Literature DB >> 21201257

catena-Poly[[tetra-aqua-cobalt(II)]-μ-2,2'-dihydroxy-5,5'-diazenediyldibenzoato].

Yu-Hui Tan, Yin-Bao Li, Fa-Ming Ji, Ting-Ting Xiong, Li-Bin Xia.

Abstract

In the title compound, [Co(C(14)H(8)N(2)O(6))(H(2)O)(4)](n), each 5,5'-diazenediylbis(2-hydroxy-benzoato) ligand acts as a dicarboxyl-ate bridge, leading to the formation of polymeric chains running in the [10] direction. The Co atom is hexa-coordinated in a distorted octa-hedral geometry by six O atoms [Co-O = 2.039 (4)-2.115 (4) Å] from two ligands and four water mol-ecules. Inter-molecular O-H⋯O and O-H⋯N hydrogen bonds build up a three-dimensional supra-molecular structure.

Entities: CellLine Chemical Disease Species

Year: 2008 PMID： 21201257 PMCID： PMC2960221 DOI： 10.1107/S1600536807067827

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

Related literature

For related literature, see: Klotz (2005 ▶); Tang, Tan & Cao (2007 ▶); Tang, Tan, Chen et al. (2007 ▶); Tang, Yang et al. (2007 ▶); Riordan & Blair (1979 ▶).

Experimental

Crystal data

[Co(C14H8N2O6)(H2O)4] M = 431.22 Monoclinic, a = 9.5152 (14) Å b = 11.2452 (17) Å c = 16.194 (2) Å β = 106.687 (2)° V = 1659.8 (4) Å3 Z = 4 Mo Kα radiation μ = 1.09 mm−1 T = 296 (2) K 0.10 × 0.08 × 0.08 mm

Data collection

Bruker SMART APEX CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T min = 0.898, T max = 0.917 11094 measured reflections 3427 independent reflections 1976 reflections with I > 2σ(I) R int = 0.062

Refinement

R[F 2 > 2σ(F 2)] = 0.049 wR(F 2) = 0.133 S = 0.94 3427 reflections 246 parameters H-atom parameters constrained Δρmax = 0.50 e Å−3 Δρmin = −0.44 e Å−3 Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: PLATON (Spek, 2003 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807067827/dn2293sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536807067827/dn2293Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Co(C₁₄H₈N₂O₆)(H₂O)₄]	F₀₀₀ = 884
M_r = 431.22	D_x = 1.726 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 935 reflections
a = 9.5152 (14) Å	θ = 2.2–26º
b = 11.2452 (17) Å	µ = 1.10 mm⁻¹
c = 16.194 (2) Å	T = 296 (2) K
β = 106.687 (2)º	Block, red
V = 1659.8 (4) Å³	0.10 × 0.08 × 0.08 mm
Z = 4

Bruker SMART APEX CCD area-detector diffractometer	3427 independent reflections
Radiation source: fine-focus sealed tube	1976 reflections with I > 2σ(I)
Monochromator: graphite	R_int = 0.062
T = 296(2) K	θ_max = 26.4º
φ and ω scans	θ_min = 1.8º
Absorption correction: multi-scan(SADABS; Bruker, 2000)	h = −11→11
T_min = 0.898, T_max = 0.918	k = −14→14
11094 measured reflections	l = −19→20

Refinement on F²	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F² > 2σ(F²)] = 0.049	w = 1/[σ²(F_o²) + (0.0717P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.133	(Δ/σ)_max = 0.001
S = 0.94	Δρ_max = 0.50 e Å⁻³
3427 reflections	Δρ_min = −0.44 e Å⁻³
246 parameters	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0050 (11)
Secondary atom site location: difference Fourier map

