Literature DB >> 21580265

Poly[[μ(2)-1,2-bis-(imidazol-1-ylmeth-yl)benzene](μ(2)-cyclo-hexane-1,4-dicarboxyl-ato)cobalt(II)].

Abstract

In the the title compound, [Co(C(8)H(10)O(4))(C(14)H(14)N(4))](n), the Co(II) atom is four-coordinated by two N atoms from two different 1,2-bis-(imidazol-1-ylmeth-yl)benzene ligands and two carboxyl-ate O atoms from two different cyclo-hexane-1,4-dicarboxyl-ate anions in a tetra-hedral coordination geometry. The resulting structure is a two-dimensional polymer with layers in the (100) plane.

Entities: CellLine Chemical Disease Species

Year: 2010 PMID： 21580265 PMCID： PMC2983598 DOI： 10.1107/S160053681000646X

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

Related literature

For a related structure, see: Li et al. (2009 ▶).

Experimental

Crystal data

[Co(C8H10O4)(C14H14N4)] M = 467.38 Monoclinic, a = 9.785 (3) Å b = 12.356 (2) Å c = 17.850 (4) Å β = 99.559 (2)° V = 2128.2 (9) Å3 Z = 4 Mo Kα radiation μ = 0.84 mm−1 T = 293 K 0.27 × 0.21 × 0.17 mm

Data collection

Oxford Diffraction Gemini R Ultra diffractometer Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006 ▶) T min = 0.51, T max = 0.83 9866 measured reflections 4923 independent reflections 3485 reflections with I > 2σ(I) R int = 0.019

Refinement

R[F 2 > 2σ(F 2)] = 0.031 wR(F 2) = 0.079 S = 0.96 4923 reflections 280 parameters H-atom parameters constrained Δρmax = 0.22 e Å−3 Δρmin = −0.36 e Å−3 Data collection: CrysAlis CCD (Oxford Diffraction, 2006 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2006 ▶); data reduction: CrysAlis RED; 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 global, I. DOI: 10.1107/S160053681000646X/bt5196sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S160053681000646X/bt5196Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Co(C₈H₁₀O₄)(C₁₄H₁₄N₄)]	F(000) = 972
M_r = 467.38	D_x = 1.459 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 4923 reflections
a = 9.785 (3) Å	θ = 2.3–29.1°
b = 12.356 (2) Å	µ = 0.84 mm⁻¹
c = 17.850 (4) Å	T = 293 K
β = 99.559 (2)°	Block, purple
V = 2128.2 (9) Å³	0.27 × 0.21 × 0.17 mm
Z = 4

Oxford Diffraction Gemini R Ultra diffractometer	4923 independent reflections
Radiation source: fine-focus sealed tube	3485 reflections with I > 2σ(I)
graphite	R_int = 0.019
Detector resolution: 10.0 pixels mm^-1	θ_max = 29.1°, θ_min = 2.3°
ω scan	h = −8→12
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006)	k = −16→15
T_min = 0.51, T_max = 0.83	l = −23→22
9866 measured reflections

