Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680702137X/dn2162sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680702137X/dn2162Isup2.hkl |
CCDC reference: 650592
To a solution of 0.2 mmol gadolinium picrate in 5 ml of ethanol was added dropwise the solution of 0.2 mmol ligand in 10 ml of ethanol. The mixture was stirred at room temperature for 6 h. The precipitated solid complex was filtered, washed with ethanol and dried in vacuo over P2O5 for 72 h. The complex was obtained as yellow powder. Single crystal of the gadolinium complex grew from CH3Cl and CH3CH2OH by slow evaporation at room temperature. After about two weeks, yellow crystal formed from the solution.
All H atoms attached were fixed geometrically and treated as riding with C—H = 0.93 Å (Caromatic), 0.97 Å (Cmethylene) and C—H =0.96 Å (Cmethyl) with Uiso(H) = 1.2Ueq(Caromatic or Cmethylene) and Uiso(H) = 1.5Ueq(Cmethyl).
Metal-directed self-assembly of organic ligands and metal ions, or organometallic moieties, to form well defined structures has been a very attractive field in recent years (Lehn, 1995; Steed & Atwood, 2000; Bourne et al., 2001;), for their fascinating structural diversities and potential application in functional materials, nanotechnology and biological recognition (Evan & Lin, 2002; Janiak, 2003; Carlucci et al., 2003; Gutschke et al., 1996;). We have now investigated the assembly of the ligand N-phenyl-2-{2'-[(phenyl- ethyl-carbamoyl)-methoxy]-biphenyl-2-yloxy}-N-ethyl-acetamide with gadolinium picrate.
In the title complex I, The Gd(III) ion is coordinated by 9 oxygen donor atoms, five of them belonging to two bidentate and one monodentate picrate groups whereas the remaining four are from the tetradentate ligand L(Fig. 1). The coordination polyhedron around Gd(III) ion is a distorted tricapped trigonal prism (Fig. 2) (Wang et al., 2003). The quadridentate ligand wraps around the metal ion with its oxygen atoms and forms a ring-like coordination structure together with the Gd atom. The two phenyl rings about the central bond in the molecule have a drastic twisting, with the dihedral angle between them being 61.18°. The mean distances between the Gd atom and the coordinated ether and carbonyl oxygen atoms are 2.575 Å and 2.3105 Å, respectively. This suggests that the Gd—O (C?O) bond is stronger than the Gd—O (C—O—C) bond.
For general backgound, see: Lehn, 1995; Steed & Atwood, 2000; Bourne et al., 2001; Evan & Lin, 2002; Janiak, 2003; Carlucci et al., 2003; Gutschke et al., 1996. For related structures, see: Wang et al., 2003.
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.
[Gd(C6H2N3O7)3(C32H32N2O4)] | F(000) = 2716 |
Mr = 1350.16 | Dx = 1.652 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 8109 reflections |
a = 20.125 (2) Å | θ = 2.2–25.3° |
b = 16.7778 (18) Å | µ = 1.32 mm−1 |
c = 16.6491 (18) Å | T = 298 K |
β = 105.051 (2)° | Block, yellow |
V = 5428.9 (10) Å3 | 0.40 × 0.37 × 0.29 mm |
Z = 4 |
Bruker SMART CCD area detector diffractometer | 9559 independent reflections |
Radiation source: fine-focus sealed tube | 6585 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.036 |
phi and ω scans | θmax = 25.0°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −16→23 |
Tmin = 0.620, Tmax = 0.701 | k = −19→19 |
28190 measured reflections | l = −19→17 |
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)] = 0.036 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.087 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0225P)2 + 8.0112P] where P = (Fo2 + 2Fc2)/3 |
9559 reflections | (Δ/σ)max = 0.002 |
786 parameters | Δρmax = 1.50 e Å−3 |
0 restraints | Δρmin = −0.58 e Å−3 |
[Gd(C6H2N3O7)3(C32H32N2O4)] | V = 5428.9 (10) Å3 |
