Literature DB >> 21836843

Poly[dimethyl-ammonium [aquadi-μ(2)-oxalato-samarate(III)] trihydrate].

Yao-Kang Lv1, Li-Hua Gan, Ming-Xian Liu, Wei Xiong.   

Abstract

In the title complex, {(C(2)H(8)N)[Sm(C(2)O(4))(2)(H(2)O)]·3H(2)O}(n), the Sm(III) atom is chelated by four oxalate ligands and one water mol-ecule forming a distorted tricapped trigonal-prismatic geometry. Each oxalate ligand chelates to two Sm(III) atoms, generating a three-dimensional anionic network with cavities in which the ammonium cations and lattice water mol-ecules reside. Various O-H⋯O, N-H⋯O and C-H⋯O hydrogen-bonding inter-actions further stablize the crystal structure.

Entities:  

Year:  2011        PMID： 21836843      PMCID： PMC3152119          DOI： 10.1107/S1600536811020058

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


Related literature

For general background to the rational design and synthesis of metal-organic polymers, see: Kim et al. (1998 ▶); Lv et al. (2011 ▶). For related structures, see: Lv et al. (2010 ▶); Trombe & Mohanu (2004 ▶). The structure of the isotypic EuIII compound was reported by Yang et al. (2005 ▶), and the DyIII compound was reported by Ye & Lin (2010 ▶).

Experimental

Crystal data

(C2H8N)[Sm(C2O4)2(H2O)]·3H2O M = 444.55 Monoclinic, a = 9.6711 (3) Å b = 11.7849 (3) Å c = 14.3863 (4) Å β = 122.276 (2)° V = 1386.30 (7) Å3 Z = 4 Mo Kα radiation μ = 4.30 mm−1 T = 296 K 0.17 × 0.14 × 0.08 mm

Data collection

Bruker APEXII area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.36, T max = 0.43 12866 measured reflections 3225 independent reflections 2739 reflections with I > 2σ(I) R int = 0.039

