metal-organic compounds
4-(Dimethylamino)pyridinium octaaquaerbium(III) tetrachloride monohydrate
aUnité de Recherche de Chimie de l'Environnement et Moléculaire Structurale, Faculté des Sciences Exactes, Département de Chimie, Université Mentouri de Constantine, 25000 Constantine, Algeria, and bLaboratoire de Chimie de Coordination, UPR-CNRS 8241, 205 route de Narbonne, 31077 Toulouse Cedex 4, France
*Correspondence e-mail: b_meriem80@yahoo.fr
In the title compound, (C7H11N2)[Er(H2O)8]Cl4·H2O, the consists of one 4-(dimethylamino)pyridinium and one octaaquaerbium cation balanced by four Cl− anions, and one water molecule. The 4-(dimethylamino)pyridinium cation is protonated at the pyridine N atom. The dimethylamino group (C/N/C) lies close to the plane of the pyridinium ring, making a dihedral angle of 4.5 (3)°. In the crystal, the [Er(H2O)8]3+ cations are linked via O—H⋯O and O—H⋯Cl hydrogen bonds, forming two-dimensional networks propagating in the ab plane. These networks are linked via O—H⋯O and O—H⋯Cl hydrogen bonds, forming a three-dimensional network. The 4-(dimethylamino)pyridinium cations are located in the cavities and are linked to the framework via N—H⋯Cl, C—H⋯O and C—H⋯Cl hydrogen bonds.
Related literature
For similar structures in this series involving 4-(dimethylamino)pyridinium, see: Benslimane et al. (2012a,b). For details of the Cambridge Structural Database, see: Allen (2002). For hydrogen-bond motifs see: Bernstein et al. (1995).
Experimental
Crystal data
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Refinement
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Data collection: CrysAlis PRO (Agilent, 2011); cell CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 2012); software used to prepare material for publication: SHELXL97.
Supporting information
10.1107/S1600536812043048/su2511sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536812043048/su2511Isup2.hkl
4-(Dimethylamino)pyridine (1 mmol, 0.051g) and hydrochloric acid (1M) was added slowly to a solution of ErCl3.6H2O (1mmol, 0.08g). The mixture was refluxed at 353 K for about 1 h and then cooled to room temperature. Slow evaporation of the solvent at room temperature lead to the formation of pink plate-like crystals of the title compound.
The H-atoms of the coordinated water molecules were located in difference Fourier syntheses and were initially refined using distance restraints: O-H = 0.85 (2) Å, and H···H= 1.40 (2) Å, with Uiso(H) = 1.5Ueq(O). In the last cycles of