Mr = 1350.16 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 20.125 (2) Å | µ = 1.32 mm−1 |
b = 16.7778 (18) Å | T = 298 K |
c = 16.6491 (18) Å | 0.40 × 0.37 × 0.29 mm |
β = 105.051 (2)° |
Bruker SMART CCD area detector diffractometer | 9559 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 6585 reflections with I > 2σ(I) |
Tmin = 0.620, Tmax = 0.701 | Rint = 0.036 |
28190 measured reflections |
R[F2 > 2σ(F2)] = 0.036 | 0 restraints |
wR(F2) = 0.087 | H-atom parameters constrained |
S = 1.08 | Δρmax = 1.50 e Å−3 |
9559 reflections | Δρmin = −0.58 e Å−3 |
786 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 | ||
Gd | 0.749509 (11) | 0.628330 (12) | 0.769967 (14) | 0.03694 (8) | |
N1 | 0.9530 (2) | 0.7437 (2) | 0.8655 (3) | 0.0527 (11) | |
N2 | 0.5485 (2) | 0.7472 (3) | 0.6819 (3) | 0.0604 (12) | |
N3 | 0.6661 (2) | 0.4428 (3) | 0.7896 (3) | 0.0558 (11) | |
N4 | 0.7446 (4) | 0.1794 (3) | 0.7376 (3) | 0.0817 (17) | |
N5 | 0.8962 (2) | 0.4044 (3) | 0.7360 (3) | 0.0580 (11) | |
N6 | 0.8047 (2) | 0.5775 (2) | 0.5830 (3) | 0.0526 (11) | |
N7 | 0.7101 (3) | 0.3392 (3) | 0.4317 (3) | 0.0794 (15) | |
N8 | 0.5725 (2) | 0.4815 (3) | 0.5851 (3) | 0.0649 (13) | |
N9 | 0.9043 (3) | 0.5088 (3) | 0.9422 (3) | 0.0657 (13) | |
N10 | 0.7864 (4) | 0.3033 (3) | 1.0554 (3) | 0.0798 (16) | |
N11 | 0.6777 (3) | 0.5639 (3) | 0.9963 (4) | 0.0712 (14) | |
O1 | 0.85746 (15) | 0.68313 (18) | 0.7941 (2) | 0.0476 (8) | |
O2 | 0.77451 (14) | 0.75760 (16) | 0.85945 (19) | 0.0421 (8) | |
O3 | 0.64424 (14) | 0.69007 (17) | 0.75993 (19) | 0.0411 (7) | |
O4 | 0.72718 (14) | 0.75474 (16) | 0.68295 (18) | 0.0398 (7) | |
O5 | 0.79637 (15) | 0.50497 (16) | 0.7700 (2) | 0.0456 (8) | |
O6 | 0.66987 (17) | 0.51556 (19) | 0.7911 (2) | 0.0602 (10) | |
O7 | 0.6175 (2) | 0.4090 (2) | 0.8044 (3) | 0.1057 (17) | |
O8 | 0.6861 (3) | 0.1556 (2) | 0.7312 (3) | 0.1065 (17) | |
O9 | 0.7935 (3) | 0.1368 (2) | 0.7345 (3) | 0.1079 (17) | |
O10 | 0.9479 (2) | 0.3659 (2) | 0.7687 (3) | 0.0836 (12) | |
O11 | 0.8964 (2) | 0.4630 (2) | 0.6944 (3) | 0.0776 (12) | |
O12 | 0.68209 (16) | 0.58803 (18) | 0.6408 (2) | 0.0524 (9) | |
O13 | 0.81129 (17) | 0.62156 (19) | 0.6441 (2) | 0.0576 (9) | |
O14 | 0.8431 (2) | 0.5811 (2) | 0.5371 (3) | 0.0747 (11) | |
O15 | 0.7645 (3) | 0.3316 (3) | 0.4143 (3) | 0.1159 (19) | |
O16 | 0.6607 (3) | 0.2947 (3) | 0.4072 (3) | 0.0965 (15) | |
O17 | 0.5489 (2) | 0.4223 (3) | 0.6085 (3) | 0.1105 (17) | |
O18 | 0.5445 (2) | 0.5463 (3) | 0.5762 (3) | 0.0924 (14) | |
O19 | 0.78189 (17) | 0.60133 (18) | 0.9109 (2) | 0.0557 (9) | |
O20 | 0.9221 (2) | 0.5779 (3) | 0.9556 (3) | 0.0882 (13) | |
O21 | 0.9358 (2) | 0.4588 (3) | 0.9138 (3) | 0.0891 (13) | |
O22 | 0.8388 (3) | 0.2635 (3) | 1.0675 (3) | 0.1086 (17) | |
O23 | 0.7321 (3) | 0.2800 (2) | 1.0683 (3) | 0.0938 (14) | |
O24 | 0.6489 (2) | 0.5496 (3) | 1.0510 (3) | 0.0947 (15) | |
O25 | 0.6636 (3) | 0.6196 (3) | 0.9512 (4) | 0.135 (2) | |
C1 | 0.7289 (2) | 0.8213 (3) | 0.8567 (3) | 0.0438 (12) | |
C2 | 0.6850 (3) | 0.8186 (3) | 0.9071 (3) | 0.0571 (14) | |
H2 | 0.6882 | 0.7775 | 0.9455 | 0.069* | |
C3 | 0.6358 (3) | 0.8777 (4) | 0.9003 (4) | 0.0713 (17) | |
H3 | 0.6048 | 0.8759 | 0.9330 | 0.086* | |
C4 | 0.6330 (3) | 0.9391 (4) | 0.8450 (4) | 0.081 (2) | |
H4 | 0.6005 | 0.9792 | 0.8413 | 0.097* | |
C5 | 0.6779 (3) | 0.9420 (3) | 0.7950 (4) | 0.0713 (17) | |
H5 | 0.6759 | 0.9845 | 0.7587 | 0.086* | |
C6 | 0.7264 (2) | 0.8814 (3) | 0.7984 (3) | 0.0495 (12) | |
C7 | 0.7730 (2) | 0.8811 (3) | 0.7422 (3) | 0.0495 (12) | |
C8 | 0.8195 (3) | 0.9428 (3) | 0.7435 (4) | 0.0711 (17) | |
H8 | 0.8203 | 0.9863 | 0.7784 | 0.085* | |
C9 | 0.8642 (3) | 0.9402 (4) | 0.6938 (5) | 0.083 (2) | |
H9 | 0.8956 | 0.9814 | 0.6963 | 0.099* | |
