Literature DB >> 21522528

Tetra-kis(μ-3-aza-niumylbenzoato)-κO:O,O';κO,O':O;κO:O'-bis-[triaqua-chloridolanthanum(III)] tetra-chloride dihydrate.

Meriem Benslimane, Hocine Merazig, Jean-Claude Daran.   

Abstract

The tiltle complex, [La(2)(C(7)H(7)NO(2))(4)Cl(2)(H(2)O)(6)]Cl(4)·2H(2)O, is a centrosymmetric dimer formed by edge-sharing LaO(5)(H(2)O)(3)Cl polyhedra linked together by a carboxyl-ate ligand. The two La(III) metal ions are linked by two bidentate bridging carboxyl-ate groups with a κ(2)O:O' coordination mode and two bidentate chelating bridging carboxyl-ate groups with a κ(3)O:O,O' coordination mode. The coordination sphere of lanthanum, completed by a terminal chloride and three water mol-ecules, adopts a distorted tricapped trigonal-prismatic arrangement. N-H⋯Cl, N-H⋯O and O-H(water)⋯Cl hydrogen bonds, and slipped π-π inter-actions between parallel benzene rings [centroid-centroid distance of 3.647 (3) Å] are observed in the structure. These combine to stabilize a three-dimensional network.

Entities:  

Year:  2010        PMID： 21522528      PMCID： PMC3050182          DOI： 10.1107/S1600536810052864

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


Related literature

For potential applications of lanthanide complexes, see: Aime et al. (1998 ▶); Bao et al. (2007 ▶); Drew et al. (2000 ▶); Ishikawa et al. (2005 ▶); Liu et al. (2004 ▶). For lanthanide complexes with organic ligands, see: Cao et al. (2002 ▶); Wang et al. (2000 ▶); Lam et al. (2003 ▶); De Sa et al. (1998 ▶); Serra et al. (1998 ▶); Bassett et al. (2004 ▶); Galaup et al. (1999 ▶); Blasse et al. (1987 ▶); Prodi et al. (1998 ▶); Ramirez et al. (2001 ▶); Thuery et al. (2000 ▶); Bunzli & Ihringer (2002 ▶); Jones et al. (1997 ▶); Bardwell et al. (1997 ▶); Horrocks et al. (1997 ▶). For similar complexes, see: Qin et al. (2005 ▶, 2006 ▶); Xiong & Qi (2007 ▶); Song et al. (2005 ▶); Anna & Kaziol (1999 ▶). For the use of the SQUEEZE function of PLATON, see: Spek (2009 ▶).

Experimental

Crystal data

[La2(C7H7NO2)4Cl2(H2O)6]Cl4·2H2O M = 1183.19 Monoclinic, a = 11.2988 (3) Å b = 19.8679 (4) Å c = 10.4679 (3) Å β = 112.693 (1)° V = 2167.96 (10) Å3 Z = 2 Mo Kα radiation μ = 2.38 mm−1 T = 293 K 0.24 × 0.22 × 0.18 mm

Data collection

Enraf–Nonius CAD-4 diffractometer Absorption correction: refined from ΔF (DIFABS; Walker & Stuart, 1983 ▶) T min = 0.550, T max = 0.789 6316 measured reflections 6315 independent reflections 4414 reflections with I > 2σ(I) R int = 0.027 2 standard reflections every 60 min intensity decay: 3%