they were constrained to ride on their parent O atoms. The N-bound H atom was located in a difference Fourier map but like the C-bound H atoms it was included in calculated positions and treated as riding: N-H=0.86 Å, C-H = 0.93 (aromatic), 0.96 (methyl), with Uiso(H) = 1.5Ueq(C) for the methyl groups and 1.2Ueq(N,C) for the other H atoms.Data collection: CrysAlis PRO (Agilent, 2011); cell
CrysAlis PRO (Agilent, 2011); data reduction: CrysAlis PRO (Agilent, 2011); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 2012); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).Fig. 1. The molecular structure of the title compound, showing the atom-numbering. Displacement ellipsoids are drawn at the 50% probability level. The O-H···Cl and N-H···Cl hydrogen bonds are shown as double dashed lines. | |
Fig. 2. A view of part of the crystal structure of the title compound lying parallel to (100), showing the formation of rings via O-H···Cl and N-H···Cl hydrogen-bonds. Hydrogen bonds are drawn as dashed lines [symmetry codes: (i) x-1, y, z; (ii) -x+2, -y+1, -z+1; (iii) x+1, y, z]. |
(C7H11N2)[Er(H2O)8]Cl4·H2O | Z = 2 |
Mr = 594.38 | F(000) = 586 |
Triclinic, P1 | Dx = 1.866 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.8775 (3) Å | Cell parameters from 17643 reflections |
b = 9.3601 (4) Å | θ = 2.8–28.5° |
c = 15.2593 (6) Å | µ = 4.51 mm−1 |
α = 105.831 (3)° | T = 180 K |
β = 101.498 (3)° | Plate, pink |
γ = 90.919 (3)° | 0.35 × 0.17 × 0.09 mm |
V = 1057.77 (8) Å3 |
Agilent Xcalibur Sapphire1 diffractometer | 4315 independent reflections |
Radiation source: fine-focus sealed tube | 4110 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
Detector resolution: 8.2632 pixels mm-1 | θmax = 26.4°, θmin = 2.8° |
ω scan | h = −9→9 |
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2011) | k = −11→11 |
Tmin = 0.415, Tmax = 0.666 | l = −19→19 |
21843 measured reflections |
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)] = 0.015 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.038 | H-atom parameters constrained |
S = 1.12 | w = 1/[σ2(Fo2) + (0.0184P)2 + 0.1863P] where P = (Fo2 + 2Fc2)/3 |
4315 reflections | (Δ/σ)max = 0.013 |
210 parameters | Δρmax = 0.38 e Å−3 |
0 restraints | Δρmin = −0.84 e Å−3 |
(C7H11N2)[Er(H2O)8]Cl4·H2O | γ = 90.919 (3)° |
Mr = 594.38 | V = 1057.77 (8) Å3 |
Triclinic, P1 | Z = 2 |
a = 7.8775 (3) Å | Mo Kα radiation |
b = 9.3601 (4) Å | µ = 4.51 mm−1 |
c = 15.2593 (6) Å | T = 180 K |
α = 105.831 (3)° | 0.35 × 0.17 × 0.09 mm |
β = 101.498 (3)° |
Agilent Xcalibur Sapphire1 diffractometer | 4315 independent reflections |
