Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807035349/hk2296sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807035349/hk2296Isup2.hkl |
CCDC reference: 1270869
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean (C-C) = 0.011 Å
- R factor = 0.042
- wR factor = 0.128
- Data-to-parameter ratio = 16.8
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.49 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.03 Ratio PLAT220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 2.74 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N3 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N5 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C6 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C15 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O7 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C22 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C29 PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 11 PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 72.00 A 3
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Nd1 (3) 3.00 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 3
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 15 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 11 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 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For related structures, see: Liu et al. (2007a,b). For bond-length data, see: Allen et al. (1987).
Crystals of the title compound were synthesized using hydrothermal method in a 23 ml Teflon-lined Parr bomb. Neodymium (III) chloride hexahydrate (143.4 mg, 0.4 mmol), phen (79.2 mg, 0.4 mmol), phenoxyacetic acid (182.6 mg, 1.2 mmol) and distilled water (6 g) were placed into the bomb and sealed. The bomb was then heated under autogenous pressure for 7 d at 433 K and allowed to cool at room temperature for 24 h. Upon opening the bomb, a clear colorless solution was decanted from small colorless crystals. These crystals were washed with distilled water followed by ethanol, and allowed to air-dry at room temperature.
H atoms were positioned geometrically, with C—H = 0.93 and 0.97 Å, for aromatic and methylene H atoms, and constrained to ride on their parent atoms, with Uiso(H) = 1.2Ueq(C).
The crystal structures of tetrakis(µ-(2-pyridyloxy)acetato)bis[(1,10-phenanthroline)((2-pyridyloxy)acetato) lanthanum(III)], (II), (Liu et al., 2007a) and tetrakis(µ-(2-pyridyloxy)acetato) bis[(1,10-phenanthroline)((2-pyridyloxy)acetato)praseodymium(III)], (III), (Liu et al., 2007b) have previously been reported. The crystal structure determination of the title compound, (I), has been carried out in order to elucidate the molecular conformation and to compare it with those of (II) and (III).
