Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807032916/ci2404sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807032916/ci2404Isup2.hkl |
CCDC reference: 657564
The Schiff base used to make the title compound was synthesized by the condensation of 3-ethoxysalicylaldehyde and 1,2- diaminopropane in a 2:1 molar ratio. Copper diacetate monohydrate (0.17 g, 1 mmol) and the ligand (0.37 g, 1 mmol) were heated in methanol (50 ml) for 3 h. Lutetium nitrate hexahydrate (0.47 g, 1 mmol) was added and the mixture was heated for another 3 h. Cooling the solution gave a precipitate, which was collected and washed with diethyl ether. Crystals were obtained upon recrystallization from methanol.
The part of the Schiff base that is made up of the C10 and C11 atoms (that belong to the cyclic system) is disordered over two positions; the occupancies of each set of atoms was arbitrarily fixed as 0.5. The displacement parameters of primed atoms were set to those of the unprimed ones. The C10—C11 and C11—C12 bond lengths were restrained to 1.50 (1) Å and the C10···C12 distance to 2.45 (1) Å. The displacement parameters of C10, C11 and C12 were restrained to approximate isotropic behaviour. The carbon- and oxygen-bound H atoms were positioned geometrically (C–H = 0.93–0.97 Å and O—H = 0.82 Å), and were included in the refinement in the riding model approximation, with Uiso(H) = 1.2–1.5Ueq(C,O). The final difference Fourier map had a large peak at 0.5 Å from H12D and a deep hole at 0.5 Å from Lu1.
3-Alkoxysalicylaldehyde condenses with ethylenediamine and related diamines to form a class of Schiff bases that react with divalent transition-metal salts to afford another class of compounds that react with lanthanum(III) salts to yield bimetallic compounds. Bis(2-oxy-3-methoxybenzylidene)ethylenediamine)(acetone)tris(nitrato)-copper- neodymium (Elmali et al., 2004), bis(2-oxy-3-methoxybenzylidene)ethylenediamine)(acetone)tris(nitrato)-copper- dysprosium (Elmali et al., 2005) and (1,2-cyclohexane)bis(3-ethoxysalicylideneaminato)aquatris(nitrato)χoppergadolinium (Koner et al., 2005) represent the copper compounds that are coordinated to lanthanum trinitrate. Their copper atoms are chelated by the deprotonated Schiff bases but the geometry is a square-pyramid owing to the coordinated solvent molecules. On the other hand, the lanthanum atom is chelated by three nitrate groups, so a ten-coordinate geometry results from the involvement of the four oxygen atoms of the copper-Schiff base portion of the bimetallic molecule. The title compound (Fig. 1) has a similar bonding mode; the lutetium atom shows bicapped square-antiprismatic coordination.
See Elmali & Elerman (2004) for bis(2-oxy-3-methoxybenzylidene)ethylenediamine)(acetone)tris(nitrato)copperneodymium, Elmali & Elerman (2005) for bis(2-oxy-3-methoxybenzylidene)ethylenediamine)(acetone)tris(nitrato)copperdysprosium and Koner et al. (2005) for (1,2-cyclohexane)bis(3-ethoxysalicylideneaminato)aquatris(nitrato)coppergadolinium.
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).
[CuLu(C21H22N2O4)(CH4O)(NO3)3] | F(000) = 1628 |
Mr = 825.00 | Dx = 1.865 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 4544 reflections |
a = 9.1795 (5) Å | θ = 2.4–22.2° |
b = 20.407 (1) Å | µ = 4.14 mm−1 |
c = 15.7058 (9) Å | T = 295 K |
β = 93.126 (1)° | Block, red |
V = 2937.7 (3) Å3 | 0.20 × 0.09 × 0.08 mm |
Z = 4 |
Bruker APEXII area-detector diffractometer | 6636 independent reflections |
Radiation source: fine-focus sealed tube | 3788 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.049 |
φ and ω scans | θmax = 27.5°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −11→11 |