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2011) | 4110 reflections with I > 2σ(I) |
Tmin = 0.415, Tmax = 0.666 | Rint = 0.031 |
21843 measured reflections |
R[F2 > 2σ(F2)] = 0.015 | 0 restraints |
wR(F2) = 0.038 | H-atom parameters constrained |
S = 1.12 | Δρmax = 0.38 e Å−3 |
4315 reflections | Δρmin = −0.84 e Å−3 |
210 parameters |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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 | ||
Er1 | 0.784214 (11) | 0.328931 (10) | 0.139815 (6) | 0.01301 (4) | |
O1 | 0.6913 (2) | 0.08907 (17) | 0.13083 (13) | 0.0290 (4) | |
H11 | 0.7409 | 0.0112 | 0.1094 | 0.043* | |
H12 | 0.5921 | 0.0645 | 0.1382 | 0.043* | |
O2 | 0.49910 (19) | 0.33181 (16) | 0.16570 (11) | 0.0196 (3) | |
H21 | 0.4352 | 0.2530 | 0.1551 | 0.029* | |
H22 | 0.4382 | 0.4056 | 0.1716 | 0.029* | |
O3 | 0.8148 (2) | 0.37949 (19) | 0.29989 (11) | 0.0246 (4) | |
H31 | 0.7391 | 0.4245 | 0.3275 | 0.037* | |
H32 | 0.9063 | 0.3747 | 0.3382 | 0.037* | |
O4 | 0.71203 (19) | 0.58031 (16) | 0.18827 (11) | 0.0202 (3) | |
H41 | 0.7442 | 0.6380 | 0.1593 | 0.030* | |
H42 | 0.6119 | 0.6010 | 0.1983 | 0.030* | |
O5 | 0.9675 (2) | 0.48121 (18) | 0.09471 (12) | 0.0231 (4) | |
H51 | 0.9316 | 0.5525 | 0.0728 | 0.035* | |
H52 | 1.0724 | 0.5045 | 0.1238 | 0.035* | |
O6 | 0.8996 (2) | 0.16376 (17) | 0.02461 (11) | 0.0222 (3) | |
H61 | 0.9847 | 0.1931 | 0.0055 | 0.033* | |
H62 | 0.8278 | 0.1097 | −0.0222 | 0.033* | |
O7 | 1.0635 (2) | 0.27890 (19) | 0.20245 (12) | 0.0275 (4) | |
H71 | 1.1090 | 0.3133 | 0.2597 | 0.041* | |
H72 | 1.1158 | 0.2053 | 0.1770 | 0.041* | |
O8 | 0.6080 (2) | 0.33727 (19) | 0.00199 (11) | 0.0253 (4) | |
H81 | 0.4987 | 0.3160 | −0.0103 | 0.038* | |
H82 | 0.6398 | 0.3342 | −0.0486 | 0.038* | |
N1 | 0.5425 (3) | −0.0329 (2) | 0.34543 (14) | 0.0269 (5) | |
H1 | 0.4717 | −0.0651 | 0.2923 | 0.032* | |
N2 | 0.8825 (3) | 0.1213 (2) | 0.59717 (14) | 0.0255 (4) | |
C1 | 0.7717 (3) | 0.0707 (3) | 0.51542 (16) | 0.0205 (5) | |
C2 | 0.7091 (3) | −0.0813 (3) | 0.47840 (17) | 0.0228 (5) | |
H2 | 0.7453 | −0.1490 | 0.5117 | 0.027* | |
C3 | 0.5969 (3) | −0.1280 (3) | 0.39497 (17) | 0.0250 (5) | |
H3 | 0.5568 | −0.2279 | 0.3715 | 0.030* | |
C4 | 0.5976 (3) | 0.1126 (3) | 0.37797 (18) | 0.0290 (6) | |
H4 | 0.5576 | 0.1769 | 0.3428 | 0.035* | |
C5 | 0.7091 (3) | 0.1666 (3) | 0.46032 (18) | 0.0264 (5) | |
H5 | 0.7456 | 0.2674 | 0.4814 | 0.032* | |
C6 | 0.9502 (4) | 0.2769 (3) | 0.6311 (2) | 0.0363 (6) | |
H6A | 0.9889 | 0.3059 | 0.5822 | 0.054* | |
H6B | 1.0459 | 0.2891 | 0.6832 | 0.054* | |
H6C | 0.8602 | 0.3383 | 0.6504 | 0.054* | |
C7 | 0.9373 (3) | 0.0284 (3) | 0.65895 (18) | 0.0331 (6) | |
