Literature DB >> 23284362

4-(Dimethyl-amino)-pyridinium octa-aqua-erbium(III) tetra-chloride monohydrate.

Meriem Benslimane1, Hocine Merazig, Jean-Claude Daran, Ouahida Zeghouan.   

Abstract

In the title compound, (C(7)H(11)N(2))[Er(H(2)O)(8)]Cl(4)·H(2)O, the asymmetric unit consists of one 4-(dimethyl-amino)-pyridinium and one octa-aqua-erbium cation balanced by four Cl(-) anions, and one water mol-ecule. The 4-(dimethyl-amino)-pyridinium cation is protonated at the pyridine N atom. The dimethyl-amino 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(H(2)O)(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-(dimethyl-amino)-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.

Entities:  

Year:  2012        PMID： 23284362      PMCID： PMC3515135          DOI： 10.1107/S1600536812043048

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


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

(C7H11N2)[Er(H2O)8]Cl4·H2O M = 594.38 Triclinic, a = 7.8775 (3) Å b = 9.3601 (4) Å c = 15.2593 (6) Å α = 105.831 (3)° β = 101.498 (3)° γ = 90.919 (3)° V = 1057.77 (8) Å3 Z = 2 Mo Kα radiation μ = 4.51 mm−1 T = 180 K 0.35 × 0.17 × 0.09 mm

Data collection

Agilent Xcalibur Sapphire1 diffractometer Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2011 ▶) T min = 0.415, T max = 0.666 21843 measured reflections 4315 independent reflections 4110 reflections with I > 2σ(I) R int = 0.031