Tmin = 0.183, Tmax = 0.733 | k = −26→26 |
21167 measured reflections | l = −20→20 |
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)] = 0.059 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.196 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.1059P)2] where P = (Fo2 + 2Fc2)/3 |
6636 reflections | (Δ/σ)max = 0.001 |
394 parameters | Δρmax = 1.20 e Å−3 |
10 restraints | Δρmin = −1.29 e Å−3 |
[CuLu(C21H22N2O4)(CH4O)(NO3)3] | V = 2937.7 (3) Å3 |
Mr = 825.00 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 9.1795 (5) Å | µ = 4.14 mm−1 |
b = 20.407 (1) Å | T = 295 K |
c = 15.7058 (9) Å | 0.20 × 0.09 × 0.08 mm |
β = 93.126 (1)° |
Bruker APEXII area-detector diffractometer | 6636 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3788 reflections with I > 2σ(I) |
Tmin = 0.183, Tmax = 0.733 | Rint = 0.049 |
21167 measured reflections |
R[F2 > 2σ(F2)] = 0.059 | 10 restraints |
wR(F2) = 0.196 | H-atom parameters constrained |
S = 1.07 | Δρmax = 1.20 e Å−3 |
6636 reflections | Δρmin = −1.29 e Å−3 |
394 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Lu1 | 0.36449 (5) | 0.34232 (2) | 0.25150 (3) | 0.05488 (19) | |
Cu1 | 0.32833 (12) | 0.50585 (5) | 0.30039 (7) | 0.0460 (3) | |
O1 | 0.1485 (8) | 0.3477 (3) | 0.1360 (4) | 0.0525 (16) | |
O2 | 0.2284 (7) | 0.4406 (3) | 0.2367 (4) | 0.0550 (16) | |
O3 | 0.4753 (7) | 0.4397 (3) | 0.3108 (4) | 0.0519 (16) | |
O4 | 0.6441 (7) | 0.3413 (3) | 0.2989 (4) | 0.0489 (15) | |
O5 | 0.4254 (11) | 0.5592 (4) | 0.1848 (5) | 0.101 (3) | |
H5O | 0.4865 | 0.5875 | 0.1969 | 0.122* | |
O6 | 0.1569 (10) | 0.3251 (5) | 0.3439 (6) | 0.097 (3) | |
O7 | 0.3518 (12) | 0.3407 (5) | 0.4097 (5) | 0.099 (3) | |
O8 | 0.1587 (12) | 0.3342 (4) | 0.4790 (6) | 0.093 (3) | |
O9 | 0.4776 (8) | 0.3859 (4) | 0.1229 (5) | 0.067 (2) | |
O10 | 0.4809 (9) | 0.2812 (4) | 0.1396 (5) | 0.071 (2) | |
O11 | 0.5937 (12) | 0.3224 (5) | 0.0349 (6) | 0.104 (3) | |
O12 | 0.2362 (8) | 0.2317 (3) | 0.2230 (6) | 0.075 (2) | |
O13 | 0.4277 (8) | 0.2285 (3) | 0.3023 (5) | 0.067 (2) | |
O14 | 0.3179 (10) | 0.1381 (3) | 0.2648 (6) | 0.086 (3) | |
N1 | 0.1675 (10) | 0.5659 (3) | 0.3038 (6) | 0.064 (2) | |
N2 | 0.4260 (9) | 0.5652 (3) | 0.3773 (5) | 0.053 (2) | |
N3 | 0.2196 (11) | 0.3338 (4) | 0.4138 (6) | 0.056 (2) | |
N4 | 0.5218 (12) | 0.3308 (5) | 0.0953 (7) | 0.070 (3) | |
N5 | 0.3281 (10) | 0.1984 (4) | 0.2624 (5) | 0.055 (2) | |
C1 | 0.1685 (19) | 0.3436 (7) | −0.0203 (8) | 0.107 (5) | |
H1A | 0.1514 | 0.3160 | −0.0693 | 0.160* | |
H1B | 0.2687 | 0.3574 | −0.0167 | 0.160* | |
H1C | 0.1062 | 0.3813 | −0.0253 | 0.160* | |
C2 | 0.1348 (14) | 0.3045 (5) | 0.0622 (6) | 0.069 (3) | |
H2A | 0.0367 | 0.2868 | 0.0565 | 0.082* | |
H2B | 0.2025 | 0.2681 | 0.0698 | 0.082* | |
C3 | 0.0473 (10) | 0.3983 (4) | 0.1446 (6) | 0.050 (2) | |
C4 | −0.0902 (14) | 0.3990 (6) | 0.1026 (7) | 0.081 (4) | |
H4 | −0.1196 | 0.3659 | 0.0647 | 0.097* | |
C5 | −0.1824 (13) | 0.4515 (7) | 0.1197 (8) | 0.086 (4) | |
H5 | −0.2774 | 0.4521 | 0.0959 | 0.103* | |
C6 | −0.1351 (12) | 0.5010 (5) | 0.1702 (8) | 0.070 (3) | |
H6 | −0.1970 | 0.5363 | 0.1781 | 0.084* | |
C7 | 0.0070 (10) | 0.5015 (5) | 0.2122 (7) | 0.056 (2) | |
C8 | 0.0955 (9) | 0.4482 (4) | 0.1980 (6) | 0.048 (2) | |
C9 | 0.0390 (13) | 0.5572 (5) | 0.2657 (7) | 0.063 (3) | |
H9 | −0.0338 | 0.5879 | 0.2735 | 0.076* | |
C10 | 0.2161 (17) | 0.6300 (6) | 0.3366 (12) | 0.053 (4) | 0.50 |
H10 | 0.2633 | 0.6537 | 0.2913 | 0.063* | 0.50 |
C10' | 0.187 (2) | 0.6104 (6) | 0.3762 (10) | 0.053 (4) | 0.50 |
H10' | 0.1607 | 0.5865 | 0.4273 | 0.063* | 0.50 |
C11 | 0.1109 (15) | 0.6748 (6) | 0.3762 (10) | 0.108 (5) | |