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)] = 0.031	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.079	H-atom parameters constrained
S = 0.96	w = 1/[σ²(F_o²) + (0.0456P)²] where P = (F_o² + 2F_c²)/3
4923 reflections	(Δ/σ)_max = 0.001
280 parameters	Δρ_max = 0.22 e Å⁻³
0 restraints	Δρ_min = −0.36 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 > 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
C1	0.73125 (18)	0.35656 (12)	0.18015 (9)	0.0353 (4)
C2	0.82011 (19)	0.44982 (12)	0.21681 (8)	0.0372 (4)
H2	0.9170	0.4315	0.2151	0.045*
C3	0.8064 (2)	0.46346 (14)	0.30090 (9)	0.0452 (4)
H3A	0.7090	0.4687	0.3049	0.054*
H3B	0.8434	0.3996	0.3287	0.054*
C4	0.8814 (2)	0.56275 (15)	0.33757 (10)	0.0515 (5)
H4A	0.9805	0.5529	0.3407	0.062*
H4B	0.8621	0.5705	0.3889	0.062*
C5	0.8367 (2)	0.66551 (14)	0.29255 (10)	0.0476 (5)
H5	0.8949	0.7248	0.3162	0.057*
C6	0.8670 (2)	0.65185 (14)	0.21139 (10)	0.0513 (5)
H6A	0.8402	0.7171	0.1824	0.062*
H6B	0.9657	0.6411	0.2130	0.062*
C7	0.7878 (2)	0.55525 (13)	0.17234 (9)	0.0450 (5)
H7A	0.8115	0.5467	0.1220	0.054*
H7B	0.6892	0.5696	0.1665	0.054*
C8	0.6860 (2)	0.69815 (14)	0.29141 (10)	0.0460 (5)
C9	0.64364 (19)	0.15946 (12)	0.36882 (9)	0.0393 (4)
H9	0.6565	0.2340	0.3690	0.047*
C10	0.65119 (17)	0.09703 (13)	0.43108 (8)	0.0368 (4)
H10	0.6699	0.1200	0.4814	0.044*
C11	0.60365 (17)	−0.00366 (12)	0.32978 (8)	0.0340 (4)
H11	0.5836	−0.0639	0.2986	0.041*
C12	0.62805 (17)	−0.10377 (13)	0.45236 (9)	0.0375 (4)
H12A	0.5627	−0.1555	0.4258	0.045*
H12B	0.5966	−0.0851	0.4995	0.045*
C13	0.76758 (16)	−0.15711 (12)	0.47099 (8)	0.0294 (3)
C14	0.88512 (18)	−0.11324 (14)	0.44907 (9)	0.0379 (4)
H14	0.8783	−0.0491	0.4214	0.046*
C15	1.01216 (19)	−0.16348 (15)	0.46771 (11)	0.0478 (5)
H15	1.0900	−0.1343	0.4517	0.057*
C16	1.02296 (19)	−0.25688 (16)	0.51008 (11)	0.0488 (5)
H16	1.1089	−0.2898	0.5239	0.059*
C17	0.90668 (18)	−0.30224 (14)	0.53235 (9)	0.0409 (4)
H17	0.9148	−0.3657	0.5608	0.049*
C18	0.77854 (16)	−0.25356 (12)	0.51251 (8)	0.0304 (3)
C19	0.64901 (18)	−0.30062 (13)	0.53515 (10)	0.0426 (4)
H19A	0.6259	−0.2593	0.5775	0.051*
H19B	0.5732	−0.2925	0.4930	0.051*
C20	0.64394 (19)	−0.45501 (12)	0.62419 (8)	0.0382 (4)
H20	0.6285	−0.4133	0.6653	0.046*
C21	0.67567 (18)	−0.58996 (13)	0.55355 (9)	0.0407 (4)
H21	0.6869	−0.6603	0.5371	0.049*
C22	0.67997 (19)	−0.50032 (14)	0.51112 (9)	0.0433 (4)
H22	0.6934	−0.4972	0.4608	0.052*
O1	0.69190 (13)	0.35191 (9)	0.11146 (6)	0.0465 (3)
O2	0.69910 (18)	0.28649 (10)	0.22607 (7)	0.0728 (5)
O3	0.63128 (16)	0.76656 (10)	0.24541 (8)	0.0623 (4)
O4	0.61815 (14)	0.65379 (10)	0.33933 (7)	0.0507 (3)