In the molecule of (I) (Fig. 1), the ligand bond lengths and angles are within normal ranges (Allen et al., 1987). It has an inversion centre between the two NdIII ions, in which they are bridged by the two terdentate and the two bidentate carboxylate groups. Each Nd atom is seven-coordinated by the two N atoms of 1,10-phenanthroline (phen) ligand and the five O atoms of 2-pyridyloxy- acetic acid ligands. The Nd—O and Nd—N bonds are in the range of [2.387 (3)–2.784 (4) Å] and [2.701 (4)–2.742 (4) Å], respectively (Table 1), as in (II) and (III).
In the crystal structure, intermolecular C—H···O hydrogen bonds (Table 2) lead to a supramolecular network structure (Fig. 2), in which they may be effective in the stabilization of the structure, as in (II) and (III).
The compounds, (I), (II) and (III), are isostructural.
For related structures, see: Liu et al. (2007a,b). For bond-length data, see: Allen et al. (1987).
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1996); software used to prepare material for publication: SHELXTL.
[Nd2(C7H6NO3)6(C12H8N2)2] | F(000) = 1564 |
Mr = 1561.66 | Dx = 1.553 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 8971 reflections |
a = 20.1233 (11) Å | θ = 2.6–26.0° |
b = 8.3987 (12) Å | µ = 1.62 mm−1 |
c = 20.6864 (13) Å | T = 273 K |
β = 107.207 (6)° | Plate, colourless |
V = 3339.7 (6) Å3 | 0.33 × 0.13 × 0.08 mm |
Z = 2 |
Bruker SMART CCD area-detector diffractometer | 6771 independent reflections |
Radiation source: fine-focus sealed tube | 4723 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
φ and ω scans | θmax = 26.4°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −25→24 |
Tmin = 0.620, Tmax = 0.880 | k = −10→10 |
25069 measured reflections | l = −25→25 |
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)] = 0.042 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.128 | H-atom parameters constrained |
S = 0.99 | w = 1/[σ2(Fo2) + (0.0839P)2] where P = (Fo2 + 2Fc2)/3 |
6771 reflections | (Δ/σ)max = 0.002 |
403 parameters | Δρmax = 1.67 e Å−3 |
3 restraints | Δρmin = −0.67 e Å−3 |
[Nd2(C7H6NO3)6(C12H8N2)2] | V = 3339.7 (6) Å3 |
Mr = 1561.66 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 20.1233 (11) Å | µ = 1.62 mm−1 |
b = 8.3987 (12) Å | T = 273 K |
c = 20.6864 (13) Å | 0.33 × 0.13 × 0.08 mm |
β = 107.207 (6)° |
Bruker SMART CCD area-detector diffractometer | 6771 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 4723 reflections with I > 2σ(I) |
Tmin = 0.620, Tmax = 0.880 | Rint = 0.041 |
25069 measured reflections |
R[F2 > 2σ(F2)] = 0.042 | 3 restraints |
wR(F2) = 0.128 | H-atom parameters constrained |
S = 0.99 | Δρmax = 1.67 e Å−3 |
6771 reflections | Δρmin = −0.67 e Å−3 |
403 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 | ||
Nd1 | 0.931198 (12) | 0.19065 (3) | 0.964296 (11) | 0.03913 (11) | |
O1 | 0.84635 (15) | −0.0360 (4) | 0.91890 (15) | 0.0436 (7) | |
O2 | 0.94655 (17) | −0.1384 (4) | 0.97708 (16) | 0.0493 (8) | |
O3 | 0.93994 (17) | 0.4208 (4) | 1.03403 (15) | 0.0473 (8) | |
O4 | 0.97062 (17) | 0.0607 (4) | 0.87489 (15) | 0.0466 (8) | |