C10 | 0.8633 (3) | 0.8781 (3) | 0.6406 (4) | 0.0692 (16) | |
H10 | 0.8940 | 0.8769 | 0.6074 | 0.083* | |
C11 | 0.8165 (2) | 0.8170 (3) | 0.6364 (3) | 0.0546 (13) | |
H11 | 0.8153 | 0.7745 | 0.6001 | 0.066* | |
C12 | 0.7720 (2) | 0.8196 (3) | 0.6860 (3) | 0.0421 (11) | |
C13 | 0.8865 (2) | 0.7291 (3) | 0.8501 (3) | 0.0404 (11) | |
C14 | 0.8455 (2) | 0.7713 (3) | 0.9012 (3) | 0.0466 (12) | |
H14A | 0.8562 | 0.7498 | 0.9572 | 0.056* | |
H14B | 0.8556 | 0.8279 | 0.9043 | 0.056* | |
C15 | 0.9900 (2) | 0.7912 (3) | 0.9347 (3) | 0.0534 (13) | |
C16 | 1.0082 (3) | 0.7587 (4) | 1.0134 (4) | 0.0774 (18) | |
H16 | 0.9959 | 0.7067 | 1.0226 | 0.093* | |
C17 | 1.0449 (4) | 0.8047 (6) | 1.0778 (5) | 0.112 (3) | |
H17 | 1.0572 | 0.7841 | 1.1314 | 0.135* | |
C18 | 1.0633 (4) | 0.8798 (6) | 1.0638 (6) | 0.114 (3) | |
H18 | 1.0885 | 0.9100 | 1.1081 | 0.137* | |
C19 | 1.0456 (3) | 0.9123 (4) | 0.9861 (6) | 0.093 (2) | |
H19 | 1.0586 | 0.9641 | 0.9774 | 0.112* | |
C20 | 1.0086 (3) | 0.8675 (3) | 0.9206 (4) | 0.0669 (15) | |
H20 | 0.9962 | 0.8887 | 0.8672 | 0.080* | |
C21 | 0.9901 (3) | 0.7119 (4) | 0.8036 (5) | 0.093 (2) | |
H21A | 0.9609 | 0.7192 | 0.7478 | 0.111* | |
H21B | 1.0317 | 0.7427 | 0.8083 | 0.111* | |
C22 | 1.0076 (4) | 0.6313 (4) | 0.8152 (5) | 0.115 (3) | |
H22A | 1.0355 | 0.6233 | 0.8709 | 0.173* | |
H22B | 1.0329 | 0.6155 | 0.7763 | 0.173* | |
H22C | 0.9665 | 0.5999 | 0.8065 | 0.173* | |
C23 | 0.6152 (2) | 0.7319 (3) | 0.6994 (3) | 0.0406 (11) | |
C24 | 0.6557 (2) | 0.7696 (3) | 0.6443 (3) | 0.0429 (11) | |
H24A | 0.6426 | 0.7462 | 0.5892 | 0.052* | |
H24B | 0.6469 | 0.8265 | 0.6394 | 0.052* | |
C25 | 0.5145 (2) | 0.7904 (3) | 0.6082 (4) | 0.0600 (15) | |
C26 | 0.4971 (3) | 0.7523 (4) | 0.5331 (4) | 0.0774 (18) | |
H26 | 0.5078 | 0.6988 | 0.5295 | 0.093* | |
C27 | 0.4633 (3) | 0.7942 (5) | 0.4619 (5) | 0.097 (2) | |
H27 | 0.4509 | 0.7688 | 0.4105 | 0.117* | |
C28 | 0.4486 (3) | 0.8726 (6) | 0.4686 (5) | 0.102 (3) | |
H28 | 0.4264 | 0.9009 | 0.4212 | 0.122* | |
C29 | 0.4658 (3) | 0.9104 (4) | 0.5432 (5) | 0.096 (2) | |
H29 | 0.4549 | 0.9639 | 0.5466 | 0.115* | |
C30 | 0.4995 (3) | 0.8692 (4) | 0.6143 (4) | 0.0760 (17) | |
H30 | 0.5118 | 0.8950 | 0.6655 | 0.091* | |
C31 | 0.5076 (3) | 0.7199 (4) | 0.7423 (4) | 0.0829 (19) | |
H31A | 0.5353 | 0.7265 | 0.7991 | 0.100* | |
H31B | 0.4666 | 0.7525 | 0.7351 | 0.100* | |
C32 | 0.4882 (4) | 0.6369 (5) | 0.7274 (5) | 0.113 (3) | |
H32A | 0.4636 | 0.6299 | 0.6702 | 0.169* | |
H32B | 0.4592 | 0.6215 | 0.7624 | 0.169* | |
H32C | 0.5288 | 0.6043 | 0.7398 | 0.169* | |
C33 | 0.7823 (2) | 0.4308 (3) | 0.7624 (3) | 0.0403 (11) | |
C34 | 0.7199 (2) | 0.3955 (3) | 0.7704 (3) | 0.0435 (11) | |
C35 | 0.7077 (3) | 0.3137 (3) | 0.7636 (3) | 0.0553 (13) | |
H35 | 0.6665 | 0.2925 | 0.7694 | 0.066* | |
C36 | 0.7573 (3) | 0.2654 (3) | 0.7482 (3) | 0.0585 (15) | |
C37 | 0.8195 (3) | 0.2949 (3) | 0.7425 (3) | 0.0569 (14) | |
H37 | 0.8536 | 0.2605 | 0.7351 | 0.068* | |
C38 | 0.8307 (2) | 0.3745 (3) | 0.7477 (3) | 0.0446 (11) | |
C39 | 0.6896 (2) | 0.5324 (3) | 0.5928 (3) | 0.0420 (11) | |
C40 | 0.7487 (2) | 0.5201 (3) | 0.5628 (3) | 0.0422 (11) | |
C41 | 0.7559 (3) | 0.4577 (3) | 0.5115 (3) | 0.0529 (13) | |
H41 | 0.7957 | 0.4524 | 0.4936 | 0.063* | |
C42 | 0.7036 (3) | 0.4038 (3) | 0.4877 (3) | 0.0548 (14) | |
C43 | 0.6442 (3) | 0.4111 (3) | 0.5133 (3) | 0.0537 (13) | |
H43 | 0.6092 | 0.3736 | 0.4974 | 0.064* | |
C44 | 0.6373 (2) | 0.4742 (3) | 0.5623 (3) | 0.0463 (12) | |
C45 | 0.7854 (3) | 0.5374 (3) | 0.9522 (3) | 0.0495 (13) | |
C46 | 0.8420 (3) | 0.4827 (3) | 0.9640 (3) | 0.0503 (13) | |
C47 | 0.8420 (3) | 0.4077 (3) | 0.9951 (3) | 0.0576 (14) | |
H47 | 0.8786 | 0.3733 | 0.9974 | 0.069* | |
