Literature DB >> 21588859

Poly[[[μ(3)-N'-(carboxymethyl)ethylene-di-amine-N,N,N'-triacetato]dysprosium(III)] trihydrate].

Xiaomei Zhuang¹, Qingping Long, Jun Wang.

Abstract

In the title coordination polymer, {[Dy(C(10)H(13)N(2)O(8))]·3H(2)O}(n), the dysprosium(III) ion is coordinated by two N atoms and six O atoms from three different (carb-oxy-meth-yl)ethyl-ene-diamine-triacetate ligands in a distorted square-anti-prismatic geometry. The ligands connect the metal atoms, forming layers parallel to the ab plane. O-H⋯O hydrogen bonds further assemble adjacent layers into a three-dimensional supra-molecular network.

Entities: Chemical Disease Species

Year: 2010 PMID： 21588859 PMCID： PMC3009363 DOI： 10.1107/S1600536810041784

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

Related literature

For general background to the topologies and potential applications of metal coordination polymers, see: Benelli & Gatteschi (2002 ▶). For related structures, see: Wang et al. (2007 ▶); You & Ng (2007 ▶); Sakagami et al. (1999 ▶); Templeton et al. (1985 ▶); Vikram & Sivasankar (2008 ▶).

Experimental

Crystal data

[Dy(C10H13N2O8)]·3H2O M = 505.77 Orthorhombic, a = 13.3835 (5) Å b = 13.0127 (4) Å c = 18.6943 (7) Å V = 3255.7 (2) Å3 Z = 8 Mo Kα radiation μ = 4.65 mm−1 T = 296 K 0.25 × 0.19 × 0.18 mm

Data collection

Bruker APEXII area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2004 ▶) T min = 0.389, T max = 0.488 19825 measured reflections 3192 independent reflections 2230 reflections with I > 2σ(I) R int = 0.034

Refinement

R[F 2 > 2σ(F 2)] = 0.024 wR(F 2) = 0.061 S = 1.07 3192 reflections 217 parameters H-atom parameters constrained Δρmax = 0.74 e Å−3 Δρmin = −0.69 e Å−3 Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810041784/rz2501sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810041784/rz2501Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Dy(C₁₀H₁₃N₂O₈)]·3H₂O	F(000) = 1976
M_r = 505.77	D_x = 2.064 Mg m⁻³
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 4800 reflections
a = 13.3835 (5) Å	θ = 1.4–28.0°
b = 13.0127 (4) Å	µ = 4.65 mm⁻¹
c = 18.6943 (7) Å	T = 296 K
V = 3255.7 (2) Å³	Block, colourless
Z = 8	0.25 × 0.19 × 0.18 mm

Bruker APEXII area-detector diffractometer	3192 independent reflections
Radiation source: fine-focus sealed tube	2230 reflections with I > 2σ(I)
graphite	R_int = 0.034
φ and ω scan	θ_max = 26.0°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 2008)	h = −13→16
T_min = 0.389, T_max = 0.488	k = −16→16
19825 measured reflections	l = −22→20

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)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.061	H-atom parameters constrained
S = 1.07	w = 1/[σ²(F_o²) + (0.0239P)² + 3.1993P] where P = (F_o² + 2F_c²)/3
3192 reflections	(Δ/σ)_max = 0.001
217 parameters	Δρ_max = 0.74 e Å⁻³
0 restraints	Δρ_min = −0.69 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.

