600 |
| C1—C2 | 1.479 (15) | C16—H16B | 0.9600 |
| C1—H1A | 0.9700 | C16—H16C | 0.9600 |
| C1—H1B | 0.9700 | C17—C18 | 1.523 (17) |
| C2—C3 | 1.387 (15) | C17—H17A | 0.9700 |
| C2—C7 | 1.426 (15) | C17—H17B | 0.9700 |
| C3—C4 | 1.404 (15) | C18—H18A | 0.9700 |
| C4—C5 | 1.355 (15) | C18—H18B | 0.9700 |
| | | |
| O3i—Er1—O3 | 100.6 (4) | C5—C4—C3 | 121.7 (11) |
| O3i—Er1—O1 | 89.5 (2) | O2—C4—C3 | 113.4 (8) |
| O3—Er1—O1 | 150.1 (2) | C4—C5—C6 | 117.5 (12) |
| O3i—Er1—O1i | 150.1 (2) | C4—C5—H5 | 121.3 |
| O3—Er1—O1i | 89.5 (2) | C6—C5—H5 | 121.3 |
| O1—Er1—O1i | 95.6 (3) | C7—C6—C5 | 122.2 (11) |
| O3i—Er1—N2 | 82.4 (3) | C7—C6—H6 | 118.9 |
| O3—Er1—N2 | 71.3 (3) | C5—C6—H6 | 118.9 |
| O1—Er1—N2 | 138.4 (3) | C6—C7—C2 | 121.9 (12) |
| O1i—Er1—N2 | 74.3 (2) | C6—C7—H7 | 119.1 |
| O3i—Er1—N2i | 71.3 (3) | C2—C7—H7 | 119.1 |
| O3—Er1—N2i | 82.4 (3) | O2—C8—H8A | 109.5 |
| O1—Er1—N2i | 74.3 (2) | O2—C8—H8B | 109.5 |
| O1i—Er1—N2i | 138.4 (3) | H8A—C8—H8B | 109.5 |
| N2—Er1—N2i | 138.4 (4) | O2—C8—H8C | 109.5 |
| O3i—Er1—N1i | 137.8 (3) | H8A—C8—H8C | 109.5 |
| O3—Er1—N1i | 73.6 (2) | H8B—C8—H8C | 109.5 |
| O1—Er1—N1i | 80.0 (2) | N2—C9—C10 | 107.3 (10) |
| O1i—Er1—N1i | 72.0 (2) | N2—C9—H9A | 110.3 |
| N2—Er1—N1i | 130.8 (3) | C10—C9—H9A | 110.3 |
| N2i—Er1—N1i | 66.5 (3) | N2—C9—H9B | 110.3 |
| O3i—Er1—N1 | 73.6 (2) | C10—C9—H9B | 110.3 |
| O3—Er1—N1 | 137.8 (3) | H9A—C9—H9B | 108.5 |
| O1—Er1—N1 | 72.0 (2) | C15—C10—C11 | 121.3 (13) |
| O1i—Er1—N1 | 80.0 (2) | C15—C10—C9 | 122.4 (12) |
| N2—Er1—N1 | 66.5 (3) | C11—C10—C9 | 116.4 (10) |
| N2i—Er1—N1 | 130.8 (3) | O3—C11—C10 | 122.6 (10) |
| N1i—Er1—N1 | 138.0 (4) | O3—C11—C12 | 118.9 (11) |
| C3—O1—Er1 | 133.1 (6) | C10—C11—C12 | 118.4 (11) |
| C3—O1—H1 | 107.7 | O4—C12—C13 | 127.4 (13) |
| Er1—O1—H1 | 107.7 | O4—C12—C11 | 115.7 (10) |
| C4—O2—C8 | 116.5 (9) | C13—C12—C11 | 116.9 (14) |
| C11—O3—Er1 | 136.7 (7) | C14—C13—C12 | 121.5 (14) |
| C12—O4—C16 | 115.7 (13) | C14—C13—H13 | 119.3 |
| C17—N1—C1 | 115.1 (9) | C12—C13—H13 | 119.3 |
| C17—N1—Er1 | 112.2 (6) | C13—C14—C15 | 121.9 (13) |
| C1—N1—Er1 | 114.2 (7) | C13—C14—H14 | 119.0 |
| C17—N1—H1C | 104.5 | C15—C14—H14 | 119.0 |
| C1—N1—H1C | 104.4 | C14—C15—C10 | 119.6 (14) |
| Er1—N1—H1C | 105.0 | C14—C15—H15 | 120.2 |
| C9—N2—C18 | 111.6 (10) | C10—C15—H15 | 120.2 |
| C9—N2—Er1 | 115.5 (8) | O4—C16—H16A | 109.5 |
| C18—N2—Er1 | 112.7 (6) | O4—C16—H16B | 109.5 |
| C9—N2—H2 | 105.1 | H16A—C16—H16B | 109.5 |
| C18—N2—H2 | 105.1 | O4—C16—H16C | 109.5 |
| Er1—N2—H2 | 105.8 | H16A—C16—H16C | 109.5 |
| C2—C1—N1 | 110.2 (9) | H16B—C16—H16C | 109.5 |
| C2—C1—H1A | 109.6 | N1—C17—C18 | 108.9 (9) |
| N1—C1—H1A | 109.6 | N1—C17—H17A | 109.9 |
| C2—C1—H1B | 109.6 | C18—C17—H17A | 109.9 |