C48 | 0.7870 (3) | 0.3842 (3) | 1.0228 (3) | 0.0586 (14) | |
C49 | 0.7337 (3) | 0.4356 (3) | 1.0239 (3) | 0.0597 (14) | |
H49 | 0.6985 | 0.4200 | 1.0472 | 0.072* | |
C50 | 0.7336 (3) | 0.5102 (3) | 0.9904 (3) | 0.0539 (13) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Gd | 0.03632 (13) | 0.02908 (11) | 0.04381 (13) | 0.00121 (11) | 0.00754 (9) | −0.00233 (11) |
N1 | 0.037 (2) | 0.055 (3) | 0.070 (3) | −0.009 (2) | 0.021 (2) | −0.017 (2) |
N2 | 0.037 (2) | 0.070 (3) | 0.076 (3) | 0.010 (2) | 0.017 (2) | 0.027 (2) |
N3 | 0.060 (3) | 0.051 (3) | 0.061 (3) | −0.011 (2) | 0.024 (2) | 0.003 (2) |
N4 | 0.141 (5) | 0.024 (2) | 0.083 (4) | −0.008 (3) | 0.034 (4) | 0.005 (2) |
N5 | 0.058 (3) | 0.053 (3) | 0.068 (3) | 0.014 (2) | 0.025 (2) | −0.007 (2) |
N6 | 0.055 (3) | 0.052 (3) | 0.049 (3) | 0.006 (2) | 0.010 (2) | 0.010 (2) |
N7 | 0.082 (4) | 0.082 (4) | 0.067 (4) | 0.012 (3) | 0.006 (3) | −0.030 (3) |
N8 | 0.056 (3) | 0.078 (4) | 0.059 (3) | −0.008 (3) | 0.013 (2) | −0.019 (3) |
N9 | 0.068 (3) | 0.074 (3) | 0.053 (3) | 0.006 (3) | 0.013 (2) | 0.007 (3) |
N10 | 0.110 (5) | 0.067 (4) | 0.062 (3) | −0.006 (4) | 0.021 (3) | 0.016 (3) |
N11 | 0.075 (4) | 0.057 (3) | 0.085 (4) | −0.009 (3) | 0.028 (3) | −0.014 (3) |
O1 | 0.0425 (19) | 0.0457 (18) | 0.055 (2) | −0.0046 (15) | 0.0132 (15) | −0.0132 (16) |
O2 | 0.0371 (18) | 0.0340 (16) | 0.053 (2) | 0.0047 (13) | 0.0076 (14) | −0.0029 (14) |
O3 | 0.0390 (18) | 0.0380 (17) | 0.047 (2) | 0.0055 (14) | 0.0124 (15) | 0.0019 (15) |
O4 | 0.0328 (17) | 0.0326 (16) | 0.053 (2) | 0.0002 (13) | 0.0082 (14) | 0.0022 (14) |
O5 | 0.0463 (19) | 0.0267 (16) | 0.067 (2) | 0.0026 (14) | 0.0214 (16) | −0.0031 (15) |
O6 | 0.057 (2) | 0.0381 (19) | 0.093 (3) | 0.0003 (17) | 0.032 (2) | 0.0017 (18) |
O7 | 0.090 (3) | 0.070 (3) | 0.186 (5) | −0.021 (2) | 0.087 (3) | −0.001 (3) |
O8 | 0.148 (5) | 0.054 (3) | 0.123 (4) | −0.038 (3) | 0.044 (4) | −0.008 (2) |
O9 | 0.167 (5) | 0.037 (2) | 0.123 (4) | 0.029 (3) | 0.043 (3) | −0.003 (2) |
O10 | 0.062 (3) | 0.086 (3) | 0.103 (3) | 0.030 (2) | 0.022 (2) | 0.005 (3) |
O11 | 0.075 (3) | 0.064 (3) | 0.109 (3) | 0.010 (2) | 0.052 (2) | 0.017 (2) |
O12 | 0.056 (2) | 0.0490 (19) | 0.048 (2) | 0.0068 (16) | 0.0069 (16) | −0.0169 (16) |
O13 | 0.061 (2) | 0.048 (2) | 0.060 (2) | −0.0081 (18) | 0.0088 (17) | −0.0074 (19) |
O14 | 0.077 (3) | 0.084 (3) | 0.070 (3) | −0.011 (2) | 0.032 (2) | 0.004 (2) |
O15 | 0.089 (4) | 0.146 (5) | 0.108 (4) | 0.025 (3) | 0.018 (3) | −0.072 (3) |
O16 | 0.111 (4) | 0.080 (3) | 0.091 (3) | −0.011 (3) | 0.013 (3) | −0.047 (3) |
O17 | 0.102 (4) | 0.116 (4) | 0.132 (5) | −0.034 (3) | 0.064 (3) | −0.001 (3) |
O18 | 0.058 (3) | 0.103 (4) | 0.114 (4) | 0.010 (3) | 0.019 (2) | −0.039 (3) |
O19 | 0.076 (2) | 0.0409 (19) | 0.048 (2) | 0.0006 (17) | 0.0120 (17) | 0.0030 (16) |
O20 | 0.084 (3) | 0.082 (3) | 0.100 (4) | −0.020 (3) | 0.025 (2) | 0.006 (3) |
O21 | 0.077 (3) | 0.104 (3) | 0.092 (3) | 0.019 (3) | 0.033 (3) | 0.006 (3) |
O22 | 0.130 (4) | 0.076 (3) | 0.121 (4) | 0.031 (3) | 0.034 (3) | 0.041 (3) |
O23 | 0.128 (4) | 0.072 (3) | 0.082 (3) | −0.026 (3) | 0.027 (3) | 0.015 (2) |
O24 | 0.093 (3) | 0.084 (3) | 0.124 (4) | −0.014 (3) | 0.059 (3) | −0.024 (3) |
O25 | 0.138 (5) | 0.114 (4) | 0.176 (6) | 0.071 (4) | 0.081 (4) | 0.067 (4) |
C1 | 0.038 (3) | 0.033 (3) | 0.056 (3) | 0.003 (2) | 0.005 (2) | −0.016 (2) |
C2 | 0.052 (3) | 0.060 (3) | 0.060 (4) | 0.000 (3) | 0.016 (3) | −0.021 (3) |
C3 | 0.056 (4) | 0.082 (4) | 0.077 (4) | 0.004 (3) | 0.018 (3) | −0.035 (4) |
C4 | 0.064 (4) | 0.077 (4) | 0.094 (5) | 0.027 (3) | 0.007 (4) | −0.038 (4) |
C5 | 0.075 (4) | 0.045 (3) | 0.085 (5) | 0.016 (3) | 0.005 (4) | −0.008 (3) |
C6 | 0.048 (3) | 0.029 (3) | 0.066 (3) | 0.005 (2) | 0.005 (3) | −0.007 (2) |