Refinement

R[F 2 > 2σ(F 2)] = 0.015 wR(F 2) = 0.038 S = 1.12 4315 reflections 210 parameters H-atom parameters constrained Δρmax = 0.38 e Å−3 Δρmin = −0.84 e Å−3 Data collection: CrysAlis PRO (Agilent, 2011 ▶); cell refinement: 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. Click here for additional data file. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812043048/su2511sup1.cif Click here for additional data file. Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812043048/su2511Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
(C7H11N2)[Er(H2O)8]Cl4·H2OZ = 2
Mr = 594.38F(000) = 586
Triclinic, P1Dx = 1.866 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.8775 (3) ÅCell parameters from 17643 reflections
b = 9.3601 (4) Åθ = 2.8–28.5°
c = 15.2593 (6) ŵ = 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 diffractometer4315 independent reflections
Radiation source: fine-focus sealed tube4110 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
Detector resolution: 8.2632 pixels mm-1θmax = 26.4°, θmin = 2.8°
ω scanh = −9→9
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2011)k = −11→11
Tmin = 0.415, Tmax = 0.666l = −19→19
21843 measured reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.015Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.038H-atom parameters constrained
S = 1.12w = 1/[σ2(Fo2) + (0.0184P)2 + 0.1863P] where P = (Fo2 + 2Fc2)/3
4315 reflections(Δ/σ)max = 0.013
210 parametersΔρmax = 0.38 e Å−3
0 restraintsΔρmin = −0.84 e Å−3
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.
xyzUiso*/Ueq
Er10.784214 (11)0.328931 (10)0.139815 (6)0.01301 (4)
O10.6913 (2)0.08907 (17)0.13083 (13)0.0290 (4)
H110.74090.01120.10940.043*
H120.59210.06450.13820.043*
O20.49910 (19)0.33181 (16)0.16570 (11)0.0196 (3)
H210.43520.25300.15510.029*
H220.43820.40560.17160.029*
O30.8148 (2)0.37949 (19)0.29989 (11)0.0246 (4)
H310.73910.42450.32750.037*
H320.90630.37470.33820.037*
O40.71203 (19)0.58031 (16)0.18827 (11)0.0202 (3)
H410.74420.63800.15930.030*
H420.61190.60100.19830.030*
O50.9675 (2)0.48121 (18)0.09471 (12)0.0231 (4)
H510.93160.55250.07280.035*
H521.07240.50450.12380.035*
O60.8996 (2)0.16376 (17)0.02461 (11)0.0222 (3)
H610.98470.19310.00550.033*
H620.82780.1097−0.02220.033*
O71.0635 (2)0.27890 (19)0.20245 (12)0.0275 (4)
H711.10900.31330.25970.041*
H721.11580.20530.17700.041*
O80.6080 (2)0.33727 (19)0.00199 (11)0.0253 (4)
H810.49870.3160−0.01030.038*
H820.63980.3342−0.04860.038*
N10.5425 (3)−0.0329 (2)0.34543 (14)0.0269 (5)
H10.4717−0.06510.29230.032*
N20.8825 (3)0.1213 (2)0.59717 (14)0.0255 (4)
C10.7717 (3)0.0707 (3)0.51542 (16)0.0205 (5)
C20.7091 (3)−0.0813 (3)0.47840 (17)0.0228 (5)
H20.7453−0.14900.51170.027*
C30.5969 (3)−0.1280 (3)0.39497 (17)0.0250 (5)
H30.5568−0.22790.37150.030*
C40.5976 (3)0.1126 (3)0.37797 (18)0.0290 (6)
H40.55760.17690.34280.035*
C50.7091 (3)0.1666 (3)0.46032 (18)0.0264 (5)
H50.74560.26740.48140.032*
C60.9502 (4)0.2769 (3)0.6311 (2)0.0363 (6)
H6A0.98890.30590.58220.054*
H6B1.04590.28910.68320.054*
H6C0.86020.33830.65040.054*
C70.9373 (3)0.0284 (3)0.65895 (18)0.0331 (6)
H7A0.8482−0.04930.64840.050*
H7B0.95710.08830.72260.050*
H7C1.0427−0.01500.64650.050*
Cl10.32218 (7)0.03390 (6)0.16034 (4)0.01959 (11)