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
Co1	0.71433 (7)	0.14001 (5)	0.21254 (4)	0.0333 (2)
O1W	0.8824 (4)	0.2527 (3)	0.2134 (2)	0.0515 (9)
H1WA	0.9251	0.3002	0.2506	0.077*
H1WB	0.8799	0.2780	0.1654	0.077*
O2W	0.6621 (4)	0.2503 (3)	0.3053 (2)	0.0537 (10)
H2WA	0.5912	0.2842	0.2726	0.080*
H2WB	0.6352	0.2127	0.3415	0.080*
O3W	0.5405 (4)	0.0277 (3)	0.2068 (2)	0.0575 (10)
H3WA	0.5494	−0.0263	0.2418	0.086*
H3WB	0.5144	0.0028	0.1579	0.086*
O4W	0.8418 (4)	0.0398 (3)	0.31539 (19)	0.0455 (9)
H4WA	0.8933	0.0663	0.3610	0.068*
H4WB	0.8900	−0.0006	0.2912	0.068*
N2	0.0915 (4)	0.6415 (3)	0.0012 (2)	0.0366 (9)
N1	0.1224 (4)	0.6059 (3)	−0.0651 (2)	0.0374 (10)
O1	0.5775 (4)	0.2345 (3)	0.10743 (19)	0.0402 (8)
O2	0.4732 (4)	0.3607 (3)	0.1776 (2)	0.0542 (10)
O3	0.5168 (4)	0.2395 (3)	−0.0547 (2)	0.0609 (11)
H3A	0.5587	0.2174	−0.0055	0.091*
O4	−0.3150 (4)	1.0087 (3)	−0.0450 (2)	0.0533 (10)
H4A	−0.3126	1.0395	0.0012	0.080*
O5	−0.2290 (4)	1.0400 (3)	0.1171 (2)	0.0455 (9)
O6	−0.0537 (4)	0.9267 (3)	0.2009 (2)	0.0637 (12)
C1	0.4906 (5)	0.3199 (4)	0.1097 (3)	0.0358 (11)
C2	0.4027 (5)	0.3698 (4)	0.0249 (3)	0.0326 (10)
C3	0.4191 (6)	0.3262 (4)	−0.0520 (3)	0.0399 (12)
C4	0.3349 (6)	0.3724 (4)	−0.1303 (3)	0.0523 (15)
H4	0.3427	0.3408	−0.1819	0.063*
C5	0.2420 (5)	0.4632 (4)	−0.1309 (3)	0.0441 (13)
H5	0.1885	0.4954	−0.1835	0.053*
C6	0.2240 (5)	0.5101 (4)	−0.0547 (3)	0.0346 (11)
C7	0.3054 (5)	0.4617 (4)	0.0228 (3)	0.0356 (11)
H7	0.2944	0.4914	0.0742	0.043*
C8	−0.0120 (5)	0.7371 (4)	−0.0142 (3)	0.0348 (11)
C9	−0.1058 (5)	0.7662 (4)	−0.0956 (3)	0.0414 (12)
H9	−0.1024	0.7229	−0.1439	0.050*
C10	−0.2027 (6)	0.8587 (4)	−0.1037 (3)	0.0446 (12)
H10	−0.2621	0.8798	−0.1580	0.054*
C11	−0.2134 (5)	0.9212 (4)	−0.0320 (3)	0.0386 (12)
C12	−0.1231 (5)	0.8923 (4)	0.0500 (3)	0.0351 (11)
C13	−0.0236 (6)	0.8005 (4)	0.0566 (3)	0.0419 (12)
H13	0.0377	0.7808	0.1108	0.050*
C14	−0.1338 (5)	0.9566 (4)	0.1286 (3)	0.0403 (12)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.0379 (4)	0.0295 (3)	0.0312 (3)	0.0035 (3)	0.0078 (3)	0.0014 (3)
O1W	0.060 (2)	0.055 (2)	0.0364 (19)	−0.0171 (19)	0.0088 (17)	−0.0010 (17)
O2W	0.061 (3)	0.060 (2)	0.040 (2)	0.023 (2)	0.0160 (18)	0.0057 (17)
O3W	0.054 (2)	0.061 (2)	0.047 (2)	−0.015 (2)	−0.0007 (17)	0.0173 (19)
O4W	0.054 (2)	0.044 (2)	0.0359 (18)	0.0113 (17)	0.0085 (16)	−0.0011 (15)
N2	0.042 (2)	0.0304 (19)	0.035 (2)	0.0096 (19)	0.0072 (18)	0.0031 (19)
N1	0.039 (3)	0.036 (2)	0.038 (2)	0.0101 (18)	0.0122 (18)	0.0017 (17)
O1	0.048 (2)	0.0362 (18)	0.0361 (18)	0.0122 (16)	0.0121 (16)	0.0027 (15)
O2	0.070 (3)	0.055 (2)	0.0340 (18)	0.028 (2)	0.0094 (18)	−0.0057 (17)
O3	0.080 (3)	0.062 (2)	0.042 (2)	0.045 (2)	0.019 (2)	0.0083 (18)
O4	0.061 (2)	0.052 (2)	0.0403 (19)	0.0296 (19)	0.0029 (17)	−0.0053 (17)
O5	0.054 (2)	0.0407 (19)	0.0385 (19)	0.0189 (18)	0.0075 (16)	−0.0045 (16)
O6	0.079 (3)	0.067 (3)	0.035 (2)	0.043 (2)	0.0014 (19)	−0.0079 (19)
C1	0.039 (3)	0.030 (2)	0.037 (3)	0.004 (2)	0.008 (2)	0.004 (2)
C2	0.036 (3)	0.031 (2)	0.030 (2)	0.002 (2)	0.009 (2)	0.003 (2)
C3	0.043 (3)	0.035 (3)	0.045 (3)	0.014 (2)	0.018 (2)	0.000 (2)
C4	0.071 (4)	0.052 (3)	0.033 (3)	0.025 (3)	0.014 (3)	0.003 (3)
C5	0.050 (3)	0.045 (3)	0.035 (3)	0.017 (3)	0.008 (2)	0.006 (2)
C6	0.041 (3)	0.028 (2)	0.035 (3)	0.007 (2)	0.012 (2)	0.001 (2)
C7	0.043 (3)	0.031 (2)	0.037 (3)	0.003 (2)	0.017 (2)	0.004 (2)
C8	0.036 (3)	0.030 (2)	0.039 (3)	0.010 (2)	0.012 (2)	0.001 (2)
C9	0.045 (3)	0.047 (3)	0.031 (3)	0.010 (2)	0.009 (2)	−0.005 (2)
C10	0.055 (3)	0.048 (3)	0.026 (2)	0.015 (3)	0.004 (2)	0.004 (2)
C11	0.041 (3)	0.033 (2)	0.039 (3)	0.006 (2)	0.006 (2)	0.001 (2)
C12	0.037 (3)	0.032 (3)	0.033 (2)	0.005 (2)	0.004 (2)	−0.0027 (19)
C13	0.050 (3)	0.037 (3)	0.034 (3)	0.014 (2)	0.003 (2)	−0.002 (2)
C14	0.038 (3)	0.039 (3)	0.038 (3)	0.012 (2)	0.003 (2)	−0.002 (2)