C7 | 0.050 (3) | 0.031 (3) | 0.062 (3) | −0.002 (2) | 0.005 (3) | 0.006 (2) |
C8 | 0.086 (5) | 0.036 (3) | 0.086 (5) | −0.016 (3) | 0.013 (4) | 0.006 (3) |
C9 | 0.076 (5) | 0.059 (4) | 0.106 (6) | −0.034 (3) | 0.010 (4) | 0.024 (4) |
C10 | 0.056 (3) | 0.067 (4) | 0.087 (5) | −0.011 (3) | 0.023 (3) | 0.027 (4) |
C11 | 0.053 (3) | 0.054 (3) | 0.058 (4) | −0.001 (3) | 0.015 (3) | 0.013 (3) |
C12 | 0.035 (3) | 0.035 (3) | 0.053 (3) | −0.002 (2) | 0.005 (2) | 0.010 (2) |
C13 | 0.039 (3) | 0.035 (2) | 0.048 (3) | −0.003 (2) | 0.014 (2) | −0.002 (2) |
C14 | 0.039 (3) | 0.049 (3) | 0.050 (3) | 0.000 (2) | 0.007 (2) | −0.011 (2) |
C15 | 0.034 (3) | 0.058 (3) | 0.066 (4) | −0.009 (2) | 0.011 (2) | −0.013 (3) |
C16 | 0.064 (4) | 0.081 (4) | 0.080 (5) | −0.008 (3) | 0.007 (3) | 0.000 (4) |
C17 | 0.094 (6) | 0.153 (8) | 0.070 (5) | −0.008 (6) | −0.012 (4) | −0.007 (5) |
C18 | 0.081 (5) | 0.134 (8) | 0.113 (7) | −0.037 (5) | 0.001 (5) | −0.053 (6) |
C19 | 0.069 (5) | 0.077 (5) | 0.137 (7) | −0.028 (4) | 0.030 (5) | −0.030 (5) |
C20 | 0.048 (3) | 0.067 (4) | 0.088 (4) | −0.012 (3) | 0.023 (3) | −0.009 (3) |
C21 | 0.057 (4) | 0.085 (5) | 0.147 (7) | −0.010 (4) | 0.044 (4) | −0.019 (5) |
C22 | 0.084 (5) | 0.109 (6) | 0.154 (8) | 0.010 (5) | 0.033 (5) | −0.011 (6) |
C23 | 0.038 (3) | 0.034 (2) | 0.049 (3) | 0.000 (2) | 0.012 (2) | −0.005 (2) |
C24 | 0.033 (3) | 0.046 (3) | 0.048 (3) | 0.005 (2) | 0.009 (2) | 0.003 (2) |
C25 | 0.034 (3) | 0.068 (4) | 0.078 (4) | 0.008 (3) | 0.015 (3) | 0.019 (3) |
C26 | 0.057 (4) | 0.084 (4) | 0.087 (5) | −0.003 (3) | 0.010 (3) | 0.012 (4) |
C27 | 0.070 (5) | 0.128 (7) | 0.088 (6) | 0.001 (5) | 0.010 (4) | 0.004 (5) |
C28 | 0.068 (4) | 0.144 (8) | 0.094 (6) | 0.027 (5) | 0.020 (4) | 0.052 (6) |
C29 | 0.074 (5) | 0.095 (5) | 0.123 (7) | 0.034 (4) | 0.031 (5) | 0.046 (5) |
C30 | 0.054 (3) | 0.082 (4) | 0.094 (5) | 0.021 (3) | 0.021 (3) | 0.021 (4) |
C31 | 0.054 (4) | 0.094 (5) | 0.101 (5) | 0.006 (3) | 0.020 (3) | 0.028 (4) |
C32 | 0.092 (5) | 0.128 (7) | 0.120 (7) | −0.025 (5) | 0.033 (5) | −0.014 (5) |
C33 | 0.049 (3) | 0.034 (3) | 0.036 (3) | 0.003 (2) | 0.008 (2) | 0.003 (2) |
C34 | 0.051 (3) | 0.040 (3) | 0.042 (3) | 0.000 (2) | 0.016 (2) | 0.000 (2) |
C35 | 0.073 (4) | 0.047 (3) | 0.048 (3) | −0.007 (3) | 0.021 (3) | 0.005 (2) |
C36 | 0.093 (4) | 0.029 (2) | 0.054 (4) | 0.000 (3) | 0.021 (3) | 0.001 (2) |
C37 | 0.075 (4) | 0.044 (3) | 0.051 (3) | 0.016 (3) | 0.016 (3) | −0.002 (2) |
C38 | 0.056 (3) | 0.032 (2) | 0.047 (3) | 0.005 (2) | 0.015 (2) | 0.000 (2) |
C39 | 0.051 (3) | 0.038 (3) | 0.034 (3) | 0.005 (2) | 0.005 (2) | 0.001 (2) |
C40 | 0.048 (3) | 0.037 (3) | 0.036 (3) | 0.000 (2) | 0.002 (2) | 0.001 (2) |
C41 | 0.055 (3) | 0.059 (3) | 0.043 (3) | 0.010 (3) | 0.009 (2) | 0.000 (3) |
C42 | 0.067 (4) | 0.054 (3) | 0.040 (3) | 0.007 (3) | 0.008 (3) | −0.016 (2) |
C43 | 0.067 (4) | 0.042 (3) | 0.048 (3) | −0.009 (3) | 0.008 (3) | −0.006 (2) |
C44 | 0.053 (3) | 0.045 (3) | 0.040 (3) | 0.002 (2) | 0.011 (2) | −0.002 (2) |
C45 | 0.061 (3) | 0.045 (3) | 0.038 (3) | −0.002 (3) | 0.005 (2) | −0.003 (2) |
C46 | 0.056 (3) | 0.050 (3) | 0.045 (3) | −0.001 (3) | 0.012 (2) | 0.005 (2) |
C47 | 0.069 (4) | 0.055 (3) | 0.047 (3) | 0.010 (3) | 0.011 (3) | 0.010 (3) |
C48 | 0.075 (4) | 0.049 (3) | 0.049 (3) | 0.003 (3) | 0.011 (3) | 0.015 (3) |
C49 | 0.063 (4) | 0.064 (4) | 0.052 (3) | −0.008 (3) | 0.016 (3) | 0.004 (3) |
C50 | 0.060 (3) | 0.048 (3) | 0.052 (3) | 0.000 (3) | 0.010 (3) | −0.003 (3) |
Gd—O5 | 2.274 (3) | C10—C11 | 1.380 (7) |
Gd—O1 | 2.296 (3) | C10—H10 | 0.9300 |
Gd—O19 | 2.311 (3) | C11—C12 | 1.369 (7) |
Gd—O3 | 2.325 (3) | C11—H11 | 0.9300 |
Gd—O12 | 2.326 (3) | C13—C14 | 1.508 (6) |
Gd—O4 | 2.542 (3) | C14—H14A | 0.9700 |