Cl20.33046 (7)0.63783 (6)0.19098 (4)0.02174 (12)
Cl40.78967 (7)0.76450 (6)0.05870 (4)0.02396 (12)
Cl31.20318 (8)0.38429 (7)0.41119 (4)0.03275 (15)
O1W0.5751 (2)0.5134 (2)0.38849 (12)0.0326 (4)
H1W0.47010.48920.38660.049*
H2W0.63350.53100.44390.049*
U11U22U33U12U13U23
Er10.01068 (5)0.01438 (6)0.01302 (6)0.00048 (4)0.00106 (4)0.00335 (4)
O10.0269 (9)0.0144 (8)0.0502 (12)0.0028 (7)0.0212 (8)0.0073 (8)
O20.0153 (8)0.0132 (7)0.0304 (9)0.0007 (6)0.0061 (7)0.0052 (7)
O30.0201 (8)0.0383 (10)0.0147 (8)0.0082 (7)0.0020 (7)0.0075 (7)
O40.0182 (8)0.0181 (8)0.0250 (9)0.0000 (6)0.0059 (7)0.0062 (7)
O50.0150 (8)0.0236 (9)0.0343 (10)0.0008 (6)0.0043 (7)0.0149 (8)
O60.0164 (8)0.0263 (9)0.0194 (8)−0.0032 (6)0.0059 (6)−0.0024 (7)
O70.0196 (9)0.0364 (10)0.0200 (9)0.0126 (7)−0.0023 (7)0.0014 (7)
O80.0152 (8)0.0432 (11)0.0168 (8)0.0004 (7)0.0002 (6)0.0097 (8)
N10.0245 (11)0.0337 (12)0.0179 (10)−0.0012 (9)−0.0032 (8)0.0052 (9)
N20.0265 (11)0.0243 (11)0.0207 (11)−0.0009 (8)−0.0026 (9)0.0036 (9)
C10.0179 (11)0.0228 (12)0.0202 (12)0.0011 (9)0.0055 (9)0.0042 (10)
C20.0237 (12)0.0214 (12)0.0229 (12)0.0016 (9)0.0032 (10)0.0069 (10)
C30.0264 (13)0.0210 (12)0.0250 (13)−0.0021 (10)0.0045 (10)0.0031 (10)
C40.0290 (14)0.0299 (14)0.0295 (14)0.0029 (11)0.0021 (11)0.0136 (11)
C50.0301 (13)0.0207 (12)0.0285 (13)−0.0004 (10)0.0032 (11)0.0091 (10)
C60.0373 (15)0.0268 (14)0.0338 (15)−0.0051 (11)−0.0026 (12)−0.0021 (12)
C70.0323 (14)0.0390 (16)0.0246 (14)0.0000 (12)−0.0044 (11)0.0108 (12)
Cl10.0179 (3)0.0183 (3)0.0215 (3)−0.0010 (2)0.0016 (2)0.0057 (2)
Cl20.0182 (3)0.0212 (3)0.0242 (3)0.0015 (2)0.0031 (2)0.0048 (2)
Cl40.0187 (3)0.0194 (3)0.0383 (3)0.0041 (2)0.0103 (2)0.0123 (2)
Cl30.0335 (3)0.0336 (3)0.0244 (3)−0.0001 (3)−0.0101 (3)0.0088 (3)
O1W0.0283 (10)0.0454 (11)0.0188 (9)0.0036 (8)0.0020 (7)0.0022 (8)
Er1—O82.2989 (15)O8—H820.8517
Er1—O12.3097 (16)N1—C31.341 (3)
Er1—O32.3195 (16)N1—C41.347 (3)
Er1—O72.3263 (15)N1—H10.8600
Er1—O52.3356 (15)N2—C11.331 (3)
Er1—O62.3465 (15)N2—C61.458 (3)
Er1—O22.3561 (15)N2—C71.459 (3)
Er1—O42.3807 (15)C1—C21.419 (3)
O1—H110.8493C1—C51.420 (3)
O1—H120.8484C2—C31.352 (3)
O2—H210.8455C2—H20.9300
O2—H220.8425C3—H30.9300
O3—H310.8495C4—C51.344 (4)
O3—H320.8439C4—H40.9300
O4—H410.8497C5—H50.9300
O4—H420.8485C6—H6A0.9600
O5—H510.8522C6—H6B0.9600
O5—H520.8499C6—H6C0.9600
O6—H610.8514C7—H7A0.9600
O6—H620.8480C7—H7B0.9600
O7—H710.8439C7—H7C0.9600
O7—H720.8498O1W—H1W0.8471
O8—H810.8520O1W—H2W0.8491
O8—Er1—O195.94 (6)Er1—O6—H61120.3
O8—Er1—O3146.14 (6)Er1—O6—H62117.0
O1—Er1—O386.60 (6)H61—O6—H62108.2
O8—Er1—O7142.03 (6)Er1—O7—H71122.0
O1—Er1—O788.39 (6)Er1—O7—H72124.1
O3—Er1—O771.64 (6)H71—O7—H72111.0
O8—Er1—O581.09 (6)Er1—O8—H81122.4
O1—Er1—O5146.98 (6)Er1—O8—H82126.5
O3—Er1—O5114.04 (6)H81—O8—H82108.6
O7—Er1—O575.30 (6)C3—N1—C4120.7 (2)
O8—Er1—O675.79 (6)C3—N1—H1119.7
O1—Er1—O671.78 (6)C4—N1—H1119.7
O3—Er1—O6135.91 (6)C1—N2—C6120.7 (2)
O7—Er1—O669.84 (6)C1—N2—C7122.8 (2)
O5—Er1—O675.65 (6)C6—N2—C7116.4 (2)
O8—Er1—O274.29 (6)N2—C1—C2122.3 (2)
O1—Er1—O271.93 (5)N2—C1—C5121.6 (2)
O3—Er1—O274.51 (6)C2—C1—C5116.2 (2)
O7—Er1—O2141.61 (6)C3—C2—C1120.3 (2)
O5—Er1—O2136.56 (5)C3—C2—H2119.9
O6—Er1—O2129.45 (5)C1—C2—H2119.9
O8—Er1—O481.90 (6)N1—C3—C2121.2 (2)