	x	y	z	U_iso*/U_eq
Dy1	0.195820 (13)	0.546220 (11)	0.248589 (10)	0.01538 (8)
N1	0.1266 (2)	0.6990 (2)	0.32682 (16)	0.0170 (7)
N2	0.0619 (2)	0.6517 (2)	0.17784 (16)	0.0167 (7)
C4	0.1889 (3)	0.5806 (3)	0.4196 (2)	0.0220 (10)
C3	0.1109 (3)	0.6609 (3)	0.4002 (2)	0.0219 (9)
H3A	0.0448	0.6310	0.4040	0.026*
H3B	0.1149	0.7178	0.4335	0.026*
C2	0.1622 (3)	0.5832 (3)	0.0792 (2)	0.0245 (10)
C1	0.0980 (3)	0.6704 (3)	0.1040 (2)	0.0231 (10)
H1A	0.1362	0.7337	0.1027	0.028*
H1B	0.0414	0.6779	0.0721	0.028*
C6	0.0396 (3)	0.7507 (3)	0.2145 (2)	0.0187 (9)
H6A	−0.0229	0.7778	0.1964	0.022*
H6B	0.0918	0.7998	0.2033	0.022*
C5	0.0323 (3)	0.7387 (3)	0.2951 (2)	0.0195 (9)
H5A	0.0166	0.8048	0.3163	0.023*
H5B	−0.0217	0.6918	0.3064	0.023*
O2	0.1990 (2)	0.5221 (2)	0.12204 (15)	0.0305 (8)
O4	0.2355 (2)	0.5364 (2)	0.36996 (14)	0.0258 (7)
O3	0.2014 (2)	0.5610 (2)	0.48468 (15)	0.0375 (8)
O1	0.1763 (3)	0.5794 (3)	0.01143 (16)	0.0444 (9)
H1	0.2118	0.5300	0.0018	0.067*
C8	0.2652 (3)	0.7845 (3)	0.2596 (2)	0.0187 (9)
C7	0.2041 (3)	0.7799 (3)	0.3277 (2)	0.0204 (9)
H7A	0.2487	0.7677	0.3677	0.024*
H7B	0.1722	0.8459	0.3352	0.024*
O5	0.2750 (2)	0.70278 (19)	0.22414 (15)	0.0228 (6)
C10	−0.0465 (3)	0.5264 (3)	0.2434 (2)	0.0180 (9)
C9	−0.0296 (3)	0.5873 (3)	0.1748 (2)	0.0219 (9)
H9A	−0.0243	0.5399	0.1349	0.026*
H9B	−0.0870	0.6312	0.1663	0.026*
O6	0.03078 (19)	0.4997 (2)	0.27769 (15)	0.0218 (6)
O7	0.30708 (18)	0.86679 (19)	0.24311 (14)	0.0243 (7)
O8	−0.13277 (19)	0.50137 (19)	0.26058 (14)	0.0216 (6)
O1W	0.9746 (4)	0.4386 (3)	0.4225 (2)	0.0840 (14)
H2W	0.9668	0.4475	0.3780	0.126*
H1W	0.9200	0.4478	0.4441	0.126*
O2W	0.8853 (3)	0.7777 (3)	0.0541 (2)	0.0798 (13)
H3W	0.8606	0.7769	0.0133	0.096*
H4W	0.9063	0.8364	0.0649	0.096*
O3W	0.3282 (4)	0.7889 (3)	0.0831 (2)	0.0966 (16)
H6W	0.2814	0.8319	0.0909	0.145*
H5W	0.3833	0.8247	0.0785	0.145*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Dy1	0.01199 (11)	0.01112 (10)	0.02303 (12)	0.00043 (6)	0.00005 (9)	−0.00001 (9)
N1	0.0157 (17)	0.0155 (15)	0.0197 (18)	0.0009 (14)	−0.0011 (14)	0.0026 (14)
N2	0.0193 (18)	0.0153 (16)	0.0156 (17)	0.0010 (14)	0.0044 (14)	0.0002 (14)
C4	0.023 (2)	0.020 (2)	0.022 (2)	0.0000 (18)	−0.0041 (19)	0.0008 (18)
C3	0.025 (2)	0.025 (2)	0.016 (2)	−0.0007 (19)	0.0048 (18)	−0.0006 (18)
C2	0.024 (2)	0.029 (2)	0.020 (2)	0.002 (2)	0.005 (2)	−0.0044 (19)
C1	0.024 (2)	0.023 (2)	0.022 (2)	0.0052 (19)	0.0024 (18)	0.0024 (18)
C6	0.015 (2)	0.0148 (19)	0.027 (2)	0.0073 (17)	−0.0028 (18)	0.0023 (17)
C5	0.017 (2)	0.0167 (19)	0.025 (2)	0.0043 (17)	0.0026 (18)	−0.0020 (17)
O2	0.042 (2)	0.0291 (16)	0.0204 (16)	0.0182 (14)	0.0014 (14)	−0.0032 (13)
O4	0.0253 (17)	0.0287 (16)	0.0233 (16)	0.0092 (14)	−0.0022 (14)	0.0028 (13)
O3	0.046 (2)	0.048 (2)	0.0180 (16)	0.0207 (16)	−0.0026 (14)	0.0043 (15)
O1	0.059 (2)	0.048 (2)	0.0260 (18)	0.0262 (18)	0.0108 (16)	0.0033 (16)
C8	0.0086 (18)	0.0125 (18)	0.035 (3)	0.0022 (15)	−0.0059 (18)	0.0031 (18)
C7	0.023 (2)	0.0147 (19)	0.023 (2)	−0.0004 (17)	−0.0021 (18)	−0.0029 (17)
O5	0.0212 (15)	0.0139 (14)	0.0332 (16)	−0.0004 (12)	0.0088 (13)	−0.0013 (12)
C10	0.017 (2)	0.0103 (16)	0.026 (2)	0.0009 (15)	−0.0007 (19)	−0.0050 (17)
C9	0.017 (2)	0.025 (2)	0.023 (2)	−0.0019 (18)	−0.0044 (18)	0.0021 (18)
O6	0.0114 (14)	0.0188 (13)	0.0352 (16)	0.0000 (12)	−0.0021 (13)	0.0088 (13)
O7	0.0177 (15)	0.0116 (12)	0.0437 (18)	−0.0019 (11)	0.0034 (14)	0.0005 (14)
O8	0.0077 (14)	0.0187 (12)	0.0383 (18)	−0.0011 (11)	0.0011 (12)	0.0039 (13)
O1W	0.109 (4)	0.097 (3)	0.046 (3)	−0.014 (3)	0.024 (3)	0.002 (2)
O2W	0.062 (3)	0.113 (4)	0.064 (3)	0.018 (3)	−0.004 (2)	0.017 (3)
O3W	0.127 (5)	0.084 (3)	0.079 (3)	0.007 (3)	0.011 (3)	−0.003 (3)