Refinement

R[F 2 > 2σ(F 2)] = 0.026 wR(F 2) = 0.061 S = 1.03 3225 reflections 207 parameters 12 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.69 e Å−3 Δρmin = −0.98 e Å−3 Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: SAINT (Bruker, 2006 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg & Putz, 2004 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶). Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811020058/om2429sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811020058/om2429Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
(C2H8N)[Sm(C2O4)2(H2O)]·3H2OF(000) = 868
Mr = 444.55Dx = 2.130 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3706 reflections
a = 9.6711 (3) Åθ = 2.5–27.7°
b = 11.7849 (3) ŵ = 4.30 mm−1
c = 14.3863 (4) ÅT = 296 K
β = 122.276 (2)°Block, colourless
V = 1386.30 (7) Å30.17 × 0.14 × 0.08 mm
Z = 4
Bruker APEXII area-detector diffractometer3225 independent reflections
Radiation source: fine-focus sealed tube2739 reflections with I > 2σ(I)
graphiteRint = 0.039
ω scansθmax = 27.7°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −12→12
Tmin = 0.36, Tmax = 0.43k = −15→14
12866 measured reflectionsl = −16→18
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.026Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.061H atoms treated by a mixture of independent and constrained refinement
S = 1.03w = 1/[σ2(Fo2) + (0.0215P)2 + 2.7236P] where P = (Fo2 + 2Fc2)/3
3225 reflections(Δ/σ)max = 0.001
207 parametersΔρmax = 0.69 e Å−3
12 restraintsΔρmin = −0.98 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
Sm10.61680 (2)0.983582 (14)0.330364 (15)0.01793 (7)
O10.7036 (3)0.7832 (2)0.3435 (2)0.0284 (6)
O20.6156 (3)0.6045 (2)0.3014 (2)0.0293 (7)
O30.3063 (3)0.6799 (2)0.1732 (2)0.0242 (6)
O40.3978 (3)0.8576 (2)0.2047 (2)0.0241 (6)
O60.5172 (3)0.8817 (2)0.4343 (2)0.0286 (6)
O70.5330 (4)1.1081 (2)0.4324 (3)0.0334 (7)
O80.8912 (3)0.9847 (2)0.3572 (2)0.0253 (6)
O90.8415 (3)0.9876 (2)0.5228 (2)0.0289 (6)
O1W0.6084 (4)0.9755 (3)0.1530 (2)0.0330 (7)
H1WA0.608 (6)1.033 (2)0.121 (3)0.040*
H1WB0.544 (5)0.932 (3)0.103 (3)0.040*
O2W1.3864 (6)0.8423 (3)0.9661 (4)0.0614 (11)
H2WA1.426 (7)0.783 (3)0.962 (5)0.074*
H2WB1.306 (5)0.827 (5)0.966 (6)0.074*
O3W0.8362 (7)0.5053 (4)0.5101 (4)0.0799 (15)
H3WA0.793 (9)0.521 (5)0.443 (2)0.096*
H3WB0.876 (8)0.442 (3)0.517 (5)0.096*
O4W1.0543 (5)0.7816 (4)0.9682 (4)0.0767 (14)
H4WA0.958 (3)0.763 (6)0.942 (5)0.092*
H4WB1.106 (6)0.742 (5)1.024 (4)0.092*