Gd—O6 | 2.562 (3) | C14—H14B | 0.9700 |
Gd—O2 | 2.605 (3) | C15—C20 | 1.370 (7) |
Gd—O13 | 2.703 (4) | C15—C16 | 1.378 (7) |
N1—C13 | 1.318 (5) | C16—C17 | 1.371 (9) |
N1—C15 | 1.440 (6) | C16—H16 | 0.9300 |
N1—C21 | 1.517 (7) | C17—C18 | 1.350 (10) |
N2—C23 | 1.321 (5) | C17—H17 | 0.9300 |
N2—C25 | 1.436 (6) | C18—C19 | 1.363 (10) |
N2—C31 | 1.527 (7) | C18—H18 | 0.9300 |
N3—O7 | 1.209 (5) | C19—C20 | 1.373 (8) |
N3—O6 | 1.223 (5) | C19—H19 | 0.9300 |
N3—C34 | 1.445 (6) | C20—H20 | 0.9300 |
N4—O8 | 1.221 (6) | C21—C22 | 1.397 (8) |
N4—O9 | 1.228 (7) | C21—H21A | 0.9700 |
N4—C36 | 1.468 (6) | C21—H21B | 0.9700 |
N5—O11 | 1.203 (5) | C22—H22A | 0.9600 |
N5—O10 | 1.225 (5) | C22—H22B | 0.9600 |
N5—C38 | 1.469 (6) | C22—H22C | 0.9600 |
N6—O14 | 1.221 (5) | C23—C24 | 1.515 (6) |
N6—O13 | 1.236 (5) | C24—H24A | 0.9700 |
N6—C40 | 1.454 (6) | C24—H24B | 0.9700 |
N7—O15 | 1.210 (6) | C25—C26 | 1.365 (8) |
N7—O16 | 1.224 (6) | C25—C30 | 1.367 (7) |
N7—C42 | 1.458 (6) | C26—C27 | 1.394 (9) |
N8—O17 | 1.208 (6) | C26—H26 | 0.9300 |
N8—O18 | 1.216 (6) | C27—C28 | 1.360 (10) |
N8—C44 | 1.453 (6) | C27—H27 | 0.9300 |
N9—O20 | 1.218 (6) | C28—C29 | 1.357 (10) |
N9—O21 | 1.219 (6) | C28—H28 | 0.9300 |
N9—C46 | 1.460 (7) | C29—C30 | 1.386 (8) |
N10—O22 | 1.221 (6) | C29—H29 | 0.9300 |
N10—O23 | 1.230 (6) | C30—H30 | 0.9300 |
N10—C48 | 1.462 (7) | C31—C32 | 1.451 (8) |
N11—O25 | 1.186 (6) | C31—H31A | 0.9700 |
N11—O24 | 1.223 (6) | C31—H31B | 0.9700 |
N11—C50 | 1.466 (7) | C32—H32A | 0.9600 |
O1—C13 | 1.234 (5) | C32—H32B | 0.9600 |
O2—C1 | 1.402 (5) | C32—H32C | 0.9600 |
O2—C14 | 1.436 (5) | C33—C38 | 1.424 (6) |
O3—C23 | 1.243 (5) | C33—C34 | 1.426 (6) |
O4—C12 | 1.405 (5) | C34—C35 | 1.393 (6) |
O4—C24 | 1.437 (5) | C35—C36 | 1.360 (7) |
O5—C33 | 1.275 (5) | C35—H35 | 0.9300 |
O12—C39 | 1.262 (5) | C36—C37 | 1.372 (7) |
O19—C45 | 1.266 (5) | C37—C38 | 1.354 (6) |
C1—C2 | 1.368 (7) | C37—H37 | 0.9300 |
C1—C6 | 1.391 (7) | C39—C40 | 1.420 (6) |
C2—C3 | 1.385 (7) | C39—C44 | 1.429 (6) |
C2—H2 | 0.9300 | C40—C41 | 1.382 (6) |
C3—C4 | 1.371 (8) | C41—C42 | 1.365 (7) |
C3—H3 | 0.9300 | C41—H41 | 0.9300 |
C4—C5 | 1.379 (8) | C42—C43 | 1.375 (7) |
C4—H4 | 0.9300 | C43—C44 | 1.367 (6) |
C5—C6 | 1.400 (7) | C43—H43 | 0.9300 |
C5—H5 | 0.9300 | C45—C50 | 1.429 (7) |
C6—C7 | 1.487 (7) | C45—C46 | 1.436 (7) |
C7—C12 | 1.390 (6) | C46—C47 | 1.361 (6) |
C7—C8 | 1.392 (7) | C47—C48 | 1.363 (7) |
C8—C9 | 1.373 (8) | C47—H47 | 0.9300 |
C8—H8 | 0.9300 | C48—C49 | 1.380 (7) |
C9—C10 | 1.364 (8) | C49—C50 | 1.369 (7) |
C9—H9 | 0.9300 | C49—H49 | 0.9300 |
O5—Gd—O1 | 89.48 (10) | C13—C14—H14B | 110.6 |
O5—Gd—O19 | 79.26 (11) | H14A—C14—H14B | 108.7 |
O1—Gd—O19 | 84.06 (12) | C20—C15—C16 | 121.0 (5) |
O5—Gd—O3 | 140.85 (10) | C20—C15—N1 | 119.2 (5) |
O1—Gd—O3 | 129.59 (10) | C16—C15—N1 | 119.7 (5) |
O19—Gd—O3 | 99.89 (11) | C17—C16—C15 | 118.4 (6) |
O5—Gd—O12 | 82.99 (11) | C17—C16—H16 | 120.8 |
O1—Gd—O12 | 125.18 (12) | C15—C16—H16 | 120.8 |
O19—Gd—O12 | 145.59 (12) | C18—C17—C16 | 120.5 (8) |
O3—Gd—O12 | 76.19 (11) | C18—C17—H17 | 119.8 |
O5—Gd—O4 | 140.48 (10) | C16—C17—H17 | 119.8 |
O1—Gd—O4 | 77.57 (10) | C17—C18—C19 | 121.4 (7) |
O19—Gd—O4 | 134.73 (10) | C17—C18—H18 | 119.3 |
O3—Gd—O4 | 64.17 (10) | C19—C18—H18 | 119.3 |
O12—Gd—O4 | 74.99 (10) | C18—C19—C20 | 119.2 (7) |
O5—Gd—O6 | 66.55 (11) | C18—C19—H19 | 120.4 |
O1—Gd—O6 | 150.32 (11) | C20—C19—H19 | 120.4 |
O19—Gd—O6 | 74.79 (12) | C15—C20—C19 | 119.5 (6) |
O3—Gd—O6 | 75.41 (10) | C15—C20—H20 | 120.3 |
O12—Gd—O6 | 71.14 (12) | C19—C20—H20 | 120.3 |
O4—Gd—O6 | 132.07 (10) | C22—C21—N1 | 113.4 (6) |
O5—Gd—O2 | 137.64 (10) | C22—C21—H21A | 108.9 |
O1—Gd—O2 | 62.18 (10) | N1—C21—H21A | 108.9 |