Refinement

R[F 2 > 2σ(F 2)] = 0.044 wR(F 2) = 0.110 S = 1.00 6315 reflections 246 parameters H-atom parameters constrained Δρmax = 2.85 e Å−3 Δρmin = −0.87 e Å−3 Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994 ▶); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1996 ▶); program(s) used to solve structure: SIR92 (Altomare et al., 1993 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810052864/su2239sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810052864/su2239Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[La2(C7H7NO2)4Cl2(H2O)6]Cl4·2H2OF(000) = 1168
Mr = 1183.19Dx = 1.813 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 6316 reflections
a = 11.2988 (3) Åθ = 1.0–30.0°
b = 19.8679 (4) ŵ = 2.38 mm−1
c = 10.4679 (3) ÅT = 293 K
β = 112.693 (1)°Prism, brown
V = 2167.96 (10) Å30.24 × 0.22 × 0.18 mm
Z = 2
Enraf–Nonius CAD-4 diffractometerRint = 0.027
graphiteθmax = 30.0°, θmin = 2.0°
non–profiled ω/2τ scansh = −15→14
Absorption correction: part of the refinement model (ΔF) DIFABS (Walker & Stuart, 1983)k = 0→27
Tmin = 0.550, Tmax = 0.789l = 0→14
6316 measured reflections2 standard reflections every 60 min
6315 independent reflections intensity decay: 3%
4414 reflections with I > 2σ(I)
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.110H-atom parameters constrained
S = 1.00w = 1/[σ2(Fo2) + (0.060P)2] where P = (Fo2 + 2Fc2)/3
6315 reflections(Δ/σ)max = 0.001
246 parametersΔρmax = 2.85 e Å−3
0 restraintsΔρmin = −0.87 e Å−3
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.
xyzUiso*/Ueq
C10.3737 (5)0.6180 (2)0.3817 (5)0.0270 (9)
C20.3278 (4)0.6773 (2)0.2831 (5)0.0265 (9)
C30.4148 (5)0.7263 (2)0.2812 (5)0.0325 (10)
H30.49850.72520.34680.039*
C40.3781 (5)0.7766 (2)0.1827 (6)0.0385 (12)
H40.43760.80810.17910.046*
C50.2527 (5)0.7798 (3)0.0900 (6)0.0390 (12)
H50.22640.81400.02430.047*
C60.1667 (5)0.7324 (3)0.0949 (5)0.0347 (11)
C70.2016 (5)0.6809 (2)0.1899 (5)0.0304 (10)
H70.14170.64910.19140.036*
C80.5026 (5)0.5348 (2)0.7463 (5)0.0252 (9)
C90.4230 (4)0.5418 (2)0.8325 (4)0.0241 (9)
C100.4425 (5)0.5977 (2)0.9175 (5)0.0298 (10)
H100.50410.62950.92080.036*
C110.3714 (5)0.6062 (2)0.9963 (5)0.0364 (11)
H010.38140.64501.04910.044*
C120.2846 (5)0.5575 (2)0.9982 (5)0.0320 (10)
H020.23730.56281.05320.038*
C130.2694 (4)0.5011 (2)0.9176 (4)0.0251 (9)
C140.3360 (4)0.4921 (2)0.8324 (4)0.0256 (9)
H140.32310.45410.77670.031*
N10.0341 (5)0.7368 (3)−0.0085 (6)0.0559 (14)
H1A0.01430.7797−0.03140.084*
H1B−0.01950.71990.02710.084*
H1C0.02740.7135−0.08350.084*
N20.1833 (4)0.4481 (2)0.9262 (4)0.0328 (8)
H2A0.22890.41560.98200.049*
H2B0.14020.43120.84220.049*
H2C0.12820.46510.95970.049*
O10.4840 (3)0.62303 (16)0.4762 (3)0.0327 (7)
O20.4623 (3)0.49888 (16)0.6384 (3)0.0296 (7)
O1W0.7267 (4)0.67276 (18)0.6974 (4)0.0509 (11)
H110.74420.68310.77740.076*
H210.71080.70580.63920.076*
O30.3002 (3)0.56857 (16)0.3589 (4)0.0361 (8)
O2W0.8388 (4)0.5038 (2)0.4974 (4)0.0454 (9)
H120.88590.46820.52800.068*
H220.89070.53010.48210.068*
O40.6072 (3)0.56602 (17)0.7855 (3)0.0331 (8)
O3W0.7332 (4)0.63595 (18)0.4301 (4)0.0459 (10)
H130.70820.66670.46070.069*