H11A | 0.1626 | 0.7116 | 0.4011 | 0.163* | 0.50 |
H11B | 0.0622 | 0.6517 | 0.4197 | 0.163* | 0.50 |
H11C | 0.0402 | 0.6899 | 0.3334 | 0.163* | 0.50 |
H11D | 0.0074 | 0.6677 | 0.3727 | 0.163* | 0.50 |
H11E | 0.1379 | 0.6985 | 0.4275 | 0.163* | 0.50 |
H11F | 0.1381 | 0.6996 | 0.3277 | 0.163* | 0.50 |
C12 | 0.328 (3) | 0.6153 (14) | 0.4072 (18) | 0.096 (8) | 0.50 |
H12A | 0.3824 | 0.6547 | 0.4226 | 0.115* | 0.50 |
H12B | 0.2805 | 0.5998 | 0.4570 | 0.115* | 0.50 |
C12' | 0.347 (2) | 0.6264 (10) | 0.386 (3) | 0.096 (8) | 0.50 |
H12C | 0.3728 | 0.6575 | 0.3429 | 0.115* | 0.50 |
H12D | 0.3696 | 0.6456 | 0.4419 | 0.115* | 0.50 |
C13 | 0.5558 (15) | 0.5608 (5) | 0.4052 (7) | 0.069 (3) | |
H13 | 0.5925 | 0.5951 | 0.4390 | 0.083* | |
C14 | 0.6568 (12) | 0.5056 (4) | 0.3894 (6) | 0.053 (2) | |
C15 | 0.7976 (13) | 0.5104 (5) | 0.4195 (6) | 0.068 (3) | |
H15 | 0.8283 | 0.5477 | 0.4494 | 0.081* | |
C16 | 0.8962 (11) | 0.4607 (5) | 0.4065 (6) | 0.057 (2) | |
H16 | 0.9939 | 0.4659 | 0.4242 | 0.068* | |
C17 | 0.8500 (11) | 0.4039 (5) | 0.3676 (6) | 0.058 (3) | |
H17 | 0.9161 | 0.3701 | 0.3597 | 0.070* | |
C18 | 0.7030 (10) | 0.3963 (4) | 0.3395 (6) | 0.046 (2) | |
C19 | 0.6058 (10) | 0.4479 (4) | 0.3458 (5) | 0.046 (2) | |
C20 | 0.7437 (10) | 0.2855 (5) | 0.2863 (7) | 0.062 (3) | |
H20A | 0.8354 | 0.3019 | 0.2670 | 0.075* | |
H20B | 0.7011 | 0.2570 | 0.2422 | 0.075* | |
C21 | 0.7735 (12) | 0.2457 (6) | 0.3676 (8) | 0.077 (3) | |
H21A | 0.7709 | 0.1998 | 0.3541 | 0.115* | |
H21B | 0.7004 | 0.2553 | 0.4072 | 0.115* | |
H21C | 0.8680 | 0.2569 | 0.3926 | 0.115* | |
C22 | 0.3956 (19) | 0.5501 (8) | 0.1039 (9) | 0.114 (5) | |
H22A | 0.4755 | 0.5654 | 0.0723 | 0.171* | |
H22B | 0.3088 | 0.5739 | 0.0865 | 0.171* | |
H22C | 0.3805 | 0.5042 | 0.0931 | 0.171* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Lu1 | 0.0553 (3) | 0.0411 (3) | 0.0676 (3) | 0.00042 (19) | −0.0023 (2) | −0.0050 (2) |
Cu1 | 0.0493 (7) | 0.0293 (5) | 0.0591 (7) | 0.0017 (5) | 0.0012 (5) | −0.0057 (5) |
O1 | 0.057 (4) | 0.041 (4) | 0.058 (4) | 0.000 (3) | −0.010 (3) | −0.003 (3) |
O2 | 0.054 (4) | 0.036 (3) | 0.074 (4) | 0.012 (3) | −0.006 (3) | −0.009 (3) |
O3 | 0.047 (4) | 0.036 (3) | 0.070 (4) | 0.008 (3) | −0.018 (3) | −0.012 (3) |
O4 | 0.047 (4) | 0.034 (3) | 0.065 (4) | −0.006 (3) | 0.001 (3) | −0.011 (3) |
O5 | 0.135 (9) | 0.086 (6) | 0.084 (6) | −0.053 (6) | 0.017 (6) | 0.002 (5) |
O6 | 0.074 (6) | 0.145 (9) | 0.072 (6) | 0.021 (6) | 0.019 (5) | 0.023 (5) |
O7 | 0.101 (8) | 0.132 (9) | 0.062 (5) | −0.032 (6) | −0.010 (5) | −0.003 (5) |
O8 | 0.138 (9) | 0.076 (6) | 0.070 (6) | −0.008 (5) | 0.040 (6) | 0.007 (4) |
O9 | 0.066 (5) | 0.063 (5) | 0.074 (5) | −0.008 (4) | 0.009 (4) | 0.015 (4) |
O10 | 0.083 (6) | 0.060 (5) | 0.071 (5) | 0.005 (4) | 0.012 (4) | −0.019 (4) |
O11 | 0.119 (8) | 0.114 (7) | 0.085 (6) | −0.026 (6) | 0.061 (6) | −0.014 (5) |
O12 | 0.058 (5) | 0.046 (4) | 0.119 (6) | −0.013 (4) | −0.023 (4) | 0.011 (4) |
O13 | 0.057 (5) | 0.045 (4) | 0.096 (5) | −0.009 (3) | −0.018 (4) | 0.011 (4) |
O14 | 0.101 (6) | 0.031 (4) | 0.127 (7) | −0.013 (4) | 0.006 (5) | −0.014 (4) |
N1 | 0.064 (6) | 0.035 (4) | 0.092 (6) | 0.016 (4) | −0.007 (5) | −0.004 (4) |
N2 | 0.061 (6) | 0.031 (4) | 0.067 (5) | 0.003 (4) | −0.006 (4) | −0.008 (4) |
N3 | 0.069 (7) | 0.041 (5) | 0.060 (6) | −0.002 (4) | 0.015 (5) | −0.010 (4) |
N4 | 0.072 (7) | 0.066 (7) | 0.071 (6) | −0.020 (5) | −0.005 (5) | −0.001 (5) |
N5 | 0.070 (6) | 0.029 (4) | 0.068 (5) | 0.000 (4) | 0.023 (5) | −0.003 (4) |
C1 | 0.124 (14) | 0.143 (14) | 0.054 (7) | 0.011 (10) | 0.007 (8) | 0.003 (8) |
C2 | 0.086 (8) | 0.054 (6) | 0.064 (7) | −0.005 (6) | −0.016 (6) | −0.006 (5) |