O1—Er1—O4141.90 (6)N1—C3—H3119.4
O3—Er1—O475.79 (6)C2—C3—H3119.4
O7—Er1—O4116.47 (6)C5—C4—N1121.3 (2)
O5—Er1—O470.61 (5)C5—C4—H4119.3
O6—Er1—O4141.89 (6)N1—C4—H4119.3
O2—Er1—O470.91 (5)C4—C5—C1120.4 (2)
Er1—O1—H11125.4C4—C5—H5119.8
Er1—O1—H12124.1C1—C5—H5119.8
H11—O1—H12109.5N2—C6—H6A109.5
Er1—O2—H21122.4N2—C6—H6B109.5
Er1—O2—H22125.8H6A—C6—H6B109.5
H21—O2—H22109.7N2—C6—H6C109.5
Er1—O3—H31121.3H6A—C6—H6C109.5
Er1—O3—H32126.0H6B—C6—H6C109.5
H31—O3—H32111.3N2—C7—H7A109.5
Er1—O4—H41115.9N2—C7—H7B109.5
Er1—O4—H42121.1H7A—C7—H7B109.5
H41—O4—H42108.9N2—C7—H7C109.5
Er1—O5—H51122.7H7A—C7—H7C109.5
Er1—O5—H52121.2H7B—C7—H7C109.5
H51—O5—H52108.1H1W—O1W—H2W109.7
D—H···AD—HH···AD···AD—H···A
N1—H1···Cl10.862.533.229 (2)139
O1W—H1W···Cl3i0.852.443.2686 (18)165
O1W—H2W···Cl3ii0.852.253.0874 (18)171
O1—H11···Cl4iii0.852.293.1036 (18)160
O1—H12···Cl10.852.243.0863 (17)172
O2—H21···Cl10.852.253.0708 (17)164
O2—H22···Cl20.842.313.1372 (17)167
O3—H31···O1W0.851.822.671 (2)177
O3—H32···Cl30.842.373.1826 (17)162
O4—H41···Cl40.852.253.0925 (17)169
O4—H42···Cl20.852.233.0685 (16)168
O5—H51···Cl40.852.333.1469 (18)160
O5—H52···Cl2iv0.852.273.0819 (18)161
O6—H61···Cl4v0.852.273.1164 (17)171
O6—H62···Cl1vi0.852.253.0858 (17)169
O7—H71···Cl30.842.193.0304 (18)173
O7—H72···Cl1iv0.852.303.1132 (18)159
O8—H81···Cl4vii0.852.293.1377 (17)173
O8—H82···Cl2vii0.852.313.1464 (17)166
C2—H2···Cl3viii0.932.773.683 (3)169
C3—H3···O1Wiii0.932.513.332 (3)148
C6—H6B···O4ii0.962.473.379 (3)158
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
N1—H1⋯Cl10.862.533.229 (2)139
O1W—H1W⋯Cl3i 0.852.443.2686 (18)165
O1W—H2W⋯Cl3ii 0.852.253.0874 (18)171
O1—H11⋯Cl4iii 0.852.293.1036 (18)160
O1—H12⋯Cl10.852.243.0863 (17)172
O2—H21⋯Cl10.852.253.0708 (17)164
O2—H22⋯Cl20.842.313.1372 (17)167
O3—H31⋯O1W 0.851.822.671 (2)177
O3—H32⋯Cl30.842.373.1826 (17)162
O4—H41⋯Cl40.852.253.0925 (17)169
O4—H42⋯Cl20.852.233.0685 (16)168
O5—H51⋯Cl40.852.333.1469 (18)160
O5—H52⋯Cl2iv 0.852.273.0819 (18)161
O6—H61⋯Cl4v 0.852.273.1164 (17)171
O6—H62⋯Cl1vi 0.852.253.0858 (17)169
O7—H71⋯Cl30.842.193.0304 (18)173
O7—H72⋯Cl1iv 0.852.303.1132 (18)159
O8—H81⋯Cl4vii 0.852.293.1377 (17)173
O8—H82⋯Cl2vii 0.852.313.1464 (17)166
C2—H2⋯Cl3viii 0.932.773.683 (3)169
C3—H3⋯O1W iii 0.932.513.332 (3)148
C6—H6B⋯O4ii 0.962.473.379 (3)158

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) .

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1.  The Cambridge Structural Database: a quarter of a million crystal structures and rising.

Authors:  Frank H Allen
Journal:  Acta Crystallogr B       Date:  2002-05-29

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

3.  Tris[4-(dimethyl-amino)-pyridinium][(bis-μ-dichlorido)-deca-aqua-dichlorido-dineodymium(III)] penta-chloride dihydrate.

Authors:  Meriem Benslimane; Hocine Merazig; Jean-Claude Daran; Ouahida Zeghouan
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2012-10-10

4.  Bis[4-(dimethyl-amino)-pyridinium] octa-aqua-chloridolanthanum(III) tetra-chloride trihydrate.

Authors:  Meriem Benslimane; Hocine Merazig; Jean-Claude Daran; Ouahida Zeghouan
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2012-10-03
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