H230.80870.62980.42130.069*
Cl10.92083 (12)0.54510 (8)0.82837 (14)0.0468 (3)
Cl20.24108 (15)0.29052 (6)0.99466 (15)0.0445 (3)
Cl3−0.02500 (13)0.88440 (7)−0.13178 (14)0.0400 (3)
La10.67532 (2)0.552876 (12)0.58587 (2)0.02160 (7)
U11U22U33U12U13U23
C10.036 (2)0.022 (2)0.030 (2)0.0100 (18)0.020 (2)0.0042 (17)
C20.036 (2)0.0151 (18)0.033 (2)0.0062 (17)0.018 (2)0.0008 (16)
C30.039 (3)0.026 (2)0.029 (2)−0.002 (2)0.010 (2)0.0035 (19)
C40.044 (3)0.028 (2)0.045 (3)−0.007 (2)0.019 (2)0.007 (2)
C50.053 (3)0.029 (2)0.039 (3)0.006 (2)0.022 (3)0.015 (2)
C60.034 (3)0.036 (3)0.034 (2)0.008 (2)0.013 (2)0.008 (2)
C70.036 (2)0.024 (2)0.038 (3)0.0043 (18)0.021 (2)0.0068 (19)
C80.037 (2)0.025 (2)0.0213 (19)0.0058 (17)0.0186 (18)0.0050 (16)
C90.027 (2)0.026 (2)0.0230 (19)−0.0010 (16)0.0134 (17)−0.0017 (16)
C100.036 (3)0.025 (2)0.032 (2)−0.0046 (19)0.017 (2)−0.0048 (18)
C110.050 (3)0.026 (2)0.042 (3)−0.006 (2)0.028 (2)−0.012 (2)
C120.036 (2)0.032 (2)0.036 (2)0.004 (2)0.023 (2)−0.004 (2)
C130.029 (2)0.025 (2)0.025 (2)−0.0008 (17)0.0142 (18)0.0002 (17)
C140.031 (2)0.026 (2)0.022 (2)−0.0022 (17)0.0121 (18)−0.0050 (16)
N10.040 (3)0.053 (3)0.066 (3)0.010 (2)0.011 (2)0.029 (3)
N20.039 (2)0.033 (2)0.033 (2)−0.0057 (19)0.0202 (17)−0.0008 (18)
O10.0361 (18)0.0295 (17)0.0296 (17)0.0098 (14)0.0094 (14)0.0047 (14)
O20.0403 (19)0.0284 (16)0.0245 (15)0.0020 (14)0.0173 (14)−0.0037 (13)
O1W0.085 (3)0.0282 (19)0.035 (2)−0.0070 (19)0.018 (2)−0.0013 (16)
O30.0395 (19)0.0224 (16)0.048 (2)0.0059 (14)0.0189 (17)0.0113 (14)
O2W0.044 (2)0.049 (2)0.053 (2)0.0137 (18)0.0309 (19)0.0096 (19)
O40.0356 (18)0.041 (2)0.0288 (16)−0.0065 (15)0.0194 (14)−0.0036 (14)
O3W0.067 (3)0.0277 (18)0.065 (3)−0.0033 (18)0.050 (2)0.0008 (17)
Cl10.0314 (6)0.0699 (10)0.0373 (6)0.0061 (6)0.0114 (5)0.0087 (6)
Cl20.0609 (9)0.0258 (6)0.0508 (8)−0.0008 (6)0.0260 (7)−0.0036 (5)
Cl30.0387 (7)0.0364 (6)0.0460 (7)0.0029 (5)0.0177 (6)0.0077 (5)
La10.02571 (12)0.02025 (11)0.02189 (11)0.00083 (11)0.01252 (9)0.00244 (11)
C1—O31.249 (6)C13—N21.460 (6)
C1—O11.261 (6)C14—H140.9300
C1—C21.518 (6)N1—H1A0.8900
C2—C71.385 (7)N1—H1B0.8900
C2—C31.390 (6)N1—H1C0.8900
C3—C41.381 (7)N2—H2A0.8900
C3—H30.9300N2—H2B0.8900
C4—C51.376 (8)N2—H2C0.8900
C4—H40.9300O1—La12.453 (3)
C5—C61.369 (7)O2—La1i2.484 (3)
C5—H50.9300O2—La12.875 (3)
C6—C71.374 (6)O1W—La12.618 (4)
C6—N11.474 (7)O1W—H110.8086
C7—H70.9300O1W—H210.8660
C8—O41.255 (6)O3—La1i2.472 (3)
C8—O21.263 (5)O2W—La12.557 (3)
C8—C91.506 (6)O2W—H120.8700
C8—La13.047 (4)O2W—H220.8447
C9—C101.387 (6)O4—La12.503 (3)
C9—C141.392 (6)O3W—La12.575 (3)
C10—C111.367 (6)O3W—H130.7901
C10—H100.9300O3W—H230.9015
C11—C121.383 (7)Cl1—La12.9545 (13)
C11—H010.9300La1—O3i2.472 (3)
C12—C131.372 (6)La1—O2i2.484 (3)
C12—H020.9300La1—La1i4.2245 (5)
C13—C141.383 (6)
O3—C1—O1126.5 (4)C1—O3—La1i135.8 (3)
O3—C1—C2116.9 (4)La1—O2W—H12127.0
O1—C1—C2116.6 (4)La1—O2W—H22119.0
C7—C2—C3119.7 (4)H12—O2W—H22101.6
C7—C2—C1120.5 (4)C8—O4—La1103.3 (3)
C3—C2—C1119.7 (4)La1—O3W—H1391.2
C4—C3—C2120.5 (5)La1—O3W—H23117.3
C4—C3—H3119.7H13—O3W—H23130.3
C2—C3—H3119.7O1—La1—O3i131.54 (12)
C5—C4—C3119.4 (5)O1—La1—O2i71.07 (11)