Dy1—O4	2.334 (3)	C6—C5	1.518 (6)
Dy1—O7ⁱ	2.337 (3)	C6—H6A	0.9700
Dy1—O5	2.342 (3)	C6—H6B	0.9700
Dy1—O6	2.354 (3)	C5—H5A	0.9700
Dy1—O8ⁱⁱ	2.373 (3)	C5—H5B	0.9700
Dy1—O2	2.387 (3)	O1—H1	0.8200
Dy1—N2	2.617 (3)	C8—O7	1.248 (4)
Dy1—N1	2.636 (3)	C8—O5	1.260 (4)
N1—C3	1.473 (4)	C8—C7	1.513 (5)
N1—C7	1.477 (5)	C7—H7A	0.9700
N1—C5	1.487 (5)	C7—H7B	0.9700
N2—C1	1.482 (5)	C10—O8	1.243 (4)
N2—C9	1.485 (5)	C10—O6	1.265 (4)
N2—C6	1.488 (5)	C10—C9	1.524 (5)
C4—O4	1.257 (5)	C9—H9A	0.9700
C4—O3	1.254 (5)	C9—H9B	0.9700
C4—C3	1.521 (5)	O7—Dy1ⁱⁱⁱ	2.337 (3)
C3—H3A	0.9700	O8—Dy1^iv	2.373 (2)
C3—H3B	0.9700	O1W—H2W	0.8462
C2—O2	1.231 (5)	O1W—H1W	0.8429
C2—O1	1.282 (5)	O2W—H3W	0.8322
C2—C1	1.496 (5)	O2W—H4W	0.8371
C1—H1A	0.9700	O3W—H6W	0.8515
C1—H1B	0.9700	O3W—H5W	0.8763