O5 | 1.06707 (17) | −0.0828 (4) | 0.92160 (15) | 0.0487 (8) | |
O6 | 1.11849 (19) | −0.0172 (5) | 0.82196 (18) | 0.0659 (10) | |
O7 | 0.7848 (2) | −0.3263 (4) | 0.8976 (2) | 0.0616 (10) | |
O8 | 1.00768 (19) | 0.6128 (4) | 1.09070 (16) | 0.0556 (9) | |
O9 | 0.9869 (2) | 0.5278 (4) | 1.20624 (16) | 0.0612 (10) | |
N1 | 0.7969 (2) | 0.2338 (5) | 0.9666 (2) | 0.0474 (10) | |
N2 | 0.8341 (2) | 0.3065 (4) | 0.8546 (2) | 0.0478 (10) | |
N3 | 1.1131 (4) | 0.1068 (9) | 0.7156 (3) | 0.113 (2) | |
N4 | 0.7850 (5) | −0.2799 (8) | 1.0109 (5) | 0.1287 (16) | |
N5 | 0.9273 (3) | 0.3784 (9) | 1.2711 (3) | 0.0954 (18) | |
C1 | 0.7784 (3) | 0.1916 (6) | 1.0202 (3) | 0.0624 (15) | |
H1 | 0.8130 | 0.1695 | 1.0603 | 0.075* | |
C2 | 0.7091 (3) | 0.1788 (8) | 1.0193 (4) | 0.081 (2) | |
H2 | 0.6978 | 0.1479 | 1.0579 | 0.097* | |
C3 | 0.6580 (3) | 0.2123 (9) | 0.9608 (4) | 0.089 (2) | |
H3 | 0.6116 | 0.2042 | 0.9597 | 0.106* | |
C4 | 0.6741 (3) | 0.2567 (9) | 0.9048 (4) | 0.0740 (18) | |
C5 | 0.7462 (3) | 0.2669 (6) | 0.9090 (3) | 0.0519 (13) | |
C6 | 0.6226 (4) | 0.2959 (11) | 0.8403 (5) | 0.109 (3) | |
H6 | 0.5754 | 0.2866 | 0.8361 | 0.131* | |
C7 | 0.6423 (4) | 0.3443 (10) | 0.7882 (4) | 0.102 (3) | |
H7 | 0.6083 | 0.3728 | 0.7486 | 0.122* | |
C8 | 0.7131 (3) | 0.3546 (8) | 0.7900 (3) | 0.0695 (17) | |
C9 | 0.7665 (3) | 0.3093 (5) | 0.8510 (3) | 0.0520 (13) | |
C10 | 0.7361 (4) | 0.4039 (8) | 0.7369 (3) | 0.085 (2) | |
H10 | 0.7040 | 0.4395 | 0.6973 | 0.102* | |
C11 | 0.8034 (4) | 0.4016 (8) | 0.7411 (3) | 0.0791 (19) | |
H11 | 0.8179 | 0.4344 | 0.7045 | 0.095* | |
C12 | 0.8525 (3) | 0.3495 (7) | 0.8009 (3) | 0.0627 (15) | |
H12 | 0.8992 | 0.3452 | 0.8028 | 0.075* | |
C13 | 0.8839 (3) | −0.1511 (6) | 0.9390 (2) | 0.0435 (11) | |
C14 | 0.8574 (3) | −0.3142 (6) | 0.9194 (3) | 0.0545 (13) | |
H14A | 0.8753 | −0.3513 | 0.8834 | 0.065* | |
H14B | 0.8753 | −0.3843 | 0.9579 | 0.065* | |
C15 | 0.7520 (7) | −0.3150 (9) | 0.9438 (7) | 0.1287 (16) | |
C16 | 0.6802 (6) | −0.3400 (10) | 0.9208 (6) | 0.1287 (16) | |
H16 | 0.6594 | −0.3615 | 0.8752 | 0.154* | |
C17 | 0.6397 (6) | −0.3341 (10) | 0.9629 (6) | 0.1287 (16) | |
H17 | 0.5923 | −0.3556 | 0.9479 | 0.154* | |
C18 | 0.6728 (6) | −0.2943 (10) | 1.0291 (6) | 0.1287 (16) | |
H18 | 0.6457 | −0.2852 | 1.0583 | 0.154* | |
C19 | 0.7388 (6) | −0.2688 (11) | 1.0536 (6) | 0.1287 (16) | |
H19 | 0.7572 | −0.2429 | 1.0991 | 0.154* | |
C20 | 0.9695 (3) | 0.4990 (6) | 1.0865 (2) | 0.0435 (11) | |
C21 | 0.9488 (3) | 0.4452 (7) | 1.1475 (2) | 0.0559 (13) | |
H21A | 0.8995 | 0.4640 | 1.1396 | 0.067* | |
H21B | 0.9572 | 0.3318 | 1.1541 | 0.067* | |
C22 | 0.9747 (3) | 0.4893 (6) | 1.2653 (2) | 0.0540 (13) | |
C23 | 1.0147 (3) | 0.5696 (8) | 1.3221 (3) | 0.0700 (16) | |
H23 | 1.0482 | 0.6423 | 1.3183 | 0.084* | |
C24 | 1.0049 (4) | 0.5417 (9) | 1.3835 (3) | 0.090 (2) | |
H24 | 1.0313 | 0.5967 | 1.4214 | 0.108* | |
C25 | 0.9566 (4) | 0.4339 (11) | 1.3898 (3) | 0.102 (3) | |