Co1	0.58188 (3)	0.163209 (16)	0.199462 (11)	0.03716 (9)
N1	0.61394 (14)	0.09605 (10)	0.30478 (7)	0.0355 (3)
N2	0.62601 (13)	−0.00679 (10)	0.40605 (6)	0.0320 (3)
N3	0.66068 (14)	−0.41468 (10)	0.55676 (7)	0.0363 (3)
N4	0.65211 (15)	−0.56183 (10)	0.62477 (7)	0.0376 (3)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0446 (10)	0.0288 (8)	0.0349 (8)	0.0005 (7)	0.0134 (7)	−0.0012 (7)
C2	0.0450 (10)	0.0350 (9)	0.0322 (8)	−0.0061 (8)	0.0081 (7)	−0.0004 (7)
C3	0.0651 (13)	0.0405 (9)	0.0284 (8)	−0.0088 (9)	0.0029 (8)	0.0044 (7)
C4	0.0632 (13)	0.0539 (11)	0.0357 (9)	−0.0103 (10)	0.0036 (9)	−0.0056 (8)
C5	0.0629 (13)	0.0392 (9)	0.0427 (10)	−0.0196 (9)	0.0144 (9)	−0.0098 (8)
C6	0.0732 (15)	0.0381 (10)	0.0474 (10)	−0.0159 (9)	0.0239 (10)	−0.0020 (8)
C7	0.0710 (14)	0.0358 (9)	0.0299 (8)	−0.0082 (9)	0.0136 (8)	0.0033 (7)
C8	0.0704 (14)	0.0320 (8)	0.0376 (9)	−0.0129 (9)	0.0144 (9)	−0.0138 (8)
C9	0.0589 (12)	0.0271 (8)	0.0317 (8)	−0.0047 (8)	0.0065 (8)	−0.0034 (7)
C10	0.0442 (10)	0.0390 (9)	0.0261 (7)	−0.0042 (8)	0.0028 (7)	−0.0037 (7)
C11	0.0484 (11)	0.0268 (7)	0.0267 (7)	−0.0009 (7)	0.0057 (7)	−0.0001 (6)
C12	0.0350 (10)	0.0401 (9)	0.0376 (8)	−0.0006 (7)	0.0064 (7)	0.0152 (7)
C13	0.0305 (9)	0.0332 (8)	0.0241 (7)	−0.0033 (7)	0.0036 (6)	0.0005 (6)
C14	0.0377 (10)	0.0389 (9)	0.0377 (8)	−0.0064 (8)	0.0077 (7)	0.0040 (7)
C15	0.0334 (11)	0.0568 (11)	0.0551 (11)	−0.0066 (9)	0.0132 (9)	−0.0003 (9)
C16	0.0302 (11)	0.0564 (11)	0.0590 (11)	0.0073 (9)	0.0050 (8)	−0.0021 (9)
C17	0.0405 (11)	0.0386 (9)	0.0421 (9)	0.0045 (8)	0.0023 (8)	0.0042 (8)
C18	0.0327 (9)	0.0321 (8)	0.0264 (7)	−0.0001 (7)	0.0052 (6)	0.0009 (6)
C19	0.0405 (11)	0.0357 (8)	0.0533 (10)	0.0041 (8)	0.0127 (8)	0.0184 (8)
C20	0.0537 (11)	0.0320 (8)	0.0305 (8)	0.0004 (8)	0.0114 (7)	0.0034 (7)
C21	0.0508 (11)	0.0338 (8)	0.0413 (9)	−0.0012 (8)	0.0187 (8)	−0.0043 (7)
C22	0.0542 (12)	0.0466 (10)	0.0337 (8)	−0.0053 (9)	0.0201 (8)	−0.0009 (8)
O1	0.0559 (8)	0.0480 (7)	0.0332 (6)	−0.0070 (6)	0.0002 (6)	−0.0032 (5)
O2	0.1385 (15)	0.0422 (7)	0.0405 (7)	−0.0395 (9)	0.0230 (8)	−0.0041 (6)
O3	0.0897 (11)	0.0376 (7)	0.0610 (8)	0.0019 (7)	0.0166 (8)	0.0034 (6)
O4	0.0642 (9)	0.0535 (8)	0.0360 (6)	−0.0124 (6)	0.0131 (6)	−0.0060 (5)
Co1	0.06634 (19)	0.02305 (11)	0.02269 (11)	−0.00140 (10)	0.00917 (10)	−0.00115 (8)
N1	0.0525 (9)	0.0282 (7)	0.0257 (6)	−0.0011 (6)	0.0065 (6)	0.0003 (5)
N2	0.0348 (8)	0.0334 (7)	0.0274 (6)	−0.0003 (6)	0.0037 (5)	0.0080 (5)
N3	0.0443 (9)	0.0333 (7)	0.0331 (6)	−0.0007 (6)	0.0115 (6)	0.0086 (6)
N4	0.0510 (9)	0.0309 (7)	0.0317 (7)	0.0005 (6)	0.0089 (6)	0.0037 (6)