O19—Gd—O2 | 67.72 (10) | C22—C21—H21B | 108.9 |
O3—Gd—O2 | 72.98 (9) | N1—C21—H21B | 108.9 |
O12—Gd—O2 | 138.64 (10) | H21A—C21—H21B | 107.7 |
O4—Gd—O2 | 67.09 (9) | C21—C22—H22A | 109.5 |
O6—Gd—O2 | 124.83 (10) | C21—C22—H22B | 109.5 |
O5—Gd—O13 | 71.81 (11) | H22A—C22—H22B | 109.5 |
O1—Gd—O13 | 63.09 (10) | C21—C22—H22C | 109.5 |
O19—Gd—O13 | 135.55 (11) | H22A—C22—H22C | 109.5 |
O3—Gd—O13 | 123.85 (10) | H22B—C22—H22C | 109.5 |
O12—Gd—O13 | 62.99 (11) | O3—C23—N2 | 121.7 (4) |
O4—Gd—O13 | 69.02 (10) | O3—C23—C24 | 120.8 (4) |
O6—Gd—O13 | 120.36 (10) | N2—C23—C24 | 117.4 (4) |
O2—Gd—O13 | 114.77 (10) | O4—C24—C23 | 106.9 (3) |
C13—N1—C15 | 123.1 (4) | O4—C24—H24A | 110.3 |
C13—N1—C21 | 117.1 (4) | C23—C24—H24A | 110.3 |
C15—N1—C21 | 119.7 (4) | O4—C24—H24B | 110.3 |
C23—N2—C25 | 121.2 (4) | C23—C24—H24B | 110.3 |
C23—N2—C31 | 119.1 (4) | H24A—C24—H24B | 108.6 |
C25—N2—C31 | 119.7 (4) | C26—C25—C30 | 120.8 (6) |
O7—N3—O6 | 120.9 (5) | C26—C25—N2 | 119.9 (5) |
O7—N3—C34 | 118.6 (4) | C30—C25—N2 | 119.3 (6) |
O6—N3—C34 | 120.5 (4) | C25—C26—C27 | 119.7 (7) |
O8—N4—O9 | 124.7 (5) | C25—C26—H26 | 120.1 |
O8—N4—C36 | 117.8 (6) | C27—C26—H26 | 120.1 |
O9—N4—C36 | 117.5 (6) | C28—C27—C26 | 119.1 (7) |
O11—N5—O10 | 123.9 (5) | C28—C27—H27 | 120.5 |
O11—N5—C38 | 119.4 (4) | C26—C27—H27 | 120.5 |
O10—N5—C38 | 116.7 (5) | C29—C28—C27 | 121.2 (7) |
O14—N6—O13 | 122.4 (5) | C29—C28—H28 | 119.4 |
O14—N6—C40 | 117.8 (5) | C27—C28—H28 | 119.4 |
O13—N6—C40 | 119.8 (4) | C28—C29—C30 | 120.1 (7) |
O15—N7—O16 | 124.3 (5) | C28—C29—H29 | 120.0 |
O15—N7—C42 | 117.8 (5) | C30—C29—H29 | 120.0 |
O16—N7—C42 | 117.9 (6) | C25—C30—C29 | 119.2 (7) |
O17—N8—O18 | 124.4 (6) | C25—C30—H30 | 120.4 |
O17—N8—C44 | 118.1 (5) | C29—C30—H30 | 120.4 |
O18—N8—C44 | 117.5 (5) | C32—C31—N2 | 110.0 (6) |
O20—N9—O21 | 124.6 (6) | C32—C31—H31A | 109.7 |
O20—N9—C46 | 118.1 (5) | N2—C31—H31A | 109.7 |
O21—N9—C46 | 117.3 (5) | C32—C31—H31B | 109.7 |
O22—N10—O23 | 124.4 (6) | N2—C31—H31B | 109.7 |
O22—N10—C48 | 118.6 (6) | H31A—C31—H31B | 108.2 |
O23—N10—C48 | 117.0 (6) | C31—C32—H32A | 109.5 |
O25—N11—O24 | 123.0 (6) | C31—C32—H32B | 109.5 |
O25—N11—C50 | 120.3 (6) | H32A—C32—H32B | 109.5 |
O24—N11—C50 | 116.7 (5) | C31—C32—H32C | 109.5 |
C13—O1—Gd | 128.6 (3) | H32A—C32—H32C | 109.5 |
C1—O2—C14 | 117.0 (3) | H32B—C32—H32C | 109.5 |
C1—O2—Gd | 126.1 (2) | O5—C33—C38 | 121.3 (4) |
C14—O2—Gd | 115.5 (2) | O5—C33—C34 | 125.1 (4) |
C23—O3—Gd | 122.6 (3) | C38—C33—C34 | 113.5 (4) |
C12—O4—C24 | 116.1 (3) | C35—C34—C33 | 122.9 (4) |
C12—O4—Gd | 127.5 (2) | C35—C34—N3 | 115.7 (4) |
C24—O4—Gd | 114.1 (2) | C33—C34—N3 | 121.4 (4) |
C33—O5—Gd | 143.8 (3) | C36—C35—C34 | 118.6 (5) |
N3—O6—Gd | 140.6 (3) | C36—C35—H35 | 120.7 |
C39—O12—Gd | 131.5 (3) | C34—C35—H35 | 120.7 |
N6—O13—Gd | 133.7 (3) | C35—C36—C37 | 121.7 (5) |
C45—O19—Gd | 132.8 (3) | C35—C36—N4 | 119.6 (6) |
C2—C1—C6 | 122.7 (4) | C37—C36—N4 | 118.7 (5) |
C2—C1—O2 | 118.4 (4) | C38—C37—C36 | 119.5 (5) |
C6—C1—O2 | 118.7 (4) | C38—C37—H37 | 120.2 |
C1—C2—C3 | 119.1 (6) | C36—C37—H37 | 120.2 |
C1—C2—H2 | 120.5 | C37—C38—C33 | 123.7 (5) |
C3—C2—H2 | 120.5 | C37—C38—N5 | 118.0 (4) |
C4—C3—C2 | 119.8 (6) | C33—C38—N5 | 118.3 (4) |
C4—C3—H3 | 120.1 | O12—C39—C40 | 125.4 (4) |
C2—C3—H3 | 120.1 | O12—C39—C44 | 122.1 (4) |
C3—C4—C5 | 120.8 (6) | C40—C39—C44 | 112.5 (4) |
C3—C4—H4 | 119.6 | C41—C40—C39 | 124.0 (4) |
C5—C4—H4 | 119.6 | C41—C40—N6 | 116.5 (5) |
C4—C5—C6 | 120.6 (6) | C39—C40—N6 | 119.5 (4) |
C4—C5—H5 | 119.7 | C42—C41—C40 | 119.1 (5) |
C6—C5—H5 | 119.7 | C42—C41—H41 | 120.5 |
C1—C6—C5 | 116.9 (5) | C40—C41—H41 | 120.5 |
C1—C6—C7 | 121.5 (4) | C41—C42—C43 | 121.1 (5) |
C5—C6—C7 | 121.6 (5) | C41—C42—N7 | 119.3 (5) |
