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The Cu atom in the title compound (systematic name: {6,6′-diethoxy-2,2′-[propane-1,2-diylbis(nitrilomethylidyne)]diphenolato-1κ
4O1,
O1′,
O6,
O6′:2κ
4O1,
N,
N′,
O1′}(methanol-2κ
O)trinitrato-1κ
6O,
O′-copper(II)lutetium(III)), [CuLu(C
21H
22N
2O
4)(CH
4O)(NO
3)
3] is
N,
N′,
O,
O′ chelated by the deprotonated Schiff base, the four chelating atoms forming a square plane above which lies the methanol molecule. The [Cu(C
21H
24N
2O
4)(CH
4O)] unit uses the two ethoxy and two hydroxy O atoms to chelate the [Lu(NO
3)
3] unit. The Cu
II atom exists in a square-pyramidal geometry and the Lu
III atom in a bicapped square-antiprismatic geometry. Molecules are linked into a chain along the
b axis by O—H
O hydrogen bonds. Two CH
2 groups of the C
2N
2Cu ring and the H atoms of the attached methyl group are disordered equally over two positions.
Supporting information
CCDC reference: 657564
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.015 Å
- Disorder in main residue
- R factor = 0.059
- wR factor = 0.196
- Data-to-parameter ratio = 16.8
checkCIF/PLATON results
No syntax errors found
Alert level A
ABSTM02_ALERT_3_A The ratio of expected to reported Tmax/Tmin(RR') is < 0.50
Tmin and Tmax reported: 0.183 0.733
Tmin(prime) and Tmax expected: 0.432 0.718
RR(prime) = 0.415
Please check that your absorption correction is appropriate.
| Author Response: The diffraction data are of marginal quality, and there is a problem
of absorption. The raw intensities were processed by using the multi-scan
absorption program, and a model with heavy atoms was used. The transmission
factors are those given by the program.
|
PLAT061_ALERT_3_A Tmax/Tmin Range Test RR' too Large ............. 0.41
| Author Response: As above.
|
PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for C11
| Author Response: The atom is part of a disordered group.
|
Alert level B
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O6
| Author Response: The atom is part of a disordered group.
|
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O7
| Author Response: The atom is part of a disordered group.
|
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C12
| Author Response: The atom is part of a disordered group.
|
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C12'
| Author Response: The atom is part of a disordered group.
|
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for N3
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C10
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C10'
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O5
| Author Response: The atom is part of a disordered group.
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O12
| Author Response: The atom is part of a disordered group.
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C13
| Author Response: The atom is part of a disordered group.
|
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cu1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N2
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N5
PLAT301_ALERT_3_C Main Residue Disorder ......................... 4.00 Perc.
PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 15
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C22 H28 Cu1 Lu1 N5 O14
Atom count from _chemical_formula_moiety:
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 10
3 ALERT level A = In general: serious problem
7 ALERT level B = Potentially serious problem
10 ALERT level C = Check and explain
2 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
14 ALERT type 2 Indicator that the structure model may be wrong or deficient
5 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
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.
Structure description
top
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).
[µ
2-
N,
N'-Bis(2-oxy-3-ethoxybenzylidene)ethylene-1,2-diamine]
(methanol)tris(nitrato)copper(II)lutetium(III)
top
Crystal data top
[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 | |
Data collection top
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 top
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 |
Crystal data top
[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)° | |
Data collection top
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 | |
Refinement top
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 | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | 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* | |
Atomic displacement parameters (Å2) top | 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) |
Geometric parameters (Å, º) top
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) |
Hydrogen-bond geometry (Å, º) top
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 |
Selected bond lengths (Å) topLu1—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) | | |
Hydrogen-bond geometry (Å, º) top
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. |
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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.