C1—O1	1.2240 (19)	C12—C13	1.503 (2)
C1—O2	1.2673 (19)	C12—H12A	0.9700
C1—C2	1.524 (2)	C12—H12B	0.9700
C2—C7	1.531 (2)	C13—C14	1.385 (2)
C2—C3	1.538 (2)	C13—C18	1.398 (2)
C2—H2	0.9800	C14—C15	1.380 (2)
C3—C4	1.521 (2)	C14—H14	0.9300
C3—H3A	0.9700	C15—C16	1.374 (3)
C3—H3B	0.9700	C15—H15	0.9300
C4—C5	1.527 (3)	C16—C17	1.385 (3)
C4—H4A	0.9700	C16—H16	0.9300
C4—H4B	0.9700	C17—C18	1.383 (2)
C5—C8	1.526 (3)	C17—H17	0.9300
C5—C6	1.536 (3)	C18—C19	1.509 (2)
C5—H5	0.9800	C19—N3	1.461 (2)
C6—C7	1.527 (2)	C19—H19A	0.9700
C6—H6A	0.9700	C19—H19B	0.9700
C6—H6B	0.9700	C20—N4	1.3222 (19)
C7—H7A	0.9700	C20—N3	1.3377 (19)
C7—H7B	0.9700	C20—H20	0.9300
C8—O3	1.237 (2)	C21—C22	1.346 (2)
C8—O4	1.289 (2)	C21—N4	1.374 (2)
C9—C10	1.345 (2)	C21—H21	0.9300
C9—N1	1.376 (2)	C22—N3	1.367 (2)
C9—H9	0.9300	C22—H22	0.9300
C10—N2	1.367 (2)	O2—Co1	1.9185 (13)
C10—H10	0.9300	O4—Co1ⁱ	1.9682 (15)
C11—N1	1.3199 (19)	Co1—O4ⁱⁱ	1.9682 (15)
C11—N2	1.3432 (18)	Co1—N4ⁱⁱⁱ	2.0306 (13)
C11—H11	0.9300	Co1—N1	2.0311 (12)
C12—N2	1.4541 (19)	N4—Co1^iv	2.0306 (13)