Co1—O1W	2.037 (3)	O5—C14	1.280 (5)
Co1—O3W	2.062 (3)	O5—Co1ⁱⁱ	2.103 (3)
Co1—O4W	2.087 (3)	O6—C14	1.245 (5)
Co1—O5ⁱ	2.103 (3)	C1—C2	1.497 (6)
Co1—O1	2.110 (3)	C2—C7	1.381 (6)
Co1—O2W	2.115 (3)	C2—C3	1.388 (6)
O1W—H1WA	0.8195	C3—C4	1.391 (7)
O1W—H1WB	0.8219	C4—C5	1.349 (6)
O2W—H2WA	0.8220	C4—H4	0.9300
O2W—H2WB	0.8212	C5—C6	1.397 (6)
O3W—H3WA	0.8183	C5—H5	0.9300
O3W—H3WB	0.8089	C6—C7	1.383 (6)
O4W—H4WA	0.8158	C7—H7	0.9300
O4W—H4WB	0.8205	C8—C13	1.383 (6)
N2—N1	1.257 (5)	C8—C9	1.401 (6)
N2—C8	1.430 (6)	C9—C10	1.371 (6)
N1—C6	1.426 (6)	C9—H9	0.9300
O1—C1	1.275 (5)	C10—C11	1.385 (6)
O2—C1	1.245 (5)	C10—H10	0.9300
O3—C3	1.357 (5)	C11—C12	1.398 (6)
O3—H3A	0.8200	C12—C13	1.383 (6)
O4—C11	1.353 (5)	C12—C14	1.493 (6)
O4—H4A	0.8200	C13—H13	0.9300

