Literature DB >> 21201061

Poly[tris-(μ(3)-5-amino-isophthalato)diaqua-dicerium(III)].

Hui-Jie Ma¹, Yu-Hua Fan, Qiang Wang, Cai-Feng Bi, Dong-Mei Zhang.

Abstract

In the title complex, [Ce(2)(C(8)H(5)NO(4))(3)(H(2)O)(2)](n), each Ce ion is in nine-coordinated environment. Eight O atoms from six ligands participate in coordination, in addition to one O atom from a water mol-ecule. Both carboxyl-ate groups from the ligands chelate the Ce atoms, forming two four-membered rings. The 5-amino-isophthalate ligands also bridge the Ce centers, forming a two-dimensional network, and O-H⋯O and N-H⋯O hydrogen bonds complete the structure.

Entities: Chemical Disease Gene

Year: 2008 PMID： 21201061 PMCID： PMC2959393 DOI： 10.1107/S160053680803033X

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

Related literature

For general background, see: Rzaczynska & Belsky (1994 ▶); Daiguebonne et al. (2000 ▶); Wu et al. (2002a ▶,b ▶); Liao et al. (2004 ▶).

Experimental

Crystal data

[Ce2(C8H5NO4)3(H2O)2] M = 853.66 Orthorhombic, a = 12.2360 (7) Å b = 8.0600 (5) Å c = 25.6700 (15) Å V = 2531.6 (3) Å3 Z = 4 Mo Kα radiation μ = 3.63 mm−1 T = 298 (2) K 0.21 × 0.20 × 0.19 mm

Data collection

Siemens SMART CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.516, T max = 0.545 (expected range = 0.474–0.501) 11818 measured reflections 2233 independent reflections 2001 reflections with I > 2σ(I) R int = 0.034

Refinement

R[F 2 > 2σ(F 2)] = 0.019 wR(F 2) = 0.045 S = 1.04 2233 reflections 196 parameters 2 restraints H-atom parameters constrained Δρmax = 0.45 e Å−3 Δρmin = −0.64 e Å−3 Data collection: SMART (Siemens, 1996 ▶); cell refinement: SAINT (Siemens, 1996 ▶); 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/S160053680803033X/bq2095sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S160053680803033X/bq2095Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Ce₂(C₈H₅NO₄)₃(H₂O)₂]	F(000) = 1648
M_r = 853.66	D_x = 2.240 Mg m⁻³
Orthorhombic, Pbcn	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2n 2ab	Cell parameters from 3043 reflections
a = 12.2360 (7) Å	θ = 2.3–28.4°
b = 8.0600 (5) Å	µ = 3.63 mm⁻¹
c = 25.6700 (15) Å	T = 298 K
V = 2531.6 (3) Å³	Block, brown
Z = 4	0.21 × 0.20 × 0.19 mm

Siemens SMART CCD area-detector diffractometer	2233 independent reflections
Radiation source: fine-focus sealed tube	2001 reflections with I > 2σ(I)
graphite	R_int = 0.034
φ and ω scans	θ_max = 25.0°, θ_min = 2.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −14→13
T_min = 0.516, T_max = 0.545	k = −9→9
11818 measured reflections	l = −30→23

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)] = 0.019	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.045	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0208P)² + 2.5416P] where P = (F_o² + 2F_c²)/3
2233 reflections	(Δ/σ)_max = 0.001
196 parameters	Δρ_max = 0.45 e Å⁻³
2 restraints	Δρ_min = −0.64 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.