C12—C7—C8 | 117.1 (5) | C43—C42—N7 | 119.5 (5) |
C12—C7—C6 | 121.6 (4) | C44—C43—C42 | 119.1 (5) |
C8—C7—C6 | 121.3 (5) | C44—C43—H43 | 120.5 |
C9—C8—C7 | 120.7 (6) | C42—C43—H43 | 120.5 |
C9—C8—H8 | 119.7 | C43—C44—C39 | 124.1 (5) |
C7—C8—H8 | 119.7 | C43—C44—N8 | 117.3 (5) |
C10—C9—C8 | 121.0 (5) | C39—C44—N8 | 118.6 (4) |
C10—C9—H9 | 119.5 | O19—C45—C50 | 124.7 (5) |
C8—C9—H9 | 119.5 | O19—C45—C46 | 123.1 (5) |
C9—C10—C11 | 119.7 (6) | C50—C45—C46 | 112.2 (4) |
C9—C10—H10 | 120.2 | C47—C46—C45 | 124.4 (5) |
C11—C10—H10 | 120.2 | C47—C46—N9 | 117.2 (5) |
C12—C11—C10 | 119.4 (5) | C45—C46—N9 | 118.4 (4) |
C12—C11—H11 | 120.3 | C46—C47—C48 | 118.5 (5) |
C10—C11—H11 | 120.3 | C46—C47—H47 | 120.8 |
C11—C12—C7 | 122.1 (4) | C48—C47—H47 | 120.8 |
C11—C12—O4 | 117.9 (4) | C47—C48—C49 | 121.6 (5) |
C7—C12—O4 | 119.8 (4) | C47—C48—N10 | 118.7 (5) |
O1—C13—N1 | 121.4 (4) | C49—C48—N10 | 119.6 (6) |
O1—C13—C14 | 119.9 (4) | C50—C49—C48 | 119.0 (5) |
N1—C13—C14 | 118.7 (4) | C50—C49—H49 | 120.5 |
O2—C14—C13 | 105.9 (3) | C48—C49—H49 | 120.5 |
O2—C14—H14A | 110.6 | C49—C50—C45 | 123.3 (5) |
C13—C14—H14A | 110.6 | C49—C50—N11 | 117.0 (5) |
O2—C14—H14B | 110.6 | C45—C50—N11 | 119.6 (5) |
Experimental details
Crystal data | |
Chemical formula | [Gd(C6H2N3O7)3(C32H32N2O4)] |
Mr | 1350.16 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 298 |
a, b, c (Å) | 20.125 (2), 16.7778 (18), 16.6491 (18) |
β (°) | 105.051 (2) |
V (Å3) | 5428.9 (10) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.32 |
Crystal size (mm) | 0.40 × 0.37 × 0.29 |
Data collection | |
Diffractometer | Bruker SMART CCD area detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.620, 0.701 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 28190, 9559, 6585 |
Rint | 0.036 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.036, 0.087, 1.08 |
No. of reflections | 9559 |
No. of parameters | 786 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.50, −0.58 |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 2001), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2001), SHELXTL.
Gd—O1 | 2.296 (3) | Gd—O4 | 2.542 (3) |
Gd—O3 | 2.325 (3) | Gd—O2 | 2.605 (3) |
O1—Gd—O4 | 77.57 (10) | O3—Gd—O2 | 72.98 (9) |
O3—Gd—O4 | 64.17 (10) | O4—Gd—O2 | 67.09 (9) |
O1—Gd—O2 | 62.18 (10) |
Metal-directed self-assembly of organic ligands and metal ions, or organometallic moieties, to form well defined structures has been a very attractive field in recent years (Lehn, 1995; Steed & Atwood, 2000; Bourne et al., 2001;), for their fascinating structural diversities and potential application in functional materials, nanotechnology and biological recognition (Evan & Lin, 2002; Janiak, 2003; Carlucci et al., 2003; Gutschke et al., 1996;). We have now investigated the assembly of the ligand N-phenyl-2-{2'-[(phenyl- ethyl-carbamoyl)-methoxy]-biphenyl-2-yloxy}-N-ethyl-acetamide with gadolinium picrate.
In the title complex I, The Gd(III) ion is coordinated by 9 oxygen donor atoms, five of them belonging to two bidentate and one monodentate picrate groups whereas the remaining four are from the tetradentate ligand L(Fig. 1). The coordination polyhedron around Gd(III) ion is a distorted tricapped trigonal prism (Fig. 2) (Wang et al., 2003). The quadridentate ligand wraps around the metal ion with its oxygen atoms and forms a ring-like coordination structure together with the Gd atom. The two phenyl rings about the central bond in the molecule have a drastic twisting, with the dihedral angle between them being 61.18°. The mean distances between the Gd atom and the coordinated ether and carbonyl oxygen atoms are 2.575 Å and 2.3105 Å, respectively. This suggests that the Gd—O (C?O) bond is stronger than the Gd—O (C—O—C) bond.