O1W—Co1—O3W	177.81 (14)	C3—C2—C1	120.9 (4)
O1W—Co1—O4W	93.15 (13)	O3—C3—C2	122.5 (4)
O3W—Co1—O4W	88.88 (13)	O3—C3—C4	117.4 (4)
O1W—Co1—O5ⁱ	88.37 (14)	C2—C3—C4	120.2 (4)
O3W—Co1—O5ⁱ	90.63 (15)	C5—C4—C3	119.6 (4)
O4W—Co1—O5ⁱ	94.86 (12)	C5—C4—H4	120.2
O1W—Co1—O1	89.64 (14)	C3—C4—H4	120.2
O3W—Co1—O1	88.33 (13)	C4—C5—C6	121.7 (4)
O4W—Co1—O1	177.14 (13)	C4—C5—H5	119.2
O5ⁱ—Co1—O1	84.59 (12)	C6—C5—H5	119.2
O1W—Co1—O2W	88.52 (15)	C7—C6—C5	118.3 (4)
O3W—Co1—O2W	92.42 (15)	C7—C6—N1	126.0 (4)
O4W—Co1—O2W	87.20 (13)	C5—C6—N1	115.6 (4)
O5ⁱ—Co1—O2W	176.36 (14)	C2—C7—C6	120.9 (4)
O1—Co1—O2W	93.49 (13)	C2—C7—H7	119.6
Co1—O1W—H1WA	129.4	C6—C7—H7	119.6
Co1—O1W—H1WB	113.6	C13—C8—C9	118.6 (4)
H1WA—O1W—H1WB	110.0	C13—C8—N2	117.2 (4)
Co1—O2W—H2WA	97.5	C9—C8—N2	124.1 (4)
Co1—O2W—H2WB	112.9	C10—C9—C8	119.8 (4)
H2WA—O2W—H2WB	109.5	C10—C9—H9	120.1
Co1—O3W—H3WA	120.1	C8—C9—H9	120.1
Co1—O3W—H3WB	105.9	C9—C10—C11	120.9 (4)
H3WA—O3W—H3WB	111.2	C9—C10—H10	119.5
Co1—O4W—H4WA	125.8	C11—C10—H10	119.5
Co1—O4W—H4WB	101.2	O4—C11—C10	117.4 (4)
H4WA—O4W—H4WB	111.2	O4—C11—C12	122.3 (4)
N1—N2—C8	114.1 (3)	C10—C11—C12	120.3 (4)
N2—N1—C6	117.2 (4)	C13—C12—C11	117.9 (4)
C1—O1—Co1	127.7 (3)	C13—C12—C14	120.5 (4)
C3—O3—H3A	109.5	C11—C12—C14	121.6 (4)
C11—O4—H4A	109.5	C8—C13—C12	122.5 (4)
C14—O5—Co1ⁱⁱ	127.3 (3)	C8—C13—H13	118.8
O2—C1—O1	123.7 (4)	C12—C13—H13	118.8
O2—C1—C2	119.4 (4)	O6—C14—O5	123.4 (4)
O1—C1—C2	116.9 (4)	O6—C14—C12	119.9 (4)
C7—C2—C3	119.3 (4)	O5—C14—C12	116.7 (4)
C7—C2—C1	119.8 (4)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WA···O6ⁱⁱⁱ	0.82	1.89	2.667 (5)	157
O1W—H1WB···N1^iv	0.82	2.08	2.871 (5)	161
O2W—H2WA···O2	0.82	1.84	2.629 (5)	161
O3W—H3WA···O2ⁱⁱⁱ	0.82	1.88	2.682 (4)	167
O3W—H3WB···O4^v	0.81	2.23	2.899 (5)	141
O4W—H4WA···N2ⁱⁱⁱ	0.82	2.35	3.074 (5)	148
O4W—H4WB···O6ⁱ	0.82	1.88	2.665 (4)	159
O3—H3A···O1	0.82	1.80	2.521 (5)	147
O4—H4A···O5	0.82	1.82	2.541 (4)	147

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1WA⋯O6ⁱ	0.82	1.89	2.667 (5)	157
O1W—H1WB⋯N1ⁱⁱ	0.82	2.08	2.871 (5)	161
O2W—H2WA⋯O2	0.82	1.84	2.629 (5)	161
O3W—H3WA⋯O2ⁱ	0.82	1.88	2.682 (4)	167
O3W—H3WB⋯O4ⁱⁱⁱ	0.81	2.23	2.899 (5)	141
O4W—H4WA⋯N2ⁱ	0.82	2.35	3.074 (5)	148
O4W—H4WB⋯O6^iv	0.82	1.88	2.665 (4)	159
O3—H3A⋯O1	0.82	1.80	2.521 (5)	147
O4—H4A⋯O5	0.82	1.82	2.541 (4)	147

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

1 in total

Review 1. Colonic targeting of aminosalicylates for the treatment of ulcerative colitis.

Authors: U Klotz
Journal: Dig Liver Dis Date: 2005-03-02 Impact factor: 4.088

1 in total