H7A | 0.8482 | −0.0493 | 0.6484 | 0.050* | |
H7B | 0.9571 | 0.0883 | 0.7226 | 0.050* | |
H7C | 1.0427 | −0.0150 | 0.6465 | 0.050* | |
Cl1 | 0.32218 (7) | 0.03390 (6) | 0.16034 (4) | 0.01959 (11) | |
Cl2 | 0.33046 (7) | 0.63783 (6) | 0.19098 (4) | 0.02174 (12) | |
Cl4 | 0.78967 (7) | 0.76450 (6) | 0.05870 (4) | 0.02396 (12) | |
Cl3 | 1.20318 (8) | 0.38429 (7) | 0.41119 (4) | 0.03275 (15) | |
O1W | 0.5751 (2) | 0.5134 (2) | 0.38849 (12) | 0.0326 (4) | |
H1W | 0.4701 | 0.4892 | 0.3866 | 0.049* | |
H2W | 0.6335 | 0.5310 | 0.4439 | 0.049* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Er1 | 0.01068 (5) | 0.01438 (6) | 0.01302 (6) | 0.00048 (4) | 0.00106 (4) | 0.00335 (4) |
O1 | 0.0269 (9) | 0.0144 (8) | 0.0502 (12) | 0.0028 (7) | 0.0212 (8) | 0.0073 (8) |
O2 | 0.0153 (8) | 0.0132 (7) | 0.0304 (9) | 0.0007 (6) | 0.0061 (7) | 0.0052 (7) |
O3 | 0.0201 (8) | 0.0383 (10) | 0.0147 (8) | 0.0082 (7) | 0.0020 (7) | 0.0075 (7) |
O4 | 0.0182 (8) | 0.0181 (8) | 0.0250 (9) | 0.0000 (6) | 0.0059 (7) | 0.0062 (7) |
O5 | 0.0150 (8) | 0.0236 (9) | 0.0343 (10) | 0.0008 (6) | 0.0043 (7) | 0.0149 (8) |
O6 | 0.0164 (8) | 0.0263 (9) | 0.0194 (8) | −0.0032 (6) | 0.0059 (6) | −0.0024 (7) |
O7 | 0.0196 (9) | 0.0364 (10) | 0.0200 (9) | 0.0126 (7) | −0.0023 (7) | 0.0014 (7) |
O8 | 0.0152 (8) | 0.0432 (11) | 0.0168 (8) | 0.0004 (7) | 0.0002 (6) | 0.0097 (8) |
N1 | 0.0245 (11) | 0.0337 (12) | 0.0179 (10) | −0.0012 (9) | −0.0032 (8) | 0.0052 (9) |
N2 | 0.0265 (11) | 0.0243 (11) | 0.0207 (11) | −0.0009 (8) | −0.0026 (9) | 0.0036 (9) |
C1 | 0.0179 (11) | 0.0228 (12) | 0.0202 (12) | 0.0011 (9) | 0.0055 (9) | 0.0042 (10) |
C2 | 0.0237 (12) | 0.0214 (12) | 0.0229 (12) | 0.0016 (9) | 0.0032 (10) | 0.0069 (10) |
C3 | 0.0264 (13) | 0.0210 (12) | 0.0250 (13) | −0.0021 (10) | 0.0045 (10) | 0.0031 (10) |
C4 | 0.0290 (14) | 0.0299 (14) | 0.0295 (14) | 0.0029 (11) | 0.0021 (11) | 0.0136 (11) |
C5 | 0.0301 (13) | 0.0207 (12) | 0.0285 (13) | −0.0004 (10) | 0.0032 (11) | 0.0091 (10) |
C6 | 0.0373 (15) | 0.0268 (14) | 0.0338 (15) | −0.0051 (11) | −0.0026 (12) | −0.0021 (12) |
C7 | 0.0323 (14) | 0.0390 (16) | 0.0246 (14) | 0.0000 (12) | −0.0044 (11) | 0.0108 (12) |
Cl1 | 0.0179 (3) | 0.0183 (3) | 0.0215 (3) | −0.0010 (2) | 0.0016 (2) | 0.0057 (2) |
Cl2 | 0.0182 (3) | 0.0212 (3) | 0.0242 (3) | 0.0015 (2) | 0.0031 (2) | 0.0048 (2) |
Cl4 | 0.0187 (3) | 0.0194 (3) | 0.0383 (3) | 0.0041 (2) | 0.0103 (2) | 0.0123 (2) |
Cl3 | 0.0335 (3) | 0.0336 (3) | 0.0244 (3) | −0.0001 (3) | −0.0101 (3) | 0.0088 (3) |
O1W | 0.0283 (10) | 0.0454 (11) | 0.0188 (9) | 0.0036 (8) | 0.0020 (7) | 0.0022 (8) |