H25 | 0.9493 | 0.4168 | 1.4316 | 0.123* | |
C26 | 0.9193 (5) | 0.3518 (11) | 1.3346 (4) | 0.104 (3) | |
H26 | 0.8876 | 0.2755 | 1.3394 | 0.125* | |
C27 | 1.0287 (3) | 0.0030 (5) | 0.8773 (2) | 0.0426 (11) | |
C28 | 1.0524 (3) | 0.0515 (7) | 0.8172 (3) | 0.0551 (13) | |
H28B | 1.0185 | 0.0165 | 0.7758 | 0.066* | |
H28A | 1.0557 | 0.1666 | 0.8157 | 0.066* | |
C29 | 1.1461 (3) | 0.0138 (7) | 0.7707 (3) | 0.0615 (14) | |
C30 | 1.2081 (3) | −0.0571 (8) | 0.7763 (3) | 0.0766 (18) | |
H30 | 1.2291 | −0.1193 | 0.8141 | 0.092* | |
C31 | 1.2402 (4) | −0.0377 (9) | 0.7267 (5) | 0.093 (2) | |
H31 | 1.2827 | −0.0869 | 0.7308 | 0.111* | |
C32 | 1.2103 (5) | 0.0519 (9) | 0.6726 (5) | 0.104 (3) | |
H32 | 1.2324 | 0.0651 | 0.6394 | 0.125* | |
C33 | 1.1489 (5) | 0.1231 (11) | 0.6652 (4) | 0.108 (3) | |
H33 | 1.1291 | 0.1842 | 0.6268 | 0.130* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nd1 | 0.04630 (17) | 0.03256 (17) | 0.03352 (16) | −0.00149 (11) | 0.00407 (10) | 0.00062 (10) |
O1 | 0.0453 (17) | 0.0325 (18) | 0.0453 (18) | 0.0007 (14) | 0.0014 (14) | −0.0035 (14) |
O2 | 0.0472 (19) | 0.0473 (19) | 0.0442 (19) | −0.0032 (16) | −0.0004 (15) | 0.0077 (15) |
O3 | 0.069 (2) | 0.0305 (17) | 0.0406 (18) | −0.0048 (16) | 0.0131 (15) | −0.0036 (14) |
O4 | 0.058 (2) | 0.0430 (19) | 0.0386 (17) | 0.0057 (17) | 0.0135 (15) | 0.0010 (15) |
O5 | 0.061 (2) | 0.047 (2) | 0.0393 (18) | 0.0069 (17) | 0.0160 (15) | 0.0100 (15) |
O6 | 0.068 (2) | 0.081 (3) | 0.055 (2) | 0.018 (2) | 0.0287 (19) | 0.0201 (19) |
O7 | 0.059 (2) | 0.044 (2) | 0.070 (3) | −0.0138 (17) | −0.0001 (19) | −0.0070 (17) |
O8 | 0.083 (3) | 0.047 (2) | 0.0369 (18) | −0.026 (2) | 0.0179 (17) | −0.0040 (15) |
O9 | 0.087 (3) | 0.058 (2) | 0.0380 (19) | −0.027 (2) | 0.0185 (18) | −0.0061 (16) |
N1 | 0.048 (2) | 0.037 (2) | 0.049 (2) | 0.0042 (18) | 0.0030 (19) | −0.0083 (18) |
N2 | 0.062 (3) | 0.036 (2) | 0.036 (2) | 0.0044 (19) | 0.0001 (18) | 0.0002 (17) |
N3 | 0.143 (6) | 0.116 (5) | 0.100 (5) | −0.007 (5) | 0.069 (5) | 0.020 (4) |
N4 | 0.154 (4) | 0.086 (2) | 0.172 (4) | 0.015 (3) | 0.088 (4) | 0.028 (3) |
N5 | 0.098 (4) | 0.115 (5) | 0.077 (4) | −0.034 (4) | 0.031 (3) | 0.001 (4) |
C1 | 0.059 (3) | 0.071 (4) | 0.056 (3) | 0.008 (3) | 0.015 (3) | −0.003 (3) |
C2 | 0.060 (4) | 0.107 (6) | 0.083 (5) | 0.002 (4) | 0.031 (4) | −0.013 (4) |
C3 | 0.046 (3) | 0.105 (6) | 0.114 (7) | −0.005 (3) | 0.021 (4) | −0.017 (5) |
C4 | 0.052 (3) | 0.081 (4) | 0.073 (4) | 0.006 (3) | −0.007 (3) | −0.017 (4) |
C5 | 0.053 (3) | 0.036 (3) | 0.057 (3) | 0.008 (2) | 0.002 (2) | −0.009 (2) |
C6 | 0.064 (5) | 0.139 (9) | 0.098 (7) | 0.016 (5) | −0.017 (4) | −0.035 (6) |
C7 | 0.077 (5) | 0.108 (6) | 0.084 (5) | 0.039 (4) | −0.033 (4) | −0.023 (5) |
C8 | 0.074 (4) | 0.060 (4) | 0.050 (4) | 0.018 (3) | −0.019 (3) | −0.011 (3) |
C9 | 0.059 (3) | 0.033 (3) | 0.046 (3) | 0.007 (2) | −0.012 (2) | −0.004 (2) |
C10 | 0.116 (6) | 0.068 (5) | 0.044 (4) | 0.016 (4) | −0.019 (4) | 0.000 (3) |
