Literature DB >> 21581506

catena-Poly[[(1,10-phenanthroline)cadmium(II)]-μ-2-(1,3-benzimidazol-2-ylsulfan-yl)acetato-κN,O:N].

Lin Cheng¹, Yan-Yan Sun, Ya-Wen Zhang, Jian-Quan Wang.

Abstract

In title compound, [Cd(C(9)H(6)N(2)O(2)S)(C(12)H(8)N(2))](n), the Cd(II) atom is in a distorted tetra-gonal-pyramidal environment, coordinated by one chelating 1,10-phenanthroline ligand, one chelating 2-(1,3-benzimidazol-2-ylsulfan-yl)acetate (bia) ligand bound through one N atom and one O atom of the carboxyl group, and one N atom from a second bia ligand. Each bia ligand acts as bridge between Cd(II) ions, forming one-dimensional coordination polymers along [010], with a shortest Cd⋯Cd distance of 4.27 (2) Å.

Entities: CellLine Chemical Disease Species

Year: 2008 PMID： 21581506 PMCID： PMC2967880 DOI： 10.1107/S1600536808041044

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

Related literature

For related structures, see: Matthews et al. (1998 ▶); Zhang et al. (2008 ▶).

Experimental

Crystal data

[Cd(C9H6N2O2S)(C12H8N2)] M = 498.84 Monoclinic, a = 9.2195 (10) Å b = 8.2577 (9) Å c = 25.620 (3) Å β = 103.215 (4)° V = 1898.8 (4) Å3 Z = 4 Mo Kα radiation μ = 1.29 mm−1 T = 293 (2) K 0.20 × 0.18 × 0.15 mm

Data collection

Bruker APEX CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 2000 ▶) T min = 0.783, T max = 0.831 9820 measured reflections 3724 independent reflections 3413 reflections with I > 2σ(I) R int = 0.025

Refinement

R[F 2 > 2σ(F 2)] = 0.041 wR(F 2) = 0.091 S = 1.04 3724 reflections 262 parameters H-atom parameters constrained Δρmax = 0.62 e Å−3 Δρmin = −0.46 e Å−3 Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808041044/bi2328sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808041044/bi2328Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Cd(C₉H₆N₂O₂S)(C₁₂H₈N₂)]	F(000) = 992
M_r = 498.84	D_x = 1.745 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 781 reflections
a = 9.2195 (10) Å	θ = 2.4–28.0°
b = 8.2577 (9) Å	µ = 1.29 mm⁻¹
c = 25.620 (3) Å	T = 293 K
β = 103.215 (4)°	Block, colorless
V = 1898.8 (4) Å³	0.20 × 0.18 × 0.15 mm
Z = 4

Bruker APEX CCD diffractometer	3724 independent reflections
Radiation source: fine-focus sealed tube	3413 reflections with I > 2σ(I)
graphite	R_int = 0.025
φ and ω scans	θ_max = 26.0°, θ_min = 2.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 2000)	h = −11→11
T_min = 0.783, T_max = 0.831	k = −9→10
9820 measured reflections	l = −31→26