Er1—O8 | 2.2989 (15) | O8—H82 | 0.8517 |
Er1—O1 | 2.3097 (16) | N1—C3 | 1.341 (3) |
Er1—O3 | 2.3195 (16) | N1—C4 | 1.347 (3) |
Er1—O7 | 2.3263 (15) | N1—H1 | 0.8600 |
Er1—O5 | 2.3356 (15) | N2—C1 | 1.331 (3) |
Er1—O6 | 2.3465 (15) | N2—C6 | 1.458 (3) |
Er1—O2 | 2.3561 (15) | N2—C7 | 1.459 (3) |
Er1—O4 | 2.3807 (15) | C1—C2 | 1.419 (3) |
O1—H11 | 0.8493 | C1—C5 | 1.420 (3) |
O1—H12 | 0.8484 | C2—C3 | 1.352 (3) |
O2—H21 | 0.8455 | C2—H2 | 0.9300 |
O2—H22 | 0.8425 | C3—H3 | 0.9300 |
O3—H31 | 0.8495 | C4—C5 | 1.344 (4) |
O3—H32 | 0.8439 | C4—H4 | 0.9300 |
O4—H41 | 0.8497 | C5—H5 | 0.9300 |
O4—H42 | 0.8485 | C6—H6A | 0.9600 |
O5—H51 | 0.8522 | C6—H6B | 0.9600 |
O5—H52 | 0.8499 | C6—H6C | 0.9600 |
O6—H61 | 0.8514 | C7—H7A | 0.9600 |
O6—H62 | 0.8480 | C7—H7B | 0.9600 |
O7—H71 | 0.8439 | C7—H7C | 0.9600 |
O7—H72 | 0.8498 | O1W—H1W | 0.8471 |
O8—H81 | 0.8520 | O1W—H2W | 0.8491 |
O8—Er1—O1 | 95.94 (6) | Er1—O6—H61 | 120.3 |
O8—Er1—O3 | 146.14 (6) | Er1—O6—H62 | 117.0 |
O1—Er1—O3 | 86.60 (6) | H61—O6—H62 | 108.2 |
O8—Er1—O7 | 142.03 (6) | Er1—O7—H71 | 122.0 |
O1—Er1—O7 | 88.39 (6) | Er1—O7—H72 | 124.1 |
O3—Er1—O7 | 71.64 (6) | H71—O7—H72 | 111.0 |
O8—Er1—O5 | 81.09 (6) | Er1—O8—H81 | 122.4 |
O1—Er1—O5 | 146.98 (6) | Er1—O8—H82 | 126.5 |
O3—Er1—O5 | 114.04 (6) | H81—O8—H82 | 108.6 |
O7—Er1—O5 | 75.30 (6) | C3—N1—C4 | 120.7 (2) |
O8—Er1—O6 | 75.79 (6) | C3—N1—H1 | 119.7 |
O1—Er1—O6 | 71.78 (6) | C4—N1—H1 | 119.7 |
O3—Er1—O6 | 135.91 (6) | C1—N2—C6 | 120.7 (2) |
O7—Er1—O6 | 69.84 (6) | C1—N2—C7 | 122.8 (2) |
O5—Er1—O6 | 75.65 (6) | C6—N2—C7 | 116.4 (2) |
O8—Er1—O2 | 74.29 (6) | N2—C1—C2 | 122.3 (2) |
O1—Er1—O2 | 71.93 (5) | N2—C1—C5 | 121.6 (2) |
O3—Er1—O2 | 74.51 (6) | C2—C1—C5 | 116.2 (2) |
O7—Er1—O2 | 141.61 (6) | C3—C2—C1 | 120.3 (2) |
O5—Er1—O2 | 136.56 (5) | C3—C2—H2 | 119.9 |
O6—Er1—O2 | 129.45 (5) | C1—C2—H2 | 119.9 |
O8—Er1—O4 | 81.90 (6) | N1—C3—C2 | 121.2 (2) |
O1—Er1—O4 | 141.90 (6) | N1—C3—H3 | 119.4 |
O3—Er1—O4 | 75.79 (6) | C2—C3—H3 | 119.4 |
O7—Er1—O4 | 116.47 (6) | C5—C4—N1 | 121.3 (2) |
O5—Er1—O4 | 70.61 (5) | C5—C4—H4 | 119.3 |
O6—Er1—O4 | 141.89 (6) | N1—C4—H4 | 119.3 |
O2—Er1—O4 | 70.91 (5) | C4—C5—C1 | 120.4 (2) |
Er1—O1—H11 | 125.4 | C4—C5—H5 | 119.8 |
Er1—O1—H12 | 124.1 | C1—C5—H5 | 119.8 |
H11—O1—H12 | 109.5 | N2—C6—H6A | 109.5 |
Er1—O2—H21 | 122.4 | N2—C6—H6B | 109.5 |
Er1—O2—H22 | 125.8 | H6A—C6—H6B | 109.5 |
H21—O2—H22 | 109.7 | N2—C6—H6C | 109.5 |
Er1—O3—H31 | 121.3 | H6A—C6—H6C | 109.5 |
Er1—O3—H32 | 126.0 | H6B—C6—H6C | 109.5 |
H31—O3—H32 | 111.3 | N2—C7—H7A | 109.5 |