O1—C1—O2	123.04 (15)	C13—C12—H12B	108.7
O1—C1—C2	121.85 (14)	H12A—C12—H12B	107.6
O2—C1—C2	115.09 (14)	C14—C13—C18	119.29 (15)
C1—C2—C7	111.52 (13)	C14—C13—C12	122.16 (14)
C1—C2—C3	111.46 (13)	C18—C13—C12	118.55 (14)
C7—C2—C3	111.64 (13)	C15—C14—C13	120.84 (16)
C1—C2—H2	107.3	C15—C14—H14	119.6
C7—C2—H2	107.3	C13—C14—H14	119.6
C3—C2—H2	107.3	C16—C15—C14	119.63 (17)
C4—C3—C2	113.23 (14)	C16—C15—H15	120.2
C4—C3—H3A	108.9	C14—C15—H15	120.2
C2—C3—H3A	108.9	C15—C16—C17	120.41 (17)
C4—C3—H3B	108.9	C15—C16—H16	119.8
C2—C3—H3B	108.9	C17—C16—H16	119.8
H3A—C3—H3B	107.7	C18—C17—C16	120.26 (16)
C3—C4—C5	111.62 (14)	C18—C17—H17	119.9
C3—C4—H4A	109.3	C16—C17—H17	119.9
C5—C4—H4A	109.3	C17—C18—C13	119.54 (15)
C3—C4—H4B	109.3	C17—C18—C19	122.00 (14)
C5—C4—H4B	109.3	C13—C18—C19	118.46 (14)
H4A—C4—H4B	108.0	N3—C19—C18	114.22 (14)
C8—C5—C4	114.75 (16)	N3—C19—H19A	108.7
C8—C5—C6	110.77 (16)	C18—C19—H19A	108.7
C4—C5—C6	108.75 (15)	N3—C19—H19B	108.7
C8—C5—H5	107.4	C18—C19—H19B	108.7
C4—C5—H5	107.4	H19A—C19—H19B	107.6
C6—C5—H5	107.4	N4—C20—N3	111.26 (14)
C7—C6—C5	110.70 (14)	N4—C20—H20	124.4
C7—C6—H6A	109.5	N3—C20—H20	124.4
C5—C6—H6A	109.5	C22—C21—N4	109.76 (14)
C7—C6—H6B	109.5	C22—C21—H21	125.1
C5—C6—H6B	109.5	N4—C21—H21	125.1
H6A—C6—H6B	108.1	C21—C22—N3	106.33 (14)
C6—C7—C2	112.53 (14)	C21—C22—H22	126.8
C6—C7—H7A	109.1	N3—C22—H22	126.8
C2—C7—H7A	109.1	C1—O2—Co1	125.78 (11)
C6—C7—H7B	109.1	C8—O4—Co1ⁱ	109.44 (12)
C2—C7—H7B	109.1	O2—Co1—O4ⁱⁱ	130.75 (6)
H7A—C7—H7B	107.8	O2—Co1—N4ⁱⁱⁱ	113.50 (6)
O3—C8—O4	121.2 (2)	O4ⁱⁱ—Co1—N4ⁱⁱⁱ	99.08 (6)
O3—C8—C5	120.01 (17)	O2—Co1—N1	95.80 (5)
O4—C8—C5	118.80 (17)	O4ⁱⁱ—Co1—N1	107.05 (5)
C10—C9—N1	109.56 (14)	N4ⁱⁱⁱ—Co1—N1	109.79 (5)
C10—C9—H9	125.2	C11—N1—C9	105.55 (12)
N1—C9—H9	125.2	C11—N1—Co1	133.27 (10)
C9—C10—N2	106.62 (13)	C9—N1—Co1	121.00 (10)
C9—C10—H10	126.7	C11—N2—C10	107.12 (12)
N2—C10—H10	126.7	C11—N2—C12	125.77 (13)
N1—C11—N2	111.14 (13)	C10—N2—C12	127.07 (12)
N1—C11—H11	124.4	C20—N3—C22	107.30 (13)
N2—C11—H11	124.4	C20—N3—C19	125.54 (14)
N2—C12—C13	114.42 (13)	C22—N3—C19	127.00 (13)
N2—C12—H12A	108.7	C20—N4—C21	105.34 (13)
C13—C12—H12A	108.7	C20—N4—Co1^iv	126.46 (11)
N2—C12—H12B	108.7	C21—N4—Co1^iv	125.35 (11)

2 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[[μ-1,4-bis-(imidazol-1-ylmeth-yl)benzene]bis-(μ(4)-cyclo-hexane-1,4-dicarboxyl-ato)dinickel(II)].

Authors: Bing-Bing Li; Gai-Xia Fang; Xiao-Na Ji; Bo Xiao; Edward R T Tiekink
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2009-07-31

2 in total