N10.9284 (5)0.6293 (4)0.6960 (3)0.0430 (10)
H1A0.88670.58900.63340.052*
H1B0.89470.59620.73690.052*
C10.5958 (4)0.7095 (3)0.2949 (3)0.0212 (8)
C20.4172 (4)0.7536 (3)0.2173 (3)0.0200 (7)
C30.4950 (4)0.9348 (3)0.5004 (3)0.0238 (8)
C41.0168 (4)0.9999 (3)0.4541 (3)0.0202 (8)
C51.1056 (7)0.6231 (7)0.7555 (5)0.076 (2)
H5A1.13920.54500.76870.091*
H5B1.15140.66210.82430.091*
H5C1.14330.65790.71260.091*
C60.8628 (9)0.7443 (6)0.6685 (6)0.083 (2)
H6A0.74550.74140.62560.100*
H6B0.90120.78130.62690.100*
H6C0.89870.78610.73490.100*
U11U22U33U12U13U23
Sm10.01682 (10)0.01446 (10)0.01891 (10)−0.00015 (7)0.00713 (8)−0.00032 (7)
O10.0186 (14)0.0194 (14)0.0365 (17)−0.0004 (10)0.0076 (12)−0.0044 (11)
O20.0225 (14)0.0156 (13)0.0327 (16)0.0014 (10)0.0032 (12)−0.0002 (11)
O30.0199 (13)0.0176 (13)0.0313 (15)0.0008 (10)0.0111 (12)−0.0021 (11)
O40.0222 (14)0.0171 (13)0.0234 (14)0.0010 (10)0.0057 (12)0.0003 (10)
O60.0358 (16)0.0225 (14)0.0311 (16)−0.0052 (11)0.0203 (13)−0.0054 (11)
O70.0479 (18)0.0213 (14)0.0428 (18)0.0052 (12)0.0322 (16)0.0063 (12)
O80.0199 (13)0.0337 (15)0.0169 (13)−0.0009 (11)0.0061 (11)−0.0030 (11)
O90.0195 (14)0.0437 (17)0.0235 (14)−0.0032 (12)0.0114 (12)−0.0030 (12)
O1W0.0363 (17)0.0349 (17)0.0209 (15)−0.0056 (13)0.0108 (13)−0.0013 (12)
O2W0.073 (3)0.035 (2)0.063 (3)0.0036 (18)0.028 (2)0.0070 (19)
O3W0.084 (3)0.078 (3)0.047 (3)0.027 (3)0.014 (3)−0.003 (2)
O4W0.056 (3)0.053 (3)0.069 (3)−0.008 (2)−0.002 (2)0.014 (2)
N10.035 (2)0.057 (3)0.036 (2)−0.0080 (18)0.0180 (18)0.0077 (18)
C10.0196 (19)0.0201 (19)0.0190 (18)0.0007 (13)0.0069 (16)−0.0017 (14)
C20.0209 (19)0.0206 (19)0.0171 (17)0.0011 (14)0.0092 (15)0.0001 (14)
C30.0196 (18)0.025 (2)0.0225 (19)0.0000 (14)0.0081 (15)0.0006 (15)
C40.0217 (19)0.0137 (17)0.0190 (18)−0.0016 (13)0.0068 (15)0.0015 (13)
C50.041 (3)0.126 (6)0.051 (4)−0.010 (4)0.018 (3)0.020 (4)
C60.104 (6)0.067 (4)0.086 (5)0.012 (4)0.056 (5)0.017 (4)
Sm1—O42.422 (3)O2W—H2WA0.811 (19)
Sm1—O3i2.440 (2)O2W—H2WB0.798 (19)
Sm1—O92.442 (3)O3W—H3WA0.839 (19)
Sm1—O82.469 (3)O3W—H3WB0.819 (19)
Sm1—O2i2.474 (3)O4W—H4WA0.83 (2)
Sm1—O62.479 (3)O4W—H4WB0.823 (19)
Sm1—O12.479 (3)N1—C51.452 (7)
Sm1—O72.497 (3)N1—C61.459 (8)
Sm1—O1W2.512 (3)N1—H1A0.9001
O1—C11.246 (4)N1—H1B0.9001
O2—C11.248 (4)C1—C21.562 (5)
O2—Sm1ii2.474 (3)C3—O7iii1.242 (5)
O3—C21.257 (4)C3—C3iii1.541 (8)
O3—Sm1ii2.440 (2)C4—O9iv1.234 (5)
O4—C21.238 (4)C4—C4iv1.519 (8)
O6—C31.248 (5)C5—H5A0.9600
O7—C3iii1.242 (5)C5—H5B0.9600
O8—C41.282 (4)C5—H5C0.9600