C3 | 0.046 (6) | 0.044 (5) | 0.058 (6) | 0.002 (4) | −0.005 (4) | 0.009 (4) |
C4 | 0.101 (10) | 0.066 (8) | 0.071 (8) | 0.012 (7) | −0.027 (7) | 0.000 (6) |
C5 | 0.054 (7) | 0.112 (11) | 0.091 (9) | 0.020 (7) | −0.007 (6) | 0.025 (8) |
C6 | 0.057 (7) | 0.053 (6) | 0.101 (9) | 0.012 (5) | 0.012 (6) | 0.007 (6) |
C7 | 0.038 (5) | 0.057 (6) | 0.073 (6) | 0.008 (4) | −0.007 (5) | 0.020 (5) |
C8 | 0.029 (5) | 0.040 (5) | 0.076 (6) | 0.004 (4) | 0.000 (4) | 0.014 (5) |
C9 | 0.073 (8) | 0.043 (6) | 0.075 (7) | 0.025 (5) | 0.012 (6) | −0.001 (5) |
C10 | 0.077 (11) | 0.028 (8) | 0.051 (11) | 0.013 (7) | −0.009 (9) | 0.005 (6) |
C10' | 0.077 (11) | 0.028 (8) | 0.051 (11) | 0.013 (7) | −0.009 (9) | 0.005 (6) |
C11 | 0.090 (11) | 0.083 (9) | 0.152 (14) | 0.015 (8) | 0.003 (10) | −0.003 (9) |
C12 | 0.107 (13) | 0.053 (10) | 0.124 (18) | 0.022 (9) | −0.024 (11) | −0.044 (11) |
C12' | 0.107 (13) | 0.053 (10) | 0.124 (18) | 0.022 (9) | −0.024 (11) | −0.044 (11) |
C13 | 0.108 (10) | 0.037 (5) | 0.063 (6) | −0.012 (6) | 0.010 (7) | −0.020 (5) |
C14 | 0.069 (7) | 0.041 (5) | 0.049 (5) | −0.010 (5) | −0.005 (5) | −0.006 (4) |
C15 | 0.087 (9) | 0.060 (7) | 0.054 (6) | −0.032 (6) | −0.018 (6) | −0.005 (5) |
C16 | 0.051 (6) | 0.051 (6) | 0.065 (6) | −0.004 (5) | −0.020 (5) | −0.002 (5) |
C17 | 0.049 (6) | 0.061 (6) | 0.065 (6) | 0.010 (5) | 0.004 (5) | 0.004 (5) |
C18 | 0.045 (6) | 0.042 (5) | 0.049 (5) | −0.008 (4) | −0.003 (4) | −0.001 (4) |
C19 | 0.041 (5) | 0.049 (5) | 0.048 (5) | −0.009 (4) | 0.002 (4) | −0.005 (4) |
C20 | 0.037 (6) | 0.062 (6) | 0.087 (7) | 0.013 (5) | −0.010 (5) | −0.024 (6) |
C21 | 0.059 (7) | 0.064 (7) | 0.106 (9) | 0.000 (6) | −0.017 (7) | 0.010 (7) |
C22 | 0.159 (16) | 0.104 (11) | 0.080 (10) | −0.022 (10) | 0.010 (10) | 0.006 (9) |
Lu1—O1 | 2.616 (7) | C4—C5 | 1.402 (16) |
Lu1—O2 | 2.368 (6) | C4—H4 | 0.93 |
Lu1—O3 | 2.397 (6) | C5—C6 | 1.342 (17) |
Lu1—O4 | 2.634 (6) | C5—H5 | 0.93 |
Lu1—O6 | 2.482 (8) | C6—C7 | 1.429 (15) |
Lu1—O7 | 2.493 (9) | C6—H6 | 0.93 |
Lu1—O9 | 2.485 (7) | C7—C8 | 1.385 (13) |
Lu1—O10 | 2.447 (7) | C7—C9 | 1.433 (14) |
Lu1—O12 | 2.574 (7) | C9—H9 | 0.93 |
Lu1—O13 | 2.514 (6) | C10—C11 | 1.490 (10) |
Cu1—O2 | 1.874 (6) | C10—C12 | 1.500 (10) |
Cu1—O3 | 1.909 (6) | C10—H10 | 0.98 |
Cu1—O5 | 2.335 (8) | C10'—C11 | 1.487 (9) |
Cu1—N1 | 1.922 (8) | C10'—C12' | 1.502 (10) |
Cu1—N2 | 1.900 (8) | C10'—H10' | 0.98 |
O1—C3 | 1.400 (11) | C11—H11A | 0.96 |
O1—C2 | 1.458 (11) | C11—H11B | 0.96 |
O2—C8 | 1.342 (11) | C11—H11C | 0.96 |
O3—C19 | 1.301 (10) | C11—H11D | 0.96 |
O4—C18 | 1.387 (10) | C11—H11E | 0.96 |
O4—C20 | 1.481 (10) | C11—H11F | 0.96 |
O5—C22 | 1.299 (14) | C12—H12A | 0.97 |
O5—H5O | 0.82 | C12—H12B | 0.97 |
O6—N3 | 1.225 (12) | C12'—H12C | 0.97 |
O7—N3 | 1.227 (13) | C12'—H12D | 0.97 |
O8—N3 | 1.193 (11) | C13—C14 | 1.488 (14) |
O9—N4 | 1.278 (11) | C13—H13 | 0.93 |
O10—N4 | 1.296 (11) | C14—C15 | 1.355 (15) |
O11—N4 | 1.196 (12) | C14—C19 | 1.429 (12) |
O12—N5 | 1.224 (10) | C15—C16 | 1.383 (15) |
O13—N5 | 1.242 (10) | C15—H15 | 0.93 |
O14—N5 | 1.235 (10) | C16—C17 | 1.367 (14) |
N1—C9 | 1.305 (13) | C16—H16 | 0.93 |
N1—C10' | 1.458 (9) | C17—C18 | 1.405 (13) |
N1—C10 | 1.466 (9) | C17—H17 | 0.93 |
N2—C13 | 1.250 (13) | C18—C19 | 1.387 (12) |
N2—C12' | 1.459 (10) | C20—C21 | 1.524 (14) |
N2—C12 | 1.458 (10) | C20—H20A | 0.97 |
C1—C2 | 1.567 (15) | C20—H20B | 0.97 |
C1—H1A | 0.96 | C21—H21A | 0.96 |
C1—H1B | 0.96 | C21—H21B | 0.96 |
C1—H1C | 0.96 | C21—H21C | 0.96 |
C2—H2A | 0.97 | C22—H22A | 0.96 |
C2—H2B | 0.97 | C22—H22B | 0.96 |
C3—C8 | 1.376 (13) | C22—H22C | 0.96 |
C3—C4 | 1.392 (14) | ||