C11 | 0.118 (6) | 0.072 (5) | 0.035 (3) | 0.001 (4) | 0.003 (3) | 0.011 (3) |
C12 | 0.081 (4) | 0.048 (3) | 0.049 (3) | −0.002 (3) | 0.005 (3) | 0.008 (2) |
C13 | 0.048 (3) | 0.048 (3) | 0.031 (2) | −0.005 (2) | 0.006 (2) | −0.003 (2) |
C14 | 0.062 (3) | 0.044 (3) | 0.052 (3) | 0.002 (2) | 0.009 (3) | −0.008 (2) |
C15 | 0.154 (4) | 0.086 (2) | 0.172 (4) | 0.015 (3) | 0.088 (4) | 0.028 (3) |
C16 | 0.154 (4) | 0.086 (2) | 0.172 (4) | 0.015 (3) | 0.088 (4) | 0.028 (3) |
C17 | 0.154 (4) | 0.086 (2) | 0.172 (4) | 0.015 (3) | 0.088 (4) | 0.028 (3) |
C18 | 0.154 (4) | 0.086 (2) | 0.172 (4) | 0.015 (3) | 0.088 (4) | 0.028 (3) |
C19 | 0.154 (4) | 0.086 (2) | 0.172 (4) | 0.015 (3) | 0.088 (4) | 0.028 (3) |
C20 | 0.060 (3) | 0.032 (3) | 0.038 (3) | −0.001 (2) | 0.014 (2) | 0.001 (2) |
C21 | 0.077 (4) | 0.049 (3) | 0.043 (3) | −0.020 (3) | 0.020 (2) | −0.004 (2) |
C22 | 0.072 (3) | 0.052 (3) | 0.039 (3) | −0.005 (3) | 0.018 (2) | 0.003 (2) |
C23 | 0.086 (4) | 0.071 (4) | 0.050 (3) | −0.020 (3) | 0.016 (3) | −0.011 (3) |
C24 | 0.122 (6) | 0.100 (5) | 0.039 (3) | −0.019 (5) | 0.011 (3) | −0.011 (3) |
C25 | 0.127 (6) | 0.138 (7) | 0.050 (4) | −0.028 (6) | 0.039 (4) | 0.009 (4) |
C26 | 0.128 (7) | 0.132 (7) | 0.066 (5) | −0.054 (6) | 0.048 (5) | −0.002 (4) |
C27 | 0.055 (3) | 0.033 (3) | 0.038 (3) | −0.006 (2) | 0.011 (2) | −0.003 (2) |
C28 | 0.065 (3) | 0.055 (3) | 0.047 (3) | 0.005 (3) | 0.019 (2) | 0.012 (2) |
C29 | 0.073 (4) | 0.064 (4) | 0.056 (3) | −0.008 (3) | 0.032 (3) | 0.005 (3) |
C30 | 0.079 (4) | 0.090 (5) | 0.071 (4) | 0.001 (4) | 0.038 (3) | 0.000 (4) |
C31 | 0.093 (5) | 0.091 (6) | 0.113 (6) | −0.006 (4) | 0.060 (5) | −0.008 (5) |
C32 | 0.140 (7) | 0.081 (5) | 0.131 (7) | −0.018 (5) | 0.100 (6) | −0.007 (5) |
C33 | 0.163 (8) | 0.099 (6) | 0.093 (6) | 0.010 (6) | 0.083 (6) | 0.028 (5) |
Nd1—O1 | 2.544 (3) | C6—H6 | 0.9300 |
Nd1—O2 | 2.784 (4) | C7—C8 | 1.418 (11) |
Nd1—O2i | 2.439 (3) | C7—H7 | 0.9300 |
Nd1—O3 | 2.387 (3) | C8—C10 | 1.376 (10) |
Nd1—O4 | 2.471 (3) | C8—C9 | 1.444 (7) |
Nd1—O5i | 2.519 (3) | C10—C11 | 1.332 (9) |
Nd1—O8ii | 2.522 (3) | C10—H10 | 0.9300 |
Nd1—N1 | 2.742 (4) | C11—C12 | 1.406 (8) |
Nd1—N2 | 2.701 (4) | C11—H11 | 0.9300 |
O1—C13 | 1.222 (6) | C12—H12 | 0.9300 |
O2—C13 | 1.278 (6) | C13—C14 | 1.482 (7) |
O2—Nd1i | 2.439 (3) | C14—H14A | 0.9700 |
O3—C20 | 1.258 (5) | C14—H14B | 0.9700 |
O4—C27 | 1.252 (5) | C15—C16 | 1.398 (15) |
O5—C27 | 1.239 (5) | C16—C17 | 1.358 (12) |
O5—Nd1i | 2.519 (3) | C16—H16 | 0.9300 |
O6—C29 | 1.360 (6) | C17—C18 | 1.374 (15) |
O6—C28 | 1.427 (6) | C17—H17 | 0.9300 |
O7—C15 | 1.316 (11) | C18—C19 | 1.292 (14) |
O7—C14 | 1.399 (6) | C18—H18 | 0.9300 |
O8—C20 | 1.213 (6) | C19—H19 | 0.9300 |
O8—Nd1ii | 2.522 (3) | C20—C21 | 1.509 (6) |
O9—C22 | 1.354 (6) | C21—H21A | 0.9700 |
O9—C21 | 1.413 (6) | C21—H21B | 0.9700 |
N1—C1 | 1.318 (7) | C22—C23 | 1.388 (7) |
N1—C5 | 1.348 (6) | C23—C24 | 1.362 (8) |
N2—C12 | 1.321 (7) | C23—H23 | 0.9300 |