C5—C4—H4120.3O3i—La1—O2i77.85 (12)
C3—C4—H4120.3O1—La1—O480.34 (11)
C6—C5—C4119.6 (5)O3i—La1—O487.11 (12)
C6—C5—H5120.2O2i—La1—O4123.36 (11)
C4—C5—H5120.2O1—La1—O2W132.54 (12)
C5—C6—C7122.0 (5)O3i—La1—O2W71.41 (12)
C5—C6—N1117.8 (5)O2i—La1—O2W77.07 (12)
C7—C6—N1120.1 (5)O4—La1—O2W147.12 (12)
C6—C7—C2118.6 (5)O1—La1—O3W74.48 (12)
C6—C7—H7120.7O3i—La1—O3W137.80 (12)
C2—C7—H7120.7O2i—La1—O3W83.47 (12)
O4—C8—O2122.7 (4)O4—La1—O3W134.14 (11)
O4—C8—C9117.6 (4)O2W—La1—O3W67.65 (12)
O2—C8—C9119.7 (4)O1—La1—O1W72.27 (13)
O4—C8—La153.1 (2)O3i—La1—O1W142.99 (13)
O2—C8—La170.1 (2)O2i—La1—O1W138.47 (12)
C9—C8—La1167.6 (3)O4—La1—O1W67.64 (12)
C10—C9—C14120.4 (4)O2W—La1—O1W116.19 (14)
C10—C9—C8118.3 (4)O3W—La1—O1W68.43 (12)
C14—C9—C8121.3 (4)O1—La1—O269.52 (10)
C11—C10—C9120.1 (4)O3i—La1—O267.52 (10)
C11—C10—H10120.0O2i—La1—O276.19 (10)
C9—C10—H10120.0O4—La1—O247.91 (10)
C10—C11—C12120.5 (4)O2W—La1—O2134.59 (11)
C10—C11—H01119.7O3W—La1—O2142.73 (12)
C12—C11—H01119.7O1W—La1—O2108.19 (12)
C13—C12—C11118.9 (4)O1—La1—Cl1142.89 (9)
C13—C12—H02120.5O3i—La1—Cl176.39 (9)
C11—C12—H02120.5O2i—La1—Cl1145.93 (8)
C12—C13—C14122.1 (4)O4—La1—Cl177.14 (9)
C12—C13—N2118.6 (4)O2W—La1—Cl173.83 (10)
C14—C13—N2119.2 (4)O3W—La1—Cl1101.19 (10)
C13—C14—C9117.9 (4)O1W—La1—Cl172.00 (10)
C13—C14—H14121.0O2—La1—Cl1113.19 (7)
C9—C14—H14121.0O1—La1—C871.87 (12)
C6—N1—H1A109.5O3i—La1—C878.12 (12)
C6—N1—H1B109.5O2i—La1—C899.88 (12)
H1A—N1—H1B109.5O4—La1—C823.63 (12)
C6—N1—H1C109.5O2W—La1—C8149.37 (12)
H1A—N1—H1C109.5O3W—La1—C8142.86 (12)
H1B—N1—H1C109.5O1W—La1—C886.58 (13)
C13—N2—H2A109.5O2—La1—C824.41 (10)
C13—N2—H2B109.5Cl1—La1—C896.26 (9)
H2A—N2—H2B109.5O1—La1—La1i64.61 (8)
C13—N2—H2C109.5O3i—La1—La1i67.42 (9)
H2A—N2—H2C109.5O2i—La1—La1i41.37 (7)
H2B—N2—H2C109.5O4—La1—La1i82.37 (8)
C1—O1—La1138.4 (3)O2W—La1—La1i110.25 (10)
C8—O2—La1i163.2 (3)O3W—La1—La1i118.34 (10)
C8—O2—La185.4 (3)O1W—La1—La1i130.75 (10)
La1i—O2—La1103.81 (10)O2—La1—La1i34.82 (6)
La1—O1W—H11128.0Cl1—La1—La1i139.03 (3)
La1—O1W—H21115.2C8—La1—La1i58.74 (9)
H11—O1W—H21116.0
D—H···AD—HH···AD···AD—H···A
N1—H1A···Cl30.892.303.170 (5)167.
N1—H1B···Cl2ii0.892.433.214 (5)147.
N2—H2A···O4iii0.892.453.046 (5)125.
N2—H2A···Cl20.892.493.221 (4)140.
N2—H2B···Cl3iv0.892.283.169 (4)177.
N2—H2C···Cl1iii0.892.493.215 (4)138.
N2—H2C···Cl1v0.892.723.349 (5)128.
O1W—H11···Cl2iii0.812.393.186 (4)170.
O1W—H21···Cl2vi0.872.383.196 (4)157.
O2W—H12···Cl3vii0.872.263.123 (4)172.
O2W—H22···Cl3viii0.842.473.276 (4)160.
O3W—H13···O1W0.792.412.920 (5)124.
O3W—H13···Cl2vi0.792.533.156 (4)137.
O3W—H23···Cl3viii0.902.173.069 (4)172.
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
N1—H1A⋯Cl30.892.303.170 (5)167
N1—H1B⋯Cl2i0.892.433.214 (5)147
N2—H2A⋯O4ii0.892.453.046 (5)125
N2—H2A⋯Cl20.892.493.221 (4)140
N2—H2B⋯Cl3iii0.892.283.169 (4)177
N2—H2C⋯Cl1ii0.892.493.215 (4)138
N2—H2C⋯Cl1iv0.892.723.349 (5)128
O1W—H11⋯Cl2ii0.812.393.186 (4)170
O1W—H21⋯Cl2v0.872.383.196 (4)157
O2W—H12⋯Cl3vi0.872.263.123 (4)172
O2W—H22⋯Cl3vii0.842.473.276 (4)160
O3W—H13⋯O1W0.792.412.920 (5)124
O3W—H13⋯Cl2v0.792.533.156 (4)137
O3W—H23⋯Cl3vii0.902.173.069 (4)172