O2—Lu1—O3 | 63.0 (2) | O1—C2—H2A | 109.7 |
O2—Lu1—O10 | 127.6 (2) | C1—C2—H2A | 109.7 |
O3—Lu1—O10 | 120.6 (3) | O1—C2—H2B | 109.7 |
O2—Lu1—O9 | 81.9 (2) | C1—C2—H2B | 109.7 |
O3—Lu1—O9 | 80.3 (2) | H2A—C2—H2B | 108.2 |
O10—Lu1—O9 | 51.7 (3) | C8—C3—C4 | 122.3 (9) |
O2—Lu1—O6 | 76.1 (3) | C8—C3—O1 | 114.3 (8) |
O3—Lu1—O6 | 102.3 (3) | C4—C3—O1 | 123.4 (9) |
O10—Lu1—O6 | 136.6 (3) | C3—C4—C5 | 117.2 (11) |
O9—Lu1—O6 | 153.3 (3) | C3—C4—H4 | 121.4 |
O2—Lu1—O7 | 93.2 (3) | C5—C4—H4 | 121.4 |
O3—Lu1—O7 | 70.5 (3) | C6—C5—C4 | 120.7 (11) |
O10—Lu1—O7 | 139.0 (3) | C6—C5—H5 | 119.7 |
O9—Lu1—O7 | 149.2 (3) | C4—C5—H5 | 119.7 |
O6—Lu1—O7 | 48.4 (3) | C5—C6—C7 | 122.4 (10) |
O2—Lu1—O13 | 157.8 (2) | C5—C6—H6 | 118.8 |
O3—Lu1—O13 | 123.9 (2) | C7—C6—H6 | 118.8 |
O10—Lu1—O13 | 69.8 (3) | C8—C7—C9 | 127.9 (9) |
O9—Lu1—O13 | 119.3 (3) | C8—C7—C6 | 116.6 (10) |
O6—Lu1—O13 | 81.7 (3) | C9—C7—C6 | 115.4 (9) |
O7—Lu1—O13 | 72.2 (3) | O2—C8—C3 | 116.5 (8) |
O2—Lu1—O12 | 119.5 (2) | O2—C8—C7 | 122.9 (9) |
O3—Lu1—O12 | 167.1 (2) | C3—C8—C7 | 120.6 (9) |
O10—Lu1—O12 | 69.0 (3) | N1—C9—C7 | 121.9 (8) |
O9—Lu1—O12 | 112.3 (3) | N1—C9—H9 | 119.0 |
O6—Lu1—O12 | 67.6 (3) | C7—C9—H9 | 119.0 |
O7—Lu1—O12 | 96.7 (3) | N1—C10—C11 | 120.1 (12) |
O13—Lu1—O12 | 48.7 (2) | N1—C10—C12 | 105.3 (17) |
O2—Lu1—O1 | 61.3 (2) | C11—C10—C12 | 104.3 (11) |
O3—Lu1—O1 | 121.59 (19) | N1—C10—H10 | 108.9 |
O10—Lu1—O1 | 82.4 (2) | C11—C10—H10 | 108.9 |
O9—Lu1—O1 | 75.8 (2) | C12—C10—H10 | 108.9 |
O6—Lu1—O1 | 80.5 (3) | N1—C10'—C11 | 120.9 (11) |
O7—Lu1—O1 | 128.1 (3) | N1—C10'—C12' | 107.1 (18) |
O13—Lu1—O1 | 114.3 (2) | C11—C10'—C12' | 105.2 (12) |
O12—Lu1—O1 | 66.0 (2) | N1—C10'—H10' | 107.6 |
O2—Lu1—O4 | 122.4 (2) | C11—C10'—H10' | 107.6 |
O3—Lu1—O4 | 60.70 (18) | C12'—C10'—H10' | 107.6 |
O10—Lu1—O4 | 75.1 (2) | C10—C11—H11A | 109.5 |
O9—Lu1—O4 | 77.8 (2) | C10—C11—H11B | 109.5 |
O6—Lu1—O4 | 126.9 (3) | H11A—C11—H11B | 109.5 |
O7—Lu1—O4 | 79.4 (3) | C10—C11—H11C | 109.5 |
O13—Lu1—O4 | 72.4 (2) | H11A—C11—H11C | 109.5 |
O12—Lu1—O4 | 118.2 (2) | H11B—C11—H11C | 109.5 |
O1—Lu1—O4 | 152.5 (2) | C10'—C11—H11D | 109.3 |
O2—Cu1—O3 | 82.3 (3) | C10'—C11—H11E | 110.2 |
O2—Cu1—N2 | 172.7 (3) | H11D—C11—H11E | 109.5 |
O3—Cu1—N2 | 95.1 (3) | C10'—C11—H11F | 108.9 |
O2—Cu1—N1 | 96.5 (3) | H11D—C11—H11F | 109.5 |
O3—Cu1—N1 | 171.4 (3) | H11E—C11—H11F | 109.5 |
N2—Cu1—N1 | 85.0 (3) | N2—C12—C10 | 108.2 (14) |
O2—Cu1—O5 | 96.4 (3) | N2—C12—H12A | 110.1 |
O3—Cu1—O5 | 95.7 (3) | C10—C12—H12A | 110.1 |
N2—Cu1—O5 | 90.6 (3) | N2—C12—H12B | 110.1 |
N1—Cu1—O5 | 92.9 (4) | C10—C12—H12B | 110.1 |
C3—O1—C2 | 119.6 (8) | H12A—C12—H12B | 108.4 |
C3—O1—Lu1 | 116.5 (5) | N2—C12'—C10' | 107.1 (15) |
C2—O1—Lu1 | 123.7 (6) | N2—C12'—H12C | 110.3 |
C8—O2—Cu1 | 124.5 (5) | C10'—C12'—H12C | 110.3 |
C8—O2—Lu1 | 127.1 (5) | N2—C12'—H12D | 110.3 |
Cu1—O2—Lu1 | 108.0 (3) | C10'—C12'—H12D | 110.3 |
C19—O3—Cu1 | 125.1 (6) | H12C—C12'—H12D | 108.5 |
C19—O3—Lu1 | 129.2 (5) | N2—C13—C14 | 125.8 (9) |
Cu1—O3—Lu1 | 105.7 (3) | N2—C13—H13 | 117.1 |
C18—O4—C20 | 117.2 (7) | C14—C13—H13 | 117.1 |
C18—O4—Lu1 | 118.2 (5) | C15—C14—C19 | 120.5 (9) |
C20—O4—Lu1 | 124.6 (5) | C15—C14—C13 | 118.6 (9) |
C22—O5—Cu1 | 128.7 (9) | C19—C14—C13 | 120.9 (9) |
C22—O5—H5O | 115.7 | C16—C15—C14 | 121.0 (9) |
Cu1—O5—H5O | 115.7 | C16—C15—H15 | 119.5 |
N3—O6—Lu1 | 99.5 (7) | C14—C15—H15 | 119.5 |
N3—O7—Lu1 | 98.9 (7) | C17—C16—C15 | 119.9 (9) |
N4—O9—Lu1 | 96.7 (6) | C17—C16—H16 | 120.0 |
N4—O10—Lu1 | 97.9 (6) | C15—C16—H16 | 120.0 |
N5—O12—Lu1 | 95.8 (5) | C16—C17—C18 | 120.2 (9) |
N5—O13—Lu1 | 98.4 (5) | C16—C17—H17 | 119.9 |
C9—N1—C10' | 120.7 (11) | C18—C17—H17 | 119.9 |