N2—C9 | 1.340 (7) | C24—C25 | 1.363 (10) |
N3—C29 | 1.380 (9) | C24—H24 | 0.9300 |
N3—C33 | 1.439 (9) | C25—C26 | 1.355 (10) |
N4—C15 | 1.382 (14) | C25—H25 | 0.9300 |
N4—C19 | 1.462 (12) | C26—H26 | 0.9300 |
N5—C22 | 1.365 (8) | C27—C28 | 1.514 (7) |
N5—C26 | 1.387 (8) | C28—H28B | 0.9700 |
C1—C2 | 1.394 (8) | C28—H28A | 0.9700 |
C1—H1 | 0.9300 | C29—C30 | 1.356 (8) |
C2—C3 | 1.365 (10) | C30—C31 | 1.375 (9) |
C2—H2 | 0.9300 | C30—H30 | 0.9300 |
C3—C4 | 1.345 (10) | C31—C32 | 1.336 (11) |
C3—H3 | 0.9300 | C31—H31 | 0.9300 |
C4—C5 | 1.431 (8) | C32—C33 | 1.339 (11) |
C4—C6 | 1.464 (10) | C32—H32 | 0.9300 |
C5—C9 | 1.422 (8) | C33—H33 | 0.9300 |
C6—C7 | 1.318 (12) | ||
O1—Nd1—O2 | 48.39 (9) | C5—C9—C8 | 118.6 (5) |
O1—Nd1—O3 | 138.63 (11) | C11—C10—C8 | 121.3 (6) |
O1—Nd1—O4 | 73.88 (11) | C11—C10—H10 | 119.4 |
O2—Nd1—O3 | 139.46 (10) | C8—C10—H10 | 119.4 |
O2—Nd1—O4 | 65.28 (10) | C10—C11—C12 | 119.9 (6) |
O3—Nd1—O4 | 145.80 (11) | C10—C11—H11 | 120.1 |
O1—Nd1—N1 | 63.12 (11) | C12—C11—H11 | 120.1 |
O2—Nd1—N1 | 102.23 (11) | N2—C12—C11 | 121.7 (6) |
O3—Nd1—N1 | 77.25 (12) | N2—C12—H12 | 119.1 |
O4—Nd1—N1 | 127.42 (11) | C11—C12—H12 | 119.1 |
O1—Nd1—N2 | 73.72 (11) | O1—C13—O2 | 122.8 (4) |
O2—Nd1—N2 | 118.03 (10) | O1—C13—C14 | 120.1 (4) |
O3—Nd1—N2 | 96.98 (11) | O2—C13—C14 | 117.1 (5) |
O4—Nd1—N2 | 80.97 (11) | O7—C14—C13 | 114.4 (4) |
N1—Nd1—N2 | 59.65 (13) | O7—C14—H14A | 108.7 |
O3—Nd1—O2i | 87.83 (12) | C13—C14—H14A | 108.7 |
O2i—Nd1—O4 | 78.04 (11) | O7—C14—H14B | 108.7 |
O3—Nd1—O5i | 75.33 (10) | C13—C14—H14B | 108.7 |
O2i—Nd1—O5i | 74.76 (11) | H14A—C14—H14B | 107.6 |
O4—Nd1—O5i | 128.61 (11) | O7—C15—N4 | 123.3 (11) |
O3—Nd1—O8ii | 77.52 (11) | O7—C15—C16 | 115.6 (12) |
O2i—Nd1—O8ii | 77.72 (12) | N4—C15—C16 | 121.1 (11) |
O4—Nd1—O8ii | 69.15 (11) | C17—C16—C15 | 122.1 (13) |
O5i—Nd1—O8ii | 141.70 (11) | C17—C16—H16 | 118.9 |
O2i—Nd1—O1 | 121.12 (12) | C15—C16—H16 | 118.9 |
O5i—Nd1—O1 | 84.18 (11) | C16—C17—C18 | 116.2 (12) |
O8ii—Nd1—O1 | 133.38 (10) | C16—C17—H17 | 121.9 |
O2i—Nd1—N2 | 148.81 (12) | C18—C17—H17 | 121.9 |
O5i—Nd1—N2 | 136.30 (12) | C19—C18—C17 | 124.8 (12) |
O8ii—Nd1—N2 | 73.35 (12) | C19—C18—H18 | 117.6 |
O2i—Nd1—N1 | 150.42 (12) | C17—C18—H18 | 117.6 |
O5i—Nd1—N1 | 76.80 (12) | C18—C19—N4 | 121.1 (12) |
O8ii—Nd1—N1 | 122.43 (13) | C18—C19—H19 | 119.5 |
O2i—Nd1—O2 | 72.96 (13) | N4—C19—H19 | 119.5 |
O5i—Nd1—O2 | 65.40 (10) | O8—C20—O3 | 126.9 (4) |
O8ii—Nd1—O2 | 129.58 (11) | O8—C20—C21 | 120.2 (4) |
C13—O1—Nd1 | 100.8 (3) | O3—C20—C21 | 112.8 (4) |
C13—O2—Nd1i | 163.1 (3) | O9—C21—C20 | 111.0 (4) |
C13—O2—Nd1 | 87.9 (3) | O9—C21—H21A | 109.4 |
Nd1i—O2—Nd1 | 107.04 (12) | C20—C21—H21A | 109.4 |
C20—O3—Nd1 | 151.1 (3) | O9—C21—H21B | 109.4 |
C27—O4—Nd1 | 130.0 (3) | C20—C21—H21B | 109.4 |
C27—O5—Nd1i | 137.2 (3) | H21A—C21—H21B | 108.0 |
C29—O6—C28 | 117.2 (4) | O9—C22—N5 | 124.1 (5) |
C15—O7—C14 | 117.4 (7) | O9—C22—C23 | 115.7 (5) |