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

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Journal:  J Am Chem Soc       Date:  2005-03-23       Impact factor: 15.419

6.  Highly luminescent, triple- and quadruple-stranded, dinuclear Eu, Nd, and Sm(III) lanthanide complexes based on bis-diketonate ligands.

Authors:  Andrew P Bassett; Steven W Magennis; Peter B Glover; David J Lewis; Neil Spencer; Simon Parsons; René M Williams; Luisa De Cola; Zoe Pikramenou
Journal:  J Am Chem Soc       Date:  2004-08-04       Impact factor: 15.419

7.  Lanthanide coordination polymers and their Ag+-modulated fluorescence.

Authors:  Weisheng Liu; Tianquan Jiao; Yizhi Li; Quanzhong Liu; Minyu Tan; Hong Wang; Liufang Wang
Journal:  J Am Chem Soc       Date:  2004-03-03       Impact factor: 15.419

8.  Structure validation in chemical crystallography.

Authors:  Anthony L Spek
Journal:  Acta Crystallogr D Biol Crystallogr       Date:  2009-01-20
  8 in total
  1 in total

1.  Tetra-kis(μ-3-aza-niumylbenzoato)-κO:O,O';κO,O':O;κO:O'-bis-[tetra-aqua-neodymium(III)] hexa-chloride tetra-hydrate.

Authors:  Meriem Benslimane; Hocine Merazig; Jean-Claude Daran
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-04-13
  1 in total

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