	x	y	z	U_iso*/U_eq
Ce1	0.694451 (12)	0.038178 (18)	0.094984 (6)	0.01318 (7)
H1A	0.4903	−0.1228	0.0487	0.016*
H1B	0.4671	−0.1140	0.0998	0.016*
N1	0.1463 (2)	0.4699 (3)	0.15158 (11)	0.0302 (7)
H1C	0.1531	0.4128	0.1797	0.036*
H1D	0.1042	0.5534	0.1571	0.036*
N2	0.5000	−0.7310 (4)	0.2500	0.0418 (11)
H2A	0.5462	−0.7843	0.2311	0.050*
O1	0.53914 (15)	0.2297 (2)	0.12641 (8)	0.0227 (5)
O2	0.62001 (17)	0.4491 (3)	0.09148 (8)	0.0250 (5)
O3	0.38087 (15)	0.8402 (2)	−0.01169 (8)	0.0220 (5)
O4	0.77549 (15)	0.2778 (2)	0.03332 (8)	0.0204 (4)
O5	0.63242 (18)	−0.0423 (2)	0.18383 (9)	0.0282 (5)
O6	0.70692 (16)	−0.2648 (2)	0.15024 (8)	0.0232 (5)
O1W	0.51934 (16)	−0.1043 (3)	0.07824 (9)	0.0280 (5)
C1	0.4286 (2)	0.4564 (3)	0.09890 (11)	0.0159 (6)
C2	0.4177 (2)	0.5614 (3)	0.05642 (12)	0.0177 (6)
H2	0.4786	0.5885	0.0365	0.021*
C3	0.3163 (2)	0.6262 (3)	0.04351 (11)	0.0174 (6)
C4	0.2262 (2)	0.5922 (4)	0.07468 (12)	0.0179 (6)
H4	0.1576	0.6316	0.0652	0.021*
C5	0.2384 (2)	0.4998 (3)	0.11991 (12)	0.0189 (6)
C6	0.3393 (2)	0.4281 (3)	0.13138 (12)	0.0182 (6)
H6	0.3469	0.3613	0.1607	0.022*
C7	0.5365 (2)	0.3728 (3)	0.10682 (11)	0.0164 (6)
C8	0.3065 (2)	0.7357 (3)	−0.00284 (12)	0.0173 (6)
C9	0.5727 (2)	−0.2982 (3)	0.21853 (11)	0.0171 (6)
C10	0.5748 (2)	−0.4714 (3)	0.21935 (12)	0.0205 (6)
H10	0.6261	−0.5283	0.1995	0.025*
C11	0.5000	−0.5599 (5)	0.2500	0.0212 (9)
C12	0.5000	−0.2132 (5)	0.2500	0.0176 (9)
H12	0.5000	−0.0978	0.2500	0.021*
C13	0.6425 (2)	−0.1977 (3)	0.18270 (11)	0.0165 (6)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ce1	0.01069 (10)	0.01242 (10)	0.01642 (12)	−0.00009 (6)	−0.00036 (6)	0.00135 (6)
N1	0.0194 (14)	0.0396 (16)	0.0314 (18)	0.0059 (12)	0.0102 (12)	0.0138 (13)
N2	0.070 (3)	0.0152 (19)	0.040 (3)	0.000	0.030 (2)	0.000
O1	0.0200 (10)	0.0169 (10)	0.0311 (13)	0.0053 (8)	0.0002 (9)	0.0026 (9)
O2	0.0132 (11)	0.0306 (12)	0.0314 (14)	−0.0012 (9)	0.0007 (9)	0.0030 (10)
O3	0.0243 (11)	0.0195 (11)	0.0224 (12)	−0.0062 (9)	−0.0041 (9)	0.0065 (9)
O4	0.0179 (10)	0.0227 (11)	0.0205 (11)	−0.0003 (8)	−0.0036 (9)	0.0016 (9)
O5	0.0395 (13)	0.0170 (11)	0.0280 (13)	0.0005 (9)	0.0133 (11)	0.0036 (9)
O6	0.0235 (11)	0.0225 (9)	0.0236 (12)	0.0025 (9)	0.0101 (9)	0.0048 (8)
O1W	0.0187 (11)	0.0323 (12)	0.0329 (13)	−0.0066 (10)	0.0010 (10)	−0.0076 (11)
C1	0.0136 (14)	0.0137 (14)	0.0204 (16)	−0.0002 (11)	−0.0011 (11)	−0.0010 (12)
C2	0.0151 (14)	0.0154 (14)	0.0226 (16)	−0.0004 (11)	0.0026 (13)	−0.0014 (12)
C3	0.0194 (15)	0.0126 (14)	0.0201 (16)	−0.0010 (11)	−0.0020 (12)	−0.0016 (12)
C4	0.0135 (13)	0.0178 (14)	0.0223 (16)	0.0017 (12)	−0.0013 (12)	−0.0024 (13)
C5	0.0140 (14)	0.0195 (14)	0.0233 (17)	0.0003 (12)	0.0011 (13)	0.0001 (13)
C6	0.0155 (14)	0.0168 (14)	0.0225 (17)	0.0002 (11)	−0.0007 (13)	0.0032 (12)
C7	0.0132 (14)	0.0191 (15)	0.0168 (15)	−0.0005 (12)	−0.0013 (12)	−0.0024 (13)
C8	0.0186 (14)	0.0156 (14)	0.0176 (16)	0.0047 (12)	−0.0009 (12)	−0.0033 (12)
C9	0.0185 (14)	0.0173 (14)	0.0155 (15)	−0.0003 (11)	0.0017 (12)	0.0005 (12)
C10	0.0255 (16)	0.0184 (14)	0.0176 (16)	0.0040 (12)	0.0050 (14)	−0.0020 (13)
C11	0.032 (2)	0.015 (2)	0.016 (2)	0.000	0.0031 (19)	0.000
C12	0.021 (2)	0.016 (2)	0.016 (2)	0.000	0.0012 (17)	0.000
C13	0.0162 (14)	0.0189 (14)	0.0144 (15)	−0.0002 (12)	0.0001 (12)	−0.0004 (12)