Er1—O4—H41 | 115.9 | N2—C7—H7B | 109.5 |
Er1—O4—H42 | 121.1 | H7A—C7—H7B | 109.5 |
H41—O4—H42 | 108.9 | N2—C7—H7C | 109.5 |
Er1—O5—H51 | 122.7 | H7A—C7—H7C | 109.5 |
Er1—O5—H52 | 121.2 | H7B—C7—H7C | 109.5 |
H51—O5—H52 | 108.1 | H1W—O1W—H2W | 109.7 |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···Cl1 | 0.86 | 2.53 | 3.229 (2) | 139 |
O1W—H1W···Cl3i | 0.85 | 2.44 | 3.2686 (18) | 165 |
O1W—H2W···Cl3ii | 0.85 | 2.25 | 3.0874 (18) | 171 |
O1—H11···Cl4iii | 0.85 | 2.29 | 3.1036 (18) | 160 |
O1—H12···Cl1 | 0.85 | 2.24 | 3.0863 (17) | 172 |
O2—H21···Cl1 | 0.85 | 2.25 | 3.0708 (17) | 164 |
O2—H22···Cl2 | 0.84 | 2.31 | 3.1372 (17) | 167 |
O3—H31···O1W | 0.85 | 1.82 | 2.671 (2) | 177 |
O3—H32···Cl3 | 0.84 | 2.37 | 3.1826 (17) | 162 |
O4—H41···Cl4 | 0.85 | 2.25 | 3.0925 (17) | 169 |
O4—H42···Cl2 | 0.85 | 2.23 | 3.0685 (16) | 168 |
O5—H51···Cl4 | 0.85 | 2.33 | 3.1469 (18) | 160 |
O5—H52···Cl2iv | 0.85 | 2.27 | 3.0819 (18) | 161 |
O6—H61···Cl4v | 0.85 | 2.27 | 3.1164 (17) | 171 |
O6—H62···Cl1vi | 0.85 | 2.25 | 3.0858 (17) | 169 |
O7—H71···Cl3 | 0.84 | 2.19 | 3.0304 (18) | 173 |
O7—H72···Cl1iv | 0.85 | 2.30 | 3.1132 (18) | 159 |
O8—H81···Cl4vii | 0.85 | 2.29 | 3.1377 (17) | 173 |
O8—H82···Cl2vii | 0.85 | 2.31 | 3.1464 (17) | 166 |
C2—H2···Cl3viii | 0.93 | 2.77 | 3.683 (3) | 169 |
C3—H3···O1Wiii | 0.93 | 2.51 | 3.332 (3) | 148 |
C6—H6B···O4ii | 0.96 | 2.47 | 3.379 (3) | 158 |
Symmetry codes: (i) x−1, y, z; (ii) −x+2, −y+1, −z+1; (iii) x, y−1, z; (iv) x+1, y, z; (v) −x+2, −y+1, −z; (vi) −x+1, −y, −z; (vii) −x+1, −y+1, −z; (viii) −x+2, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | (C7H11N2)[Er(H2O)8]Cl4·H2O |
Mr | 594.38 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 180 |
a, b, c (Å) | 7.8775 (3), 9.3601 (4), 15.2593 (6) |
α, β, γ (°) | 105.831 (3), 101.498 (3), 90.919 (3) |
V (Å3) | 1057.77 (8) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 4.51 |
Crystal size (mm) | 0.35 × 0.17 × 0.09 |
Data collection | |
Diffractometer | Agilent Xcalibur Sapphire1 diffractometer |
Absorption correction | Multi-scan (CrysAlis PRO; Agilent, 2011) |
Tmin, Tmax | 0.415, 0.666 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 21843, 4315, 4110 |
Rint | 0.031 |
(sin θ/λ)max (Å−1) | 0.625 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.015, 0.038, 1.12 |
No. of reflections | 4315 |
No. of parameters | 210 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.38, −0.84 |
Computer programs: CrysAlis PRO (Agilent, 2011), SIR92 (Altomare et al., 1993), SHELXL97 (Sheldrick, 2008), ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 2012).