C9—N1—C10 | 122.2 (10) | C19—C18—O4 | 114.3 (8) |
C9—N1—Cu1 | 125.2 (6) | C19—C18—C17 | 120.4 (8) |
C10'—N1—Cu1 | 111.0 (8) | O4—C18—C17 | 125.2 (8) |
C10—N1—Cu1 | 111.0 (8) | O3—C19—C18 | 117.0 (8) |
C13—N2—C12' | 119.9 (13) | O3—C19—C14 | 125.3 (8) |
C13—N2—C12 | 122.0 (13) | C18—C19—C14 | 117.7 (8) |
C13—N2—Cu1 | 125.9 (6) | O4—C20—C21 | 112.5 (9) |
C12'—N2—Cu1 | 112.7 (12) | O4—C20—H20A | 109.1 |
C12—N2—Cu1 | 111.9 (12) | C21—C20—H20A | 109.1 |
O8—N3—O7 | 123.8 (11) | O4—C20—H20B | 109.1 |
O8—N3—O6 | 123.5 (11) | C21—C20—H20B | 109.1 |
O7—N3—O6 | 112.7 (9) | H20A—C20—H20B | 107.8 |
O11—N4—O9 | 126.5 (10) | C20—C21—H21A | 109.5 |
O11—N4—O10 | 120.1 (10) | C20—C21—H21B | 109.5 |
O9—N4—O10 | 113.4 (9) | H21A—C21—H21B | 109.5 |
O13—N5—O12 | 116.7 (8) | C20—C21—H21C | 109.5 |
O13—N5—O14 | 122.1 (9) | H21A—C21—H21C | 109.5 |
O12—N5—O14 | 121.1 (9) | H21B—C21—H21C | 109.5 |
C2—C1—H1A | 109.5 | O5—C22—H22A | 109.5 |
C2—C1—H1B | 109.5 | O5—C22—H22B | 109.5 |
H1A—C1—H1B | 109.5 | H22A—C22—H22B | 109.5 |
C2—C1—H1C | 109.5 | O5—C22—H22C | 109.5 |
H1A—C1—H1C | 109.5 | H22A—C22—H22C | 109.5 |
H1B—C1—H1C | 109.5 | H22B—C22—H22C | 109.5 |
O1—C2—C1 | 109.7 (9) | ||
O2—Lu1—O1—C3 | −17.2 (6) | O6—Lu1—O12—N5 | −102.2 (6) |
O3—Lu1—O1—C3 | −36.6 (7) | O7—Lu1—O12—N5 | −62.6 (6) |
O10—Lu1—O1—C3 | −158.0 (6) | O13—Lu1—O12—N5 | −3.4 (5) |
O9—Lu1—O1—C3 | −105.6 (6) | O1—Lu1—O12—N5 | 168.5 (7) |
O6—Lu1—O1—C3 | 62.1 (6) | O4—Lu1—O12—N5 | 18.9 (7) |
O7—Lu1—O1—C3 | 52.4 (7) | O2—Lu1—O13—N5 | 68.7 (9) |
O13—Lu1—O1—C3 | 138.3 (6) | O3—Lu1—O13—N5 | 170.1 (5) |
O12—Lu1—O1—C3 | 131.7 (6) | O10—Lu1—O13—N5 | −76.0 (6) |
O4—Lu1—O1—C3 | −122.9 (6) | O9—Lu1—O13—N5 | −91.6 (6) |
O2—Lu1—O1—C2 | 158.6 (7) | O6—Lu1—O13—N5 | 70.8 (6) |
O3—Lu1—O1—C2 | 139.3 (6) | O7—Lu1—O13—N5 | 119.7 (6) |
O10—Lu1—O1—C2 | 17.9 (7) | O12—Lu1—O13—N5 | 3.4 (5) |
O9—Lu1—O1—C2 | 70.3 (7) | O1—Lu1—O13—N5 | −4.7 (6) |
O6—Lu1—O1—C2 | −122.1 (7) | O4—Lu1—O13—N5 | −156.1 (6) |
O7—Lu1—O1—C2 | −131.7 (7) | O2—Cu1—N1—C9 | −3.2 (9) |
O13—Lu1—O1—C2 | −45.8 (7) | N2—Cu1—N1—C9 | −176.1 (9) |
O12—Lu1—O1—C2 | −52.5 (7) | O5—Cu1—N1—C9 | 93.6 (9) |
O4—Lu1—O1—C2 | 52.9 (8) | O2—Cu1—N1—C10' | 156.9 (11) |
O3—Cu1—O2—C8 | −178.4 (7) | N2—Cu1—N1—C10' | −15.9 (11) |
N1—Cu1—O2—C8 | 10.2 (7) | O5—Cu1—N1—C10' | −106.3 (11) |
O5—Cu1—O2—C8 | −83.5 (7) | O2—Cu1—N1—C10 | −169.1 (10) |
O3—Cu1—O2—Lu1 | 8.3 (3) | N2—Cu1—N1—C10 | 18.0 (10) |
N1—Cu1—O2—Lu1 | −163.1 (3) | O5—Cu1—N1—C10 | −72.3 (10) |
O5—Cu1—O2—Lu1 | 103.2 (3) | O3—Cu1—N2—C13 | 12.6 (9) |
O3—Lu1—O2—C8 | 179.5 (8) | N1—Cu1—N2—C13 | −176.0 (9) |
O10—Lu1—O2—C8 | 70.3 (8) | O5—Cu1—N2—C13 | −83.1 (9) |
O9—Lu1—O2—C8 | 96.3 (7) | O3—Cu1—N2—C12' | 178.6 (18) |
O6—Lu1—O2—C8 | −68.6 (7) | N1—Cu1—N2—C12' | −10.0 (18) |
O7—Lu1—O2—C8 | −114.3 (7) | O5—Cu1—N2—C12' | 82.9 (18) |
O13—Lu1—O2—C8 | −66.5 (10) | O3—Cu1—N2—C12 | −162.6 (17) |
O12—Lu1—O2—C8 | −14.8 (8) | N1—Cu1—N2—C12 | 8.8 (17) |
O1—Lu1—O2—C8 | 18.0 (7) | O5—Cu1—N2—C12 | 101.7 (17) |
O4—Lu1—O2—C8 | 166.2 (7) | Lu1—O7—N3—O8 | −175.4 (8) |
O3—Lu1—O2—Cu1 | −7.3 (3) | Lu1—O7—N3—O6 | 6.0 (10) |
O10—Lu1—O2—Cu1 | −116.5 (3) | Lu1—O6—N3—O8 | 175.4 (8) |
O9—Lu1—O2—Cu1 | −90.6 (3) | Lu1—O6—N3—O7 | −6.0 (10) |
O6—Lu1—O2—Cu1 | 104.5 (4) | Lu1—O9—N4—O11 | −175.5 (11) |
O7—Lu1—O2—Cu1 | 58.8 (4) | Lu1—O9—N4—O10 | 4.7 (9) |
O13—Lu1—O2—Cu1 | 106.6 (6) | Lu1—O10—N4—O11 | 175.4 (10) |
O12—Lu1—O2—Cu1 | 158.3 (3) | Lu1—O10—N4—O9 | −4.8 (9) |
O1—Lu1—O2—Cu1 | −168.9 (4) | Lu1—O13—N5—O12 | −6.0 (9) |
O4—Lu1—O2—Cu1 | −20.7 (4) | Lu1—O13—N5—O14 | 176.9 (7) |
O2—Cu1—O3—C19 | 173.7 (8) | Lu1—O12—N5—O13 | 5.8 (9) |
N2—Cu1—O3—C19 | −13.2 (8) | Lu1—O12—N5—O14 | −177.0 (7) |