Ce1—O2ⁱ	2.383 (2)	O6—Ce1ⁱ	2.448 (2)
Ce1—O6ⁱⁱ	2.448 (2)	O1W—H1A	0.8500
Ce1—O1W	2.469 (2)	O1W—H1B	0.8500
Ce1—O5	2.490 (2)	C1—C2	1.387 (4)
Ce1—O3ⁱⁱⁱ	2.5263 (19)	C1—C6	1.393 (4)
Ce1—O1	2.5779 (19)	C1—C7	1.496 (4)
Ce1—O4ⁱ	2.654 (2)	C2—C3	1.387 (4)
Ce1—O4	2.6870 (19)	C2—H2	0.9300
Ce1—O6	2.828 (2)	C3—C4	1.389 (4)
Ce1—C8ⁱⁱⁱ	2.986 (3)	C3—C8	1.486 (4)
N1—C5	1.410 (4)	C4—C5	1.387 (4)
N1—H1C	0.8600	C4—H4	0.9300
N1—H1D	0.8599	C5—C6	1.395 (4)
N2—C11	1.379 (5)	C6—H6	0.9300
N2—H2A	0.8600	C8—O4ⁱⁱⁱ	1.276 (3)
O1—C7	1.258 (3)	C8—Ce1ⁱⁱⁱ	2.986 (3)
O2—C7	1.256 (3)	C9—C12	1.384 (3)
O2—Ce1ⁱⁱ	2.383 (2)	C9—C10	1.396 (4)
O3—C8	1.261 (3)	C9—C13	1.494 (4)
O3—Ce1ⁱⁱⁱ	2.5263 (19)	C10—C11	1.402 (3)
O4—C8ⁱⁱⁱ	1.276 (3)	C10—H10	0.9300
O4—Ce1ⁱⁱ	2.654 (2)	C11—C10^iv	1.402 (3)
O5—C13	1.259 (3)	C12—C9^iv	1.384 (3)
O6—C13	1.268 (3)	C12—H12	0.9300