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···Cl1 | 0.86 | 2.53 | 3.229 (2) | 139 |
O1W—H1W···Cl3i | 0.85 | 2.44 | 3.2686 (18) | 165 |
O1W—H2W···Cl3ii | 0.85 | 2.25 | 3.0874 (18) | 171 |
O1—H11···Cl4iii | 0.85 | 2.29 | 3.1036 (18) | 160 |
O1—H12···Cl1 | 0.85 | 2.24 | 3.0863 (17) | 172 |
O2—H21···Cl1 | 0.85 | 2.25 | 3.0708 (17) | 164 |
O2—H22···Cl2 | 0.84 | 2.31 | 3.1372 (17) | 167 |
O3—H31···O1W | 0.85 | 1.82 | 2.671 (2) | 177 |
O3—H32···Cl3 | 0.84 | 2.37 | 3.1826 (17) | 162 |
O4—H41···Cl4 | 0.85 | 2.25 | 3.0925 (17) | 169 |
O4—H42···Cl2 | 0.85 | 2.23 | 3.0685 (16) | 168 |
O5—H51···Cl4 | 0.85 | 2.33 | 3.1469 (18) | 160 |
O5—H52···Cl2iv | 0.85 | 2.27 | 3.0819 (18) | 161 |
O6—H61···Cl4v | 0.85 | 2.27 | 3.1164 (17) | 171 |
O6—H62···Cl1vi | 0.85 | 2.25 | 3.0858 (17) | 169 |
O7—H71···Cl3 | 0.84 | 2.19 | 3.0304 (18) | 173 |
O7—H72···Cl1iv | 0.85 | 2.30 | 3.1132 (18) | 159 |
O8—H81···Cl4vii | 0.85 | 2.29 | 3.1377 (17) | 173 |
O8—H82···Cl2vii | 0.85 | 2.31 | 3.1464 (17) | 166 |
C2—H2···Cl3viii | 0.93 | 2.77 | 3.683 (3) | 169 |
C3—H3···O1Wiii | 0.93 | 2.51 | 3.332 (3) | 148 |
C6—H6B···O4ii | 0.96 | 2.47 | 3.379 (3) | 158 |
Symmetry codes: (i) x−1, y, z; (ii) −x+2, −y+1, −z+1; (iii) x, y−1, z; (iv) x+1, y, z; (v) −x+2, −y+1, −z; (vi) −x+1, −y, −z; (vii) −x+1, −y+1, −z; (viii) −x+2, −y, −z+1. |
Acknowledgements
Technical support (X-ray measurements) from Laboratory of Coordination Chemistry, UPR-CNRS 8241, Toulouse, are acknowledged.
References
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This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
The title compound is part of a series of lanthanide complexes with the organic cation 4-(dimethylamino)pyridinium, for example: (C7H10N2)2.LaCl(H2O)8.Cl4.3H2O (I) (Benslimane et al., 2012a) and (C7H10N2)3.[Nd2Cl4(H2O)10].Cl5.2H2O (II) (Benslimane et al., 2012b).
The title compound (III) contains an inorganic [Er(H2O)8]3+ and an organic (C7H10N2)+ cation equilibrated by four Cl anions, and one lattice water molecule (Fig. 1). Atom Er1 is coordinated by eight water molecules with Er-O bond distances ranging from 2.2989 (15) to 2.3807 (15) Å. The [Er(H2O)8]3+ cations are linked to the organic cations via Cl- anions through intermolecular O-H···Cl and N-H···Cl hydrogen bonds. Each Cl- anion acts as an acceptor of hydrogen bonds from the pyridinium groups and the water molecules. The water molecules, which act as bridging units between the cations, form cooperative infinite chains parallel to the (100) plane through O-H···Cl hydrogen bonds generating centrosymmetric R24(8) ring motives (Bernstein et al., 1995), as shown in Fig. 2 and Table 1.
In the three compounds, (I) - (III), there is a decrease in the bond lengths of the metal-O(water) bonds, from 2.5101 (15) - 2.5632 (15) Å in (I), 2.404 (3) - 2.479 (4) Å in (II) and 2.2989 (15) - 2.3807 (15) Å in (III). This trend corresponds to the decreasing metallic radius of the lanthanide ion involved; La3+, Nd3+ and Er3+, respectively. In addition, the 4-(dimethylamino)pyridinium cation in the three compounds is protonated at the pyridine N atom. The N-C bond linking the dimethylamino substituent to the pyridinium ring is short, 1.321 (3), 1.324 (3)Å for (I), 1.330 (5), 1.2855 (2) Å for (II) and 1.331 (3) Å for (III), suggesting some delocalization in the cation. A search of the Cambridge Structural Database (CSD, V5.33, Update 4, August 2012; Allen, 2002) reveals similar structures incorporating the 4-(dimethylamino)pyridinium cation for which the corresponding mean N-C distance is 1.34 (1) Å. The dimethylamino group lies close to the plane of the pyridinium ring, with dihedral angles of 3.5 (3) and 2.0 (3)° for (I), 1.6 (6)° and 6.5 (3)° for (II) and 4.5 (3)° for (III).
In conclusion, on the structural level the atomic arrangement in all three compounds, (I) - (III), consists of networks of alternating organic–inorganic layers. The chloride anions are located between these entities forming hydrogen bonds with the NH atoms of the 4-(dimethylamino)pyridinium cations and the water molecules. There are also C—H···Cl interactions present involving one of the 4-(dimethylamino)pyridinium cations. The result is the formation of three-dimensional supramolecular architectures.