O5—Cu1—O3—C19 | 77.9 (7) | C3—O1—C2—C1 | 68.5 (12) |
O2—Cu1—O3—Lu1 | −8.1 (3) | Lu1—O1—C2—C1 | −107.2 (9) |
N2—Cu1—O3—Lu1 | 165.1 (3) | C2—O1—C3—C8 | −159.1 (8) |
O5—Cu1—O3—Lu1 | −103.9 (3) | Lu1—O1—C3—C8 | 16.9 (10) |
O2—Lu1—O3—C19 | −174.7 (8) | C2—O1—C3—C4 | 20.3 (14) |
O10—Lu1—O3—C19 | −55.2 (8) | Lu1—O1—C3—C4 | −163.7 (8) |
O9—Lu1—O3—C19 | −89.0 (8) | C8—C3—C4—C5 | −3.0 (16) |
O6—Lu1—O3—C19 | 118.0 (7) | O1—C3—C4—C5 | 177.7 (10) |
O7—Lu1—O3—C19 | 80.9 (8) | C3—C4—C5—C6 | 4.4 (18) |
O13—Lu1—O3—C19 | 29.9 (8) | C4—C5—C6—C7 | −3.3 (19) |
O12—Lu1—O3—C19 | 80.8 (13) | C5—C6—C7—C8 | 0.5 (17) |
O1—Lu1—O3—C19 | −155.7 (7) | C5—C6—C7—C9 | −178.3 (11) |
O4—Lu1—O3—C19 | −7.7 (7) | Cu1—O2—C8—C3 | 171.5 (6) |
O2—Lu1—O3—Cu1 | 7.1 (3) | Lu1—O2—C8—C3 | −16.4 (11) |
O10—Lu1—O3—Cu1 | 126.7 (3) | Cu1—O2—C8—C7 | −10.8 (12) |
O9—Lu1—O3—Cu1 | 92.8 (3) | Lu1—O2—C8—C7 | 161.2 (7) |
O6—Lu1—O3—Cu1 | −60.1 (3) | C4—C3—C8—O2 | 178.0 (9) |
O7—Lu1—O3—Cu1 | −97.2 (4) | O1—C3—C8—O2 | −2.6 (12) |
O13—Lu1—O3—Cu1 | −148.3 (3) | C4—C3—C8—C7 | 0.4 (15) |
O12—Lu1—O3—Cu1 | −97.3 (10) | O1—C3—C8—C7 | 179.7 (8) |
O1—Lu1—O3—Cu1 | 26.1 (4) | C9—C7—C8—O2 | 2.1 (16) |
O4—Lu1—O3—Cu1 | 174.2 (4) | C6—C7—C8—O2 | −176.6 (9) |
O2—Lu1—O4—C18 | 18.9 (7) | C9—C7—C8—C3 | 179.6 (10) |
O3—Lu1—O4—C18 | 5.3 (6) | C6—C7—C8—C3 | 1.0 (14) |
O10—Lu1—O4—C18 | 144.2 (6) | C10'—N1—C9—C7 | −161.7 (12) |
O9—Lu1—O4—C18 | 90.9 (6) | C10—N1—C9—C7 | 161.1 (12) |
O6—Lu1—O4—C18 | −78.0 (7) | Cu1—N1—C9—C7 | −3.3 (15) |
O7—Lu1—O4—C18 | −68.2 (6) | C8—C7—C9—N1 | 5.5 (17) |
O13—Lu1—O4—C18 | −142.7 (6) | C6—C7—C9—N1 | −175.8 (10) |
O12—Lu1—O4—C18 | −160.1 (6) | C9—N1—C10—C11 | 37 (2) |
O1—Lu1—O4—C18 | 108.1 (6) | C10'—N1—C10—C11 | −60.1 (15) |
O2—Lu1—O4—C20 | −161.9 (7) | Cu1—N1—C10—C11 | −156.2 (13) |
O3—Lu1—O4—C20 | −175.6 (7) | C9—N1—C10—C12 | 154.4 (17) |
O10—Lu1—O4—C20 | −36.6 (7) | C10'—N1—C10—C12 | 57 (3) |
O9—Lu1—O4—C20 | −89.9 (7) | Cu1—N1—C10—C12 | −39.2 (18) |
O6—Lu1—O4—C20 | 101.1 (7) | C9—N1—C10'—C11 | −41 (2) |
O7—Lu1—O4—C20 | 111.0 (7) | C10—N1—C10'—C11 | 61.2 (14) |
O13—Lu1—O4—C20 | 36.5 (7) | Cu1—N1—C10'—C11 | 157.5 (16) |
O12—Lu1—O4—C20 | 19.1 (8) | C9—N1—C10'—C12' | −161.7 (16) |
O1—Lu1—O4—C20 | −72.7 (8) | C10—N1—C10'—C12' | −59 (3) |
O2—Cu1—O5—C22 | 9.4 (14) | Cu1—N1—C10'—C12' | 37.2 (18) |
O3—Cu1—O5—C22 | 92.3 (13) | N1—C10'—C11—C10 | −61.2 (14) |
N2—Cu1—O5—C22 | −172.5 (13) | C12'—C10'—C11—C10 | 60 (3) |
N1—Cu1—O5—C22 | −87.5 (13) | N1—C10—C11—C10' | 59.8 (14) |
O2—Lu1—O6—N3 | −103.6 (7) | C12—C10—C11—C10' | −58 (3) |
O3—Lu1—O6—N3 | −45.8 (7) | C13—N2—C12—C10 | 151.7 (17) |
O10—Lu1—O6—N3 | 125.7 (7) | C12'—N2—C12—C10 | 63 (6) |
O9—Lu1—O6—N3 | −138.7 (6) | Cu1—N2—C12—C10 | −33 (3) |
O7—Lu1—O6—N3 | 3.7 (6) | N1—C10—C12—N2 | 46 (3) |
O13—Lu1—O6—N3 | 77.2 (7) | C11—C10—C12—N2 | 173 (2) |
O12—Lu1—O6—N3 | 125.9 (7) | C13—N2—C12'—C10' | −160.6 (17) |
O1—Lu1—O6—N3 | −166.2 (7) | C12—N2—C12'—C10' | −59 (5) |
O4—Lu1—O6—N3 | 16.7 (8) | Cu1—N2—C12'—C10' | 32 (3) |
O2—Lu1—O7—N3 | 64.6 (6) | N1—C10'—C12'—N2 | −44 (3) |
O3—Lu1—O7—N3 | 124.4 (7) | C11—C10'—C12'—N2 | −174 (2) |
O10—Lu1—O7—N3 | −121.1 (7) | C12'—N2—C13—C14 | −170 (2) |
O9—Lu1—O7—N3 | 144.0 (6) | C12—N2—C13—C14 | 170 (2) |
O6—Lu1—O7—N3 | −3.6 (6) | Cu1—N2—C13—C14 | −5.1 (16) |
O13—Lu1—O7—N3 | −98.3 (7) | N2—C13—C14—C15 | 175.5 (10) |
O12—Lu1—O7—N3 | −55.6 (7) | N2—C13—C14—C19 | −6.5 (16) |
O1—Lu1—O7—N3 | 9.1 (8) | C19—C14—C15—C16 | 2.1 (16) |
O4—Lu1—O7—N3 | −173.1 (7) | C13—C14—C15—C16 | −179.9 (9) |
O2—Lu1—O9—N4 | −156.7 (6) | C14—C15—C16—C17 | −4.3 (16) |
O3—Lu1—O9—N4 | 139.4 (6) | C15—C16—C17—C18 | 1.1 (15) |
O10—Lu1—O9—N4 | −2.9 (6) | C20—O4—C18—C19 | 177.2 (8) |