O2ⁱ—Ce1—O6ⁱⁱ	75.39 (7)	C8ⁱⁱⁱ—O4—Ce1ⁱⁱ	122.81 (17)
O2ⁱ—Ce1—O1W	132.85 (7)	C8ⁱⁱⁱ—O4—Ce1	90.56 (16)
O6ⁱⁱ—Ce1—O1W	146.17 (7)	Ce1ⁱⁱ—O4—Ce1	105.55 (7)
O2ⁱ—Ce1—O5	104.28 (7)	C13—O5—Ce1	102.02 (18)
O6ⁱⁱ—Ce1—O5	77.79 (7)	C13—O6—Ce1ⁱ	164.58 (18)
O1W—Ce1—O5	76.92 (7)	C13—O6—Ce1	85.86 (16)
O2ⁱ—Ce1—O3ⁱⁱⁱ	115.63 (7)	Ce1ⁱ—O6—Ce1	107.23 (7)
O6ⁱⁱ—Ce1—O3ⁱⁱⁱ	114.74 (6)	Ce1—O1W—H1A	126.9
O1W—Ce1—O3ⁱⁱⁱ	73.53 (7)	Ce1—O1W—H1B	125.6
O5—Ce1—O3ⁱⁱⁱ	139.93 (7)	H1A—O1W—H1B	104.5
O2ⁱ—Ce1—O1	153.47 (7)	C2—C1—C6	119.7 (3)
O6ⁱⁱ—Ce1—O1	78.08 (6)	C2—C1—C7	117.8 (3)
O1W—Ce1—O1	72.14 (7)	C6—C1—C7	122.5 (2)
O5—Ce1—O1	69.18 (7)	C3—C2—C1	120.2 (3)
O3ⁱⁱⁱ—Ce1—O1	76.33 (7)	C3—C2—H2	119.9
O2ⁱ—Ce1—O4ⁱ	66.87 (7)	C1—C2—H2	119.9
O6ⁱⁱ—Ce1—O4ⁱ	142.22 (6)	C2—C3—C4	119.9 (3)
O1W—Ce1—O4ⁱ	69.43 (6)	C2—C3—C8	119.1 (2)
O5—Ce1—O4ⁱ	112.50 (6)	C4—C3—C8	121.0 (2)
O3ⁱⁱⁱ—Ce1—O4ⁱ	81.52 (6)	C5—C4—C3	120.2 (3)
O1—Ce1—O4ⁱ	139.66 (6)	C5—C4—H4	119.9
O2ⁱ—Ce1—O4	80.95 (6)	C3—C4—H4	119.9
O6ⁱⁱ—Ce1—O4	72.12 (7)	C4—C5—C6	119.6 (3)
O1W—Ce1—O4	123.51 (7)	C4—C5—N1	119.3 (3)
O5—Ce1—O4	147.09 (6)	C6—C5—N1	121.0 (3)
O3ⁱⁱⁱ—Ce1—O4	49.99 (6)	C1—C6—C5	120.0 (3)
O1—Ce1—O4	91.49 (6)	C1—C6—H6	120.0
O4ⁱ—Ce1—O4	99.54 (6)	C5—C6—H6	120.0
O2ⁱ—Ce1—O6	72.98 (6)	O2—C7—O1	123.6 (3)
O6ⁱⁱ—Ce1—O6	104.06 (7)	O2—C7—C1	117.1 (2)
O1W—Ce1—O6	74.48 (7)	O1—C7—C1	119.3 (2)
O5—Ce1—O6	48.09 (6)	O3—C8—O4ⁱⁱⁱ	120.9 (3)
O3ⁱⁱⁱ—Ce1—O6	141.19 (6)	O3—C8—C3	118.9 (2)
O1—Ce1—O6	113.57 (6)	O4ⁱⁱⁱ—C8—C3	120.2 (2)
O4ⁱ—Ce1—O6	66.99 (6)	O3—C8—Ce1ⁱⁱⁱ	56.79 (15)
O4—Ce1—O6	153.67 (5)	O4ⁱⁱⁱ—C8—Ce1ⁱⁱⁱ	64.13 (15)
O2ⁱ—Ce1—C8ⁱⁱⁱ	99.07 (7)	C3—C8—Ce1ⁱⁱⁱ	175.47 (19)
O6ⁱⁱ—Ce1—C8ⁱⁱⁱ	93.72 (7)	C12—C9—C10	119.9 (3)
O1W—Ce1—C8ⁱⁱⁱ	98.21 (7)	C12—C9—C13	117.3 (3)
O5—Ce1—C8ⁱⁱⁱ	152.07 (7)	C10—C9—C13	122.8 (3)
O3ⁱⁱⁱ—Ce1—C8ⁱⁱⁱ	24.68 (7)	C9—C10—C11	120.4 (3)
O1—Ce1—C8ⁱⁱⁱ	83.09 (7)	C9—C10—H10	119.8
O4ⁱ—Ce1—C8ⁱⁱⁱ	90.61 (7)	C11—C10—H10	119.8
O4—Ce1—C8ⁱⁱⁱ	25.31 (6)	N2—C11—C10^iv	120.60 (18)
O6—Ce1—C8ⁱⁱⁱ	157.60 (7)	N2—C11—C10	120.60 (18)
C5—N1—H1C	119.9	C10^iv—C11—C10	118.8 (4)
C5—N1—H1D	116.1	C9^iv—C12—C9	120.6 (4)
H1C—N1—H1D	109.7	C9^iv—C12—H12	119.7
C11—N2—H2A	120.0	C9—C12—H12	119.7
C7—O1—Ce1	116.27 (17)	O5—C13—O6	120.0 (3)
C7—O2—Ce1ⁱⁱ	155.62 (19)	O5—C13—C9	118.0 (2)
C8—O3—Ce1ⁱⁱⁱ	98.53 (17)	O6—C13—C9	121.9 (2)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2A···O5^v	0.86	2.63	3.436 (3)	157.
N1—H1D···O1^vi	0.86	2.39	3.154 (3)	148.
O1W—H1A···O3^v	0.85	2.07	2.898 (3)	165.

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H2A⋯O5ⁱ	0.86	2.63	3.436 (3)	157
N1—H1D⋯O1ⁱⁱ	0.86	2.39	3.154 (3)	148
O1W—H1A⋯O3ⁱ	0.85	2.07	2.898 (3)	165

Symmetry codes: (i) ; (ii) .

3 in total

1. Hybrid coordination polymer constructed from beta-octamolybdates linked by quinoxaline and its oxidized product benzimidazole coordinated to binuclear copper(I) fragments.

Authors: Chuan-De Wu; Can-Zhong Lu; Hong-Hui Zhuang; Jin-Shun Huang
Journal: Inorg Chem Date: 2002-11-04 Impact factor: 5.165

2. Poly[[copper(II)-di-mu-5-aminoisophthalato(1-)-kappa4N:O] monohydrate].

Authors: Qiu-Xia Liao; Zhao-Ji Li; Jian Zhang; Yao Kang; Yu-Mei Dai; Yuan-Gen Yao
Journal: Acta Crystallogr C Date: 2004-09-25 Impact factor: 1.172

3. A short history of SHELX.

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

3 in total