| N1—C1—H1B | 109.6 | N1—C17—H17B | 109.9 |
| H1A—C1—H1B | 108.1 | C18—C17—H17B | 109.9 |
| C3—C2—C7 | 118.5 (11) | H17A—C17—H17B | 108.3 |
| C3—C2—C1 | 118.1 (10) | N2—C18—C17 | 108.3 (8) |
| C7—C2—C1 | 123.2 (10) | N2—C18—H18A | 110.0 |
| O1—C3—C2 | 120.5 (10) | C17—C18—H18A | 110.0 |
| O1—C3—C4 | 121.3 (9) | N2—C18—H18B | 110.0 |
| C2—C3—C4 | 118.2 (9) | C17—C18—H18B | 110.0 |
| C5—C4—O2 | 124.9 (10) | H18A—C18—H18B | 108.4 |
| | | |
| O3i—Er1—O1—C3 | 33.8 (8) | Er1—O1—C3—C2 | 64.0 (13) |
| O3—Er1—O1—C3 | 144.6 (8) | Er1—O1—C3—C4 | −116.8 (9) |
| O1i—Er1—O1—C3 | −116.7 (9) | C7—C2—C3—O1 | 178.5 (10) |
| N2—Er1—O1—C3 | −44.0 (10) | C1—C2—C3—O1 | −6.0 (15) |
| N2i—Er1—O1—C3 | 104.5 (9) | C7—C2—C3—C4 | −0.7 (15) |
| N1i—Er1—O1—C3 | 172.7 (9) | C1—C2—C3—C4 | 174.8 (10) |
| N1—Er1—O1—C3 | −39.1 (8) | C8—O2—C4—C5 | −10.6 (15) |
| O3i—Er1—O3—C11 | −106.2 (10) | C8—O2—C4—C3 | 168.9 (10) |
| O1—Er1—O3—C11 | 145.9 (9) | O1—C3—C4—C5 | −179.0 (10) |
| O1i—Er1—O3—C11 | 45.5 (10) | C2—C3—C4—C5 | 0.2 (16) |
| N2—Er1—O3—C11 | −28.1 (9) | O1—C3—C4—O2 | 1.5 (14) |
| N2i—Er1—O3—C11 | −175.4 (10) | C2—C3—C4—O2 | −179.3 (9) |
| N1i—Er1—O3—C11 | 116.9 (10) | O2—C4—C5—C6 | 179.7 (10) |
| N1—Er1—O3—C11 | −29.0 (11) | C3—C4—C5—C6 | 0.2 (17) |
| O3i—Er1—N1—C17 | 107.2 (7) | C4—C5—C6—C7 | 0(2) |
| O3—Er1—N1—C17 | 19.4 (8) | C5—C6—C7—C2 | 0(2) |
| O1—Er1—N1—C17 | −157.9 (7) | C3—C2—C7—C6 | 0.9 (18) |
| O1i—Er1—N1—C17 | −58.7 (7) | C1—C2—C7—C6 | −174.4 (13) |
| N2—Er1—N1—C17 | 18.5 (6) | C18—N2—C9—C10 | −154.4 (9) |
| N2i—Er1—N1—C17 | 153.1 (7) | Er1—N2—C9—C10 | 75.2 (10) |
| N1i—Er1—N1—C17 | −107.1 (7) | N2—C9—C10—C15 | 122.1 (13) |
| O3i—Er1—N1—C1 | −119.5 (7) | N2—C9—C10—C11 | −58.5 (14) |
| O3—Er1—N1—C1 | 152.8 (6) | Er1—O3—C11—C10 | 52.0 (14) |
| O1—Er1—N1—C1 | −24.5 (7) | Er1—O3—C11—C12 | −124.9 (10) |
| O1i—Er1—N1—C1 | 74.7 (7) | C15—C10—C11—O3 | 177.0 (10) |
| N2—Er1—N1—C1 | 151.9 (7) | C9—C10—C11—O3 | −2.4 (16) |
| N2i—Er1—N1—C1 | −73.6 (8) | C15—C10—C11—C12 | −6.0 (17) |
| N1i—Er1—N1—C1 | 26.3 (6) | C9—C10—C11—C12 | 174.5 (9) |
| O3i—Er1—N2—C9 | 69.5 (9) | C16—O4—C12—C13 | −7.5 (19) |
| O3—Er1—N2—C9 | −34.5 (9) | C16—O4—C12—C11 | 170.7 (12) |
| O1—Er1—N2—C9 | 150.1 (8) | O3—C11—C12—O4 | 0.9 (14) |
| O1i—Er1—N2—C9 | −129.4 (9) | C10—C11—C12—O4 | −176.1 (11) |
| N2i—Er1—N2—C9 | 19.2 (8) | O3—C11—C12—C13 | 179.3 (10) |
| N1i—Er1—N2—C9 | −81.1 (9) | C10—C11—C12—C13 | 2.3 (15) |
| N1—Er1—N2—C9 | 144.9 (9) | O4—C12—C13—C14 | 177.5 (12) |
| O3i—Er1—N2—C18 | −60.3 (7) | C11—C12—C13—C14 | −0.7 (17) |
| O3—Er1—N2—C18 | −164.3 (7) | C12—C13—C14—C15 | 3(2) |
| O1—Er1—N2—C18 | 20.2 (8) | C13—C14—C15—C10 | −6(2) |
| O1i—Er1—N2—C18 | 100.8 (7) | C11—C10—C15—C14 | 8(2) |
| N2i—Er1—N2—C18 | −110.7 (7) | C9—C10—C15—C14 | −172.5 (12) |