O4—Dy1—O7ⁱ	89.53 (9)	O2—C2—O1	124.0 (4)
O4—Dy1—O5	97.72 (10)	O2—C2—C1	121.2 (4)
O7ⁱ—Dy1—O5	150.23 (9)	O1—C2—C1	114.8 (4)
O4—Dy1—O6	88.56 (10)	N2—C1—C2	110.6 (3)
O7ⁱ—Dy1—O6	74.80 (9)	N2—C1—H1A	109.5
O5—Dy1—O6	133.90 (9)	C2—C1—H1A	109.5
O4—Dy1—O8ⁱⁱ	80.61 (10)	N2—C1—H1B	109.5
O7ⁱ—Dy1—O8ⁱⁱ	76.54 (8)	C2—C1—H1B	109.5
O5—Dy1—O8ⁱⁱ	76.25 (9)	H1A—C1—H1B	108.1
O6—Dy1—O8ⁱⁱ	149.38 (9)	N2—C6—C5	112.4 (3)
O4—Dy1—O2	162.25 (10)	N2—C6—H6A	109.1
O7ⁱ—Dy1—O2	79.94 (10)	C5—C6—H6A	109.1
O5—Dy1—O2	85.01 (10)	N2—C6—H6B	109.1
O6—Dy1—O2	102.22 (10)	C5—C6—H6B	109.1
O8ⁱⁱ—Dy1—O2	83.05 (9)	H6A—C6—H6B	107.9
O4—Dy1—N2	132.53 (9)	N1—C5—C6	112.1 (3)
O7ⁱ—Dy1—N2	119.38 (9)	N1—C5—H5A	109.2
O5—Dy1—N2	75.81 (10)	C6—C5—H5A	109.2
O6—Dy1—N2	66.98 (9)	N1—C5—H5B	109.2
O8ⁱⁱ—Dy1—N2	138.99 (9)	C6—C5—H5B	109.2
O2—Dy1—N2	65.17 (9)	H5A—C5—H5B	107.9
O4—Dy1—N1	65.28 (9)	C2—O2—Dy1	123.5 (3)
O7ⁱ—Dy1—N1	140.53 (9)	C4—O4—Dy1	125.5 (3)
O5—Dy1—N1	67.10 (9)	C2—O1—H1	109.5
O6—Dy1—N1	74.70 (10)	O7—C8—O5	123.1 (4)
O8ⁱⁱ—Dy1—N1	124.40 (9)	O7—C8—C7	119.0 (3)
O2—Dy1—N1	130.94 (9)	O5—C8—C7	117.8 (3)
N2—Dy1—N1	69.15 (9)	N1—C7—C8	113.4 (3)
C3—N1—C7	109.2 (3)	N1—C7—H7A	108.9
C3—N1—C5	111.5 (3)	C8—C7—H7A	108.9
C7—N1—C5	110.7 (3)	N1—C7—H7B	108.9
C3—N1—Dy1	108.2 (2)	C8—C7—H7B	108.9
C7—N1—Dy1	107.3 (2)	H7A—C7—H7B	107.7
C5—N1—Dy1	109.8 (2)	C8—O5—Dy1	125.7 (2)
C1—N2—C9	109.0 (3)	O8—C10—O6	123.8 (4)
C1—N2—C6	110.6 (3)	O8—C10—C9	119.4 (3)
C9—N2—C6	109.9 (3)	O6—C10—C9	116.7 (3)
C1—N2—Dy1	109.4 (2)	N2—C9—C10	112.5 (3)
C9—N2—Dy1	106.7 (2)	N2—C9—H9A	109.1
C6—N2—Dy1	111.0 (2)	C10—C9—H9A	109.1
O4—C4—O3	123.9 (4)	N2—C9—H9B	109.1
O4—C4—C3	118.5 (4)	C10—C9—H9B	109.1
O3—C4—C3	117.6 (4)	H9A—C9—H9B	107.8
N1—C3—C4	110.9 (3)	C10—O6—Dy1	125.4 (2)
N1—C3—H3A	109.5	C8—O7—Dy1ⁱⁱⁱ	147.0 (2)
C4—C3—H3A	109.5	C10—O8—Dy1^iv	144.6 (2)
N1—C3—H3B	109.5	H2W—O1W—H1W	110.2
C4—C3—H3B	109.5	H3W—O2W—H4W	111.4
H3A—C3—H3B	108.1	H6W—O3W—H5W	106.7

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···O3^v	0.82	1.69	2.504 (5)	172
O1W—H2W···O6^vi	0.85	2.17	2.920 (5)	148
O1W—H1W···O3^vii	0.84	2.10	2.925 (5)	165
O2W—H3W···O3W^viii	0.83	2.04	2.813 (6)	154
O2W—H4W···O1W^ix	0.84	2.09	2.844 (6)	150
O3W—H6W···O2ⁱⁱⁱ	0.85	2.56	3.141 (5)	127

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1⋯O3ⁱ	0.82	1.69	2.504 (5)	172
O1W—H2W⋯O6ⁱⁱ	0.85	2.17	2.920 (5)	148
O1W—H1W⋯O3ⁱⁱⁱ	0.84	2.10	2.925 (5)	165
O2W—H3W⋯O3W^iv	0.83	2.04	2.813 (6)	154
O2W—H4W⋯O1W^v	0.84	2.09	2.844 (6)	150
O3W—H6W⋯O2^vi	0.85	2.56	3.141 (5)	127

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

2 in total

1. Magnetism of lanthanides in molecular materials with transition-metal ions and organic radicals.

Authors: Cristiano Benelli; Dante Gatteschi
Journal: Chem Rev Date: 2002-06 Impact factor: 60.622

2. A short history of SHELX.

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

2 in total