O6—Lu1—O9—N4 | −122.4 (8) | Lu1—O4—C18—C19 | −3.6 (10) |
O7—Lu1—O9—N4 | 120.7 (8) | C20—O4—C18—C17 | 1.7 (13) |
O13—Lu1—O9—N4 | 15.9 (7) | Lu1—O4—C18—C17 | −179.1 (7) |
O12—Lu1—O9—N4 | −38.1 (6) | C16—C17—C18—C19 | 4.3 (15) |
O1—Lu1—O9—N4 | −94.3 (6) | C16—C17—C18—O4 | 179.6 (9) |
O4—Lu1—O9—N4 | 77.5 (6) | Cu1—O3—C19—C18 | −173.2 (6) |
O2—Lu1—O10—N4 | 36.4 (7) | Lu1—O3—C19—C18 | 9.0 (12) |
O3—Lu1—O10—N4 | −41.5 (7) | Cu1—O3—C19—C14 | 6.3 (13) |
O9—Lu1—O10—N4 | 2.9 (6) | Lu1—O3—C19—C14 | −171.5 (6) |
O6—Lu1—O10—N4 | 148.2 (6) | O4—C18—C19—O3 | −2.5 (12) |
O7—Lu1—O10—N4 | −136.5 (6) | C17—C18—C19—O3 | 173.2 (8) |
O13—Lu1—O10—N4 | −159.7 (7) | O4—C18—C19—C14 | 178.0 (8) |
O12—Lu1—O10—N4 | 148.0 (7) | C17—C18—C19—C14 | −6.3 (13) |
O1—Lu1—O10—N4 | 80.8 (6) | C15—C14—C19—O3 | −176.4 (9) |
O4—Lu1—O10—N4 | −83.2 (6) | C13—C14—C19—O3 | 5.7 (15) |
O2—Lu1—O12—N5 | −160.1 (5) | C15—C14—C19—C18 | 3.2 (14) |
O3—Lu1—O12—N5 | −62.5 (13) | C13—C14—C19—C18 | −174.8 (9) |
O10—Lu1—O12—N5 | 77.7 (6) | C18—O4—C20—C21 | 77.7 (10) |
O9—Lu1—O12—N5 | 106.7 (6) | Lu1—O4—C20—C21 | −101.5 (8) |
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5O···O14i | 0.82 | 2.13 | 2.93 (1) | 164 |
Symmetry code: (i) −x+1, y+1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [CuLu(C21H22N2O4)(CH4O)(NO3)3] |
Mr | 825.00 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 295 |
a, b, c (Å) | 9.1795 (5), 20.407 (1), 15.7058 (9) |
β (°) | 93.126 (1) |
V (Å3) | 2937.7 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 4.14 |
Crystal size (mm) | 0.20 × 0.09 × 0.08 |
Data collection | |
Diffractometer | Bruker APEXII area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.183, 0.733 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 21167, 6636, 3788 |
Rint | 0.049 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.059, 0.196, 1.07 |
No. of reflections | 6636 |
No. of parameters | 394 |
No. of restraints | 10 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.20, −1.29 |
Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).
Lu1—O1 | 2.616 (7) | Lu1—O12 | 2.574 (7) |
Lu1—O2 | 2.368 (6) | Lu1—O13 | 2.514 (6) |
Lu1—O3 | 2.397 (6) | Cu1—O2 | 1.874 (6) |
Lu1—O4 | 2.634 (6) | Cu1—O3 | 1.909 (6) |
Lu1—O6 | 2.482 (8) | Cu1—O5 | 2.335 (8) |
Lu1—O7 | 2.493 (9) | Cu1—N1 | 1.922 (8) |
Lu1—O9 | 2.485 (7) | Cu1—N2 | 1.900 (8) |
Lu1—O10 | 2.447 (7) |
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5O···O14i | 0.82 | 2.13 | 2.93 (1) | 164 |
Symmetry code: (i) −x+1, y+1/2, −z+1/2. |
3-Alkoxysalicylaldehyde condenses with ethylenediamine and related diamines to form a class of Schiff bases that react with divalent transition-metal salts to afford another class of compounds that react with lanthanum(III) salts to yield bimetallic compounds. Bis(2-oxy-3-methoxybenzylidene)ethylenediamine)(acetone)tris(nitrato)-copper- neodymium (Elmali et al., 2004), bis(2-oxy-3-methoxybenzylidene)ethylenediamine)(acetone)tris(nitrato)-copper- dysprosium (Elmali et al., 2005) and (1,2-cyclohexane)bis(3-ethoxysalicylideneaminato)aquatris(nitrato)χoppergadolinium (Koner et al., 2005) represent the copper compounds that are coordinated to lanthanum trinitrate. Their copper atoms are chelated by the deprotonated Schiff bases but the geometry is a square-pyramid owing to the coordinated solvent molecules. On the other hand, the lanthanum atom is chelated by three nitrate groups, so a ten-coordinate geometry results from the involvement of the four oxygen atoms of the copper-Schiff base portion of the bimetallic molecule. The title compound (Fig. 1) has a similar bonding mode; the lutetium atom shows bicapped square-antiprismatic coordination.