O9—C4iv1.234 (5)C6—H6A0.9600
O1W—H1WA0.817 (18)C6—H6B0.9600
O1W—H1WB0.828 (18)C6—H6C0.9600
O4—Sm1—O3i136.09 (9)C3—O6—Sm1119.8 (2)
O4—Sm1—O9138.78 (9)C3iii—O7—Sm1119.5 (2)
O3i—Sm1—O984.76 (9)C4—O8—Sm1119.1 (2)
O4—Sm1—O8123.92 (9)C4iv—O9—Sm1119.7 (2)
O3i—Sm1—O871.56 (9)Sm1—O1W—H1WA122 (3)
O9—Sm1—O865.88 (9)Sm1—O1W—H1WB120 (3)
O4—Sm1—O2i72.94 (8)H1WA—O1W—H1WB104 (3)
O3i—Sm1—O2i66.43 (8)H2WA—O2W—H2WB108 (3)
O9—Sm1—O2i138.73 (9)H3WA—O3W—H3WB105 (3)
O8—Sm1—O2i125.24 (9)H4WA—O4W—H4WB105 (3)
O4—Sm1—O671.76 (9)C5—N1—C6114.3 (5)
O3i—Sm1—O6133.88 (9)C5—N1—H1A108.6
O9—Sm1—O673.91 (9)C6—N1—H1A108.8
O8—Sm1—O6129.79 (9)C5—N1—H1B108.5
O2i—Sm1—O6104.74 (10)C6—N1—H1B108.8
O4—Sm1—O166.34 (8)H1A—N1—H1B107.6
O3i—Sm1—O1144.12 (9)O1—C1—O2126.9 (3)
O9—Sm1—O182.65 (9)O1—C1—C2116.3 (3)
O8—Sm1—O172.62 (9)O2—C1—C2116.8 (3)
O2i—Sm1—O1137.62 (9)O4—C2—O3126.0 (3)
O6—Sm1—O173.62 (9)O4—C2—C1117.2 (3)
O4—Sm1—O7111.72 (10)O3—C2—C1116.8 (3)
O3i—Sm1—O769.72 (9)O7iii—C3—O6125.9 (4)
O9—Sm1—O772.18 (10)O7iii—C3—C3iii116.9 (4)
O8—Sm1—O7124.34 (9)O6—C3—C3iii117.2 (4)
O2i—Sm1—O770.42 (10)O9iv—C4—O8125.5 (4)
O6—Sm1—O764.99 (9)O9iv—C4—C4iv119.2 (4)
O1—Sm1—O7135.89 (10)O8—C4—C4iv115.3 (4)
O4—Sm1—O1W71.17 (10)N1—C5—H5A109.5
O3i—Sm1—O1W81.92 (10)N1—C5—H5B109.5
O9—Sm1—O1W132.76 (10)H5A—C5—H5B109.5
O8—Sm1—O1W66.90 (9)N1—C5—H5C109.5
O2i—Sm1—O1W73.75 (10)H5A—C5—H5C109.5
O6—Sm1—O1W141.50 (9)H5B—C5—H5C109.5
O1—Sm1—O1W82.35 (10)N1—C6—H6A109.5
O7—Sm1—O1W140.82 (10)N1—C6—H6B109.5
C1—O1—Sm1118.3 (2)H6A—C6—H6B109.5
C1—O2—Sm1ii118.2 (2)N1—C6—H6C109.5
C2—O3—Sm1ii118.6 (2)H6A—C6—H6C109.5
C2—O4—Sm1119.6 (2)H6B—C6—H6C109.5
O4—Sm1—O1—C1−10.9 (3)O4—Sm1—O8—C4−141.7 (2)
O3i—Sm1—O1—C1−148.3 (3)O3i—Sm1—O8—C484.6 (2)
O9—Sm1—O1—C1141.3 (3)O9—Sm1—O8—C4−7.9 (2)
O8—Sm1—O1—C1−151.8 (3)O2i—Sm1—O8—C4125.8 (2)
O2i—Sm1—O1—C1−28.1 (4)O6—Sm1—O8—C4−47.7 (3)
O6—Sm1—O1—C166.0 (3)O1—Sm1—O8—C4−97.6 (3)
O7—Sm1—O1—C186.5 (3)O7—Sm1—O8—C436.7 (3)
O1W—Sm1—O1—C1−83.6 (3)O1W—Sm1—O8—C4173.5 (3)
O3i—Sm1—O4—C2158.7 (3)O4—Sm1—O9—C4iv122.0 (3)
O9—Sm1—O4—C2−31.0 (3)O3i—Sm1—O9—C4iv−64.8 (3)
O8—Sm1—O4—C260.2 (3)O8—Sm1—O9—C4iv7.4 (3)
O2i—Sm1—O4—C2−178.4 (3)O2i—Sm1—O9—C4iv−109.3 (3)
O6—Sm1—O4—C2−66.0 (3)O6—Sm1—O9—C4iv156.6 (3)
O1—Sm1—O4—C213.6 (3)O1—Sm1—O9—C4iv81.6 (3)
O7—Sm1—O4—C2−118.4 (3)O7—Sm1—O9—C4iv−135.1 (3)
O1W—Sm1—O4—C2103.4 (3)O1W—Sm1—O9—C4iv9.2 (3)
O4—Sm1—O6—C3−136.1 (3)Sm1—O1—C1—O2−172.2 (3)
O3i—Sm1—O6—C31.2 (3)Sm1—O1—C1—C28.1 (4)
O9—Sm1—O6—C367.1 (3)Sm1ii—O2—C1—O1−169.5 (3)
O8—Sm1—O6—C3104.5 (3)Sm1ii—O2—C1—C210.2 (5)