| N1i—Er1—N2—C18 | 149.1 (6) | C1—N1—C17—C18 | 177.7 (9) |
| N1—Er1—N2—C18 | 15.1 (6) | Er1—N1—C17—C18 | −49.4 (9) |
| C17—N1—C1—C2 | −159.7 (9) | C9—N2—C18—C17 | −177.3 (10) |
| Er1—N1—C1—C2 | 68.3 (10) | Er1—N2—C18—C17 | −45.5 (9) |
| N1—C1—C2—C3 | −58.1 (13) | N1—C17—C18—N2 | 63.8 (10) |
| N1—C1—C2—C7 | 117.1 (12) | | |
| Symmetry codes: (i) −x+2, −y+2, z. |
Hydrogen-bond geometry (Å, °) top
| D—H···A | D—H | H···A | D···A | D—H···A |
| C16—H16A···O4ii | 0.96 | 2.70 | 3.49 (3) | 140 |
| N2—H2···O2i | 0.91 | 2.34 | 3.230 (10) | 166 |
| N1—H1C···O4i | 0.91 | 2.59 | 3.462 (12) | 162 |
| O1—H1···O2 | 0.82 | 2.21 | 2.646 (9) | 113 |
| Symmetry codes: (ii) −x+3, −y+2, z; (i) −x+2, −y+2, z. |
Table 1
Selected geometric parameters (Å) top| Er1—O3i | 2.202 (6) | Er1—N2 | 2.595 (8) |
| Er1—O3 | 2.202 (6) | Er1—N2i | 2.595 (8) |
| Er1—O1 | 2.203 (6) | Er1—N1i | 2.628 (8) |
| Er1—O1i | 2.203 (6) | Er1—N1 | 2.628 (8) |
| Symmetry codes: (i) −x+2, −y+2, z. |
Table 2
Hydrogen-bond geometry (Å, °) top
| D—H···A | D—H | H···A | D···A | D—H···A |
| C16—H16A···O4ii | 0.96 | 2.70 | 3.49 (3) | 140 |
| N2—H2···O2i | 0.91 | 2.34 | 3.230 (10) | 166 |
| N1—H1C···O4i | 0.91 | 2.59 | 3.462 (12) | 162 |
| O1—H1···O2 | 0.82 | 2.21 | 2.646 (9) | 113 |
| Symmetry codes: (ii) −x+3, −y+2, z; (i) −x+2, −y+2, z. |
We acknowledge the financial support of the Huaihai Institute of Technology
Science Foundation.
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Diamine derivatives are potentially multidentate ligands. We have recently reported the crystal structure (C18H24O2N4) (II) (Xia et al., 2006) which is the ligand of the title compound and a complex [Ce(C18H22N2O4)2] (III) (Liu et al., 2007). We report here the crystal structure of new rare earth complex (I).
In the title complex (I), the coordination environment of the Er atom and coordination modes of (I) ligands to ErIII ion is in agreement with the complexes reported above (Fig. 1). The average bond lengths of between the Erbium center oxygen atoms are 2.203 (6)Å and nitrogen atom are 2.612 (8) Å, longer than the 2.199 (4)Å and shorter than the 2.624 (4)Å of complexes (III), respectively. The dihedral angles between phenyl ring (C2-C7 ring) and anotother phenyl ring are 42.20 (28)°(C10—C15 ring), 42.29 (26)°(C2A—C7A ring) and 15.47 (43)°(C10A—C15A ring) [symmetry codes: (A) 2 - x, 2 - y, z].
In (I), the Er atom is eight-coordinated by four O atoms and four N atoms from two 6,6'-dimethoxy-2,2'-(ethane-1,2-diyldiiminodimethylene)diphenol. The molecules are linked into a chain parallel to the a axis by one C—H···O hydrogen bond. Neighbouring chains are connected by van der Waals forces, resulting in a three-dimensional network.