C20—O8—Nd1ii | 150.1 (3) | N5—C22—C23 | 120.2 (5) |
C22—O9—C21 | 117.5 (4) | C24—C23—C22 | 119.9 (6) |
C1—N1—C5 | 118.2 (5) | C24—C23—H23 | 120.0 |
C1—N1—Nd1 | 120.2 (3) | C22—C23—H23 | 120.0 |
C5—N1—Nd1 | 120.2 (3) | C23—C24—C25 | 120.5 (6) |
C12—N2—C9 | 118.8 (4) | C23—C24—H24 | 119.7 |
C12—N2—Nd1 | 119.4 (4) | C25—C24—H24 | 119.7 |
C9—N2—Nd1 | 121.6 (3) | C26—C25—C24 | 119.3 (6) |
C29—N3—C33 | 115.5 (7) | C26—C25—H25 | 120.3 |
C15—N4—C19 | 114.6 (10) | C24—C25—H25 | 120.3 |
C22—N5—C26 | 118.3 (6) | C25—C26—N5 | 121.8 (7) |
N1—C1—C2 | 122.6 (6) | C25—C26—H26 | 119.1 |
N1—C1—H1 | 118.7 | N5—C26—H26 | 119.1 |
C2—C1—H1 | 118.7 | O5—C27—O4 | 128.7 (4) |
C3—C2—C1 | 119.0 (6) | O5—C27—C28 | 119.0 (4) |
C3—C2—H2 | 120.5 | O4—C27—C28 | 112.3 (4) |
C1—C2—H2 | 120.5 | O6—C28—C27 | 110.4 (4) |
C4—C3—C2 | 120.7 (6) | O6—C28—H28B | 109.6 |
C4—C3—H3 | 119.6 | C27—C28—H28B | 109.6 |
C2—C3—H3 | 119.6 | O6—C28—H28A | 109.6 |
C3—C4—C5 | 117.6 (6) | C27—C28—H28A | 109.6 |
C3—C4—C6 | 124.1 (7) | H28B—C28—H28A | 108.1 |
C5—C4—C6 | 118.3 (7) | C30—C29—O6 | 115.3 (5) |
N1—C5—C9 | 117.9 (5) | C30—C29—N3 | 121.7 (6) |
N1—C5—C4 | 121.9 (5) | O6—C29—N3 | 123.0 (5) |
C9—C5—C4 | 120.2 (5) | C29—C30—C31 | 120.5 (7) |
C7—C6—C4 | 120.7 (8) | C29—C30—H30 | 119.8 |
C7—C6—H6 | 119.6 | C31—C30—H30 | 119.8 |
C4—C6—H6 | 119.6 | C32—C31—C30 | 119.8 (7) |
C6—C7—C8 | 122.7 (7) | C32—C31—H31 | 120.1 |
C6—C7—H7 | 118.6 | C30—C31—H31 | 120.1 |
C8—C7—H7 | 118.6 | C31—C32—C33 | 121.3 (7) |
C10—C8—C7 | 124.8 (6) | C31—C32—H32 | 119.4 |
C10—C8—C9 | 116.0 (6) | C33—C32—H32 | 119.4 |
C7—C8—C9 | 119.3 (7) | C32—C33—N3 | 121.2 (8) |
N2—C9—C5 | 119.2 (4) | C32—C33—H33 | 119.4 |
N2—C9—C8 | 122.2 (5) | N3—C33—H33 | 119.4 |
Symmetry codes: (i) −x+2, −y, −z+2; (ii) −x+2, −y+1, −z+2. |
D—H···A | D—H | H···A | D···A | D—H···A |
C10—H10···O1iii | 0.93 | 2.32 | 3.198 (7) | 157 |
C14—H14B···O3iv | 0.97 | 2.37 | 3.317 (6) | 164 |
C12—H12···O8ii | 0.93 | 2.46 | 3.051 (7) | 122 |
C1—H1···O5i | 0.93 | 2.44 | 3.120 (7) | 130 |
Symmetry codes: (i) −x+2, −y, −z+2; (ii) −x+2, −y+1, −z+2; (iii) −x+3/2, y+1/2, −z+3/2; (iv) x, y−1, z. |
Experimental details
Crystal data | |
Chemical formula | [Nd2(C7H6NO3)6(C12H8N2)2] |
Mr | 1561.66 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 273 |
a, b, c (Å) | 20.1233 (11), 8.3987 (12), 20.6864 (13) |
β (°) | 107.207 (6) |
V (Å3) | 3339.7 (6) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.62 |
Crystal size (mm) | 0.33 × 0.13 × 0.08 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.620, 0.880 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 25069, 6771, 4723 |
Rint | 0.041 |
(sin θ/λ)max (Å−1) | 0.626 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.042, 0.128, 0.99 |
No. of reflections | 6771 |
No. of parameters | 403 |
No. of restraints | 3 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.67, −0.67 |
Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Siemens, 1996), SHELXTL.