O2i—Sm1—O6—C3−70.1 (3)Sm1—O4—C2—O3165.1 (3)
O1—Sm1—O6—C3154.0 (3)Sm1—O4—C2—C1−15.0 (4)
O7—Sm1—O6—C3−10.4 (3)Sm1ii—O3—C2—O4162.8 (3)
O1W—Sm1—O6—C3−152.4 (3)Sm1ii—O3—C2—C1−17.2 (4)
O4—Sm1—O7—C3iii66.9 (3)O1—C1—C2—O44.4 (5)
O3i—Sm1—O7—C3iii−160.3 (3)O2—C1—C2—O4−175.4 (4)
O9—Sm1—O7—C3iii−69.4 (3)O1—C1—C2—O3−175.7 (3)
O8—Sm1—O7—C3iii−111.7 (3)O2—C1—C2—O34.5 (5)
O2i—Sm1—O7—C3iii128.4 (3)Sm1—O6—C3—O7iii−169.7 (3)
O6—Sm1—O7—C3iii10.8 (3)Sm1—O6—C3—C3iii9.6 (5)
O1—Sm1—O7—C3iii−11.0 (4)Sm1—O8—C4—O9iv−173.2 (3)
O1W—Sm1—O7—C3iii153.4 (3)Sm1—O8—C4—C4iv7.9 (5)
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O2Wiv0.82 (2)1.95 (2)2.764 (5)174 (5)
O1W—H1WB···O2Wv0.83 (2)2.03 (2)2.852 (5)172 (4)
O2W—H2WA···O6vi0.81 (2)2.26 (2)3.065 (5)175 (6)
O2W—H2WA···O7vii0.81 (2)2.47 (5)3.023 (5)126 (5)
O2W—H2WB···O4W0.80 (2)2.51 (2)3.306 (7)179 (6)
O2W—H2WB···O3Wviii0.80 (2)2.64 (5)3.039 (8)113 (5)
O3W—H3WA···O20.84 (2)2.08 (3)2.845 (5)151 (6)
O3W—H3WB···O4Wvii0.82 (2)1.98 (2)2.796 (6)172 (8)
O4W—H4WA···O1ix0.83 (2)2.15 (2)2.967 (5)169 (6)
O4W—H4WB···O3x0.82 (2)2.11 (2)2.898 (5)160 (6)
N1—H1A···O3W0.901.852.744 (6)171
N1—H1B···O8ix0.901.992.864 (5)163
N1—H1B···O1Wix0.902.503.071 (5)122
C5—H5C···O4vi0.962.533.283 (7)135
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1W—H1WA⋯O2Wi0.82 (2)1.95 (2)2.764 (5)174 (5)
O1W—H1WB⋯O2Wii0.83 (2)2.03 (2)2.852 (5)172 (4)
O2W—H2WA⋯O6iii0.81 (2)2.26 (2)3.065 (5)175 (6)
O2W—H2WA⋯O7iv0.81 (2)2.47 (5)3.023 (5)126 (5)
O2W—H2WB⋯O4W0.80 (2)2.51 (2)3.306 (7)179 (6)
O2W—H2WB⋯O3Wv0.80 (2)2.64 (5)3.039 (8)113 (5)
O3W—H3WA⋯O20.84 (2)2.08 (3)2.845 (5)151 (6)
O3W—H3WB⋯O4Wiv0.82 (2)1.98 (2)2.796 (6)172 (8)
O4W—H4WA⋯O1vi0.83 (2)2.15 (2)2.967 (5)169 (6)
O4W—H4WB⋯O3vii0.82 (2)2.11 (2)2.898 (5)160 (6)
N1—H1A⋯O3W0.901.852.744 (6)171
N1—H1B⋯O8vi0.901.992.864 (5)163
N1—H1B⋯O1Wvi0.902.503.071 (5)122
C5—H5C⋯O4iii0.962.533.283 (7)135

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

  3 in total

1.  A short history of SHELX.

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

2.  Poly[dimethyl-ammonium [aquadi-μ(2)-oxalato-dysprosate(III)] trihydrate].

Authors:  Su-Fang Ye; Hong Lin
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-07-07

3.  catena-Poly[[(1,10-phenanthroline-κN,N')cadmium(II)]-μ-oxalato-κO,O:O,O].

Authors:  Yao-Kang Lv; Li-Hua Gan; Yong-Jie Cao; Biao-Feng Gao; Liu-Hua Chen
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-10-23
  3 in total

北京卡尤迪生物科技股份有限公司 © 2022-2023.