Nd1—O1 | 2.544 (3) | Nd1—O5i | 2.519 (3) |
Nd1—O2 | 2.784 (4) | Nd1—O8ii | 2.522 (3) |
Nd1—O2i | 2.439 (3) | Nd1—N1 | 2.742 (4) |
Nd1—O3 | 2.387 (3) | Nd1—N2 | 2.701 (4) |
Nd1—O4 | 2.471 (3) | ||
O1—Nd1—O2 | 48.39 (9) | O3—Nd1—N1 | 77.25 (12) |
O1—Nd1—O3 | 138.63 (11) | O4—Nd1—N1 | 127.42 (11) |
O1—Nd1—O4 | 73.88 (11) | O1—Nd1—N2 | 73.72 (11) |
O2—Nd1—O3 | 139.46 (10) | O2—Nd1—N2 | 118.03 (10) |
O2—Nd1—O4 | 65.28 (10) | O3—Nd1—N2 | 96.98 (11) |
O3—Nd1—O4 | 145.80 (11) | O4—Nd1—N2 | 80.97 (11) |
O1—Nd1—N1 | 63.12 (11) | N1—Nd1—N2 | 59.65 (13) |
O2—Nd1—N1 | 102.23 (11) |
Symmetry codes: (i) −x+2, −y, −z+2; (ii) −x+2, −y+1, −z+2. |
D—H···A | D—H | H···A | D···A | D—H···A |
C10—H10···O1iii | 0.93 | 2.32 | 3.198 (7) | 157 |
C14—H14B···O3iv | 0.97 | 2.37 | 3.317 (6) | 164 |
C12—H12···O8ii | 0.93 | 2.46 | 3.051 (7) | 122 |
C1—H1···O5i | 0.93 | 2.44 | 3.120 (7) | 130 |
Symmetry codes: (i) −x+2, −y, −z+2; (ii) −x+2, −y+1, −z+2; (iii) −x+3/2, y+1/2, −z+3/2; (iv) x, y−1, z. |
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The crystal structures of tetrakis(µ-(2-pyridyloxy)acetato)bis[(1,10-phenanthroline)((2-pyridyloxy)acetato) lanthanum(III)], (II), (Liu et al., 2007a) and tetrakis(µ-(2-pyridyloxy)acetato) bis[(1,10-phenanthroline)((2-pyridyloxy)acetato)praseodymium(III)], (III), (Liu et al., 2007b) have previously been reported. The crystal structure determination of the title compound, (I), has been carried out in order to elucidate the molecular conformation and to compare it with those of (II) and (III).
In the molecule of (I) (Fig. 1), the ligand bond lengths and angles are within normal ranges (Allen et al., 1987). It has an inversion centre between the two NdIII ions, in which they are bridged by the two terdentate and the two bidentate carboxylate groups. Each Nd atom is seven-coordinated by the two N atoms of 1,10-phenanthroline (phen) ligand and the five O atoms of 2-pyridyloxy- acetic acid ligands. The Nd—O and Nd—N bonds are in the range of [2.387 (3)–2.784 (4) Å] and [2.701 (4)–2.742 (4) Å], respectively (Table 1), as in (II) and (III).
In the crystal structure, intermolecular C—H···O hydrogen bonds (Table 2) lead to a supramolecular network structure (Fig. 2), in which they may be effective in the stabilization of the structure, as in (II) and (III).
The compounds, (I), (II) and (III), are isostructural.