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)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.091	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0401P)² + 3.0611P] where P = (F_o² + 2F_c²)/3
3724 reflections	(Δ/σ)_max < 0.001
262 parameters	Δρ_max = 0.62 e Å⁻³
0 restraints	Δρ_min = −0.46 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
Cd1	−0.02266 (3)	−0.35415 (3)	−0.160159 (10)	0.03702 (11)
S1	−0.16960 (11)	−0.61304 (14)	−0.27062 (4)	0.0438 (2)
O1	−0.2554 (4)	−0.4866 (4)	−0.42417 (12)	0.0656 (9)
O2	−0.1646 (3)	−0.7175 (4)	−0.38778 (11)	0.0536 (8)
N1	0.0906 (3)	−0.5378 (4)	−0.20121 (12)	0.0375 (7)
N2	0.1161 (3)	−0.6933 (4)	−0.27140 (12)	0.0382 (7)
N3	−0.2011 (4)	−0.2403 (4)	−0.11518 (12)	0.0420 (8)
N4	−0.0690 (3)	−0.5365 (4)	−0.09663 (12)	0.0372 (7)
C1	0.3638 (5)	−0.5327 (6)	−0.15550 (18)	0.0543 (11)
H1A	0.3548	−0.4674	−0.1268	0.065*
C2	0.4989 (5)	−0.5924 (7)	−0.1596 (2)	0.0638 (13)
H2A	0.5829	−0.5674	−0.1331	0.077*
C3	0.5142 (5)	−0.6896 (6)	−0.2025 (2)	0.0578 (12)
H3A	0.6080	−0.7285	−0.2038	0.069*
C4	0.3944 (4)	−0.7286 (6)	−0.24257 (17)	0.0481 (10)
H4A	0.4049	−0.7929	−0.2713	0.058*
C5	0.2560 (4)	−0.6688 (5)	−0.23888 (15)	0.0369 (8)
C6	0.2405 (4)	−0.5729 (5)	−0.19558 (15)	0.0382 (8)
C7	0.0246 (4)	−0.6129 (4)	−0.24705 (14)	0.0350 (8)
C8	−0.1951 (5)	−0.4915 (5)	−0.33087 (16)	0.0503 (10)
H8A	−0.2856	−0.4290	−0.3335	0.060*
H8B	−0.1133	−0.4147	−0.3255	0.060*
C9	−0.2050 (4)	−0.5725 (5)	−0.38529 (15)	0.0401 (9)
C10	−0.2683 (5)	−0.0977 (6)	−0.12479 (18)	0.0533 (11)
H10A	−0.2493	−0.0352	−0.1527	0.064*
C11	−0.3653 (5)	−0.0372 (6)	−0.09554 (19)	0.0600 (12)
H11A	−0.4117	0.0624	−0.1042	0.072*
C12	−0.3913 (5)	−0.1260 (6)	−0.05392 (18)	0.0577 (12)
H12A	−0.4549	−0.0865	−0.0335	0.069*
C13	−0.3225 (4)	−0.2768 (6)	−0.04181 (16)	0.0443 (9)
C14	−0.3439 (5)	−0.3777 (6)	0.00100 (18)	0.0551 (12)
H14A	−0.4031	−0.3409	0.0234	0.066*
C15	−0.2810 (5)	−0.5237 (6)	0.00960 (17)	0.0519 (11)
H15A	−0.2986	−0.5873	0.0375	0.062*
C16	−0.1871 (4)	−0.5838 (5)	−0.02325 (15)	0.0400 (9)
C17	−0.1199 (5)	−0.7361 (6)	−0.01553 (16)	0.0480 (10)
H17A	−0.1378	−0.8042	0.0112	0.058*
C18	−0.0281 (5)	−0.7844 (5)	−0.04729 (17)	0.0497 (10)
H18A	0.0185	−0.8849	−0.0423	0.060*
C19	−0.0053 (5)	−0.6804 (5)	−0.08740 (16)	0.0450 (10)
H19A	0.0579	−0.7139	−0.1088	0.054*
C20	−0.1588 (4)	−0.4874 (5)	−0.06459 (14)	0.0351 (8)
C21	−0.2282 (4)	−0.3303 (5)	−0.07459 (14)	0.0372 (8)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.04657 (18)	0.03648 (18)	0.02956 (16)	0.00219 (12)	0.01194 (11)	0.00272 (11)
S1	0.0372 (5)	0.0561 (6)	0.0393 (5)	−0.0041 (5)	0.0109 (4)	−0.0040 (5)
O1	0.093 (3)	0.056 (2)	0.0449 (18)	0.0063 (18)	0.0098 (17)	0.0128 (15)
O2	0.0666 (19)	0.0493 (18)	0.0396 (16)	0.0129 (15)	0.0011 (14)	−0.0080 (13)
N1	0.0437 (18)	0.0410 (18)	0.0279 (15)	−0.0012 (14)	0.0085 (13)	−0.0034 (13)
N2	0.0396 (17)	0.0422 (18)	0.0341 (16)	−0.0015 (14)	0.0112 (13)	−0.0054 (14)
N3	0.0515 (19)	0.0405 (19)	0.0335 (17)	0.0040 (16)	0.0088 (14)	0.0000 (14)
N4	0.0410 (17)	0.0374 (18)	0.0352 (16)	0.0000 (14)	0.0129 (13)	−0.0012 (14)
C1	0.056 (3)	0.054 (3)	0.047 (2)	−0.007 (2)	−0.002 (2)	−0.011 (2)
C2	0.043 (3)	0.071 (3)	0.068 (3)	−0.012 (2)	−0.007 (2)	−0.006 (3)
C3	0.037 (2)	0.067 (3)	0.069 (3)	0.001 (2)	0.011 (2)	0.014 (3)
C4	0.043 (2)	0.058 (3)	0.047 (2)	0.003 (2)	0.0191 (19)	0.003 (2)
C5	0.041 (2)	0.038 (2)	0.0325 (19)	−0.0045 (16)	0.0108 (16)	0.0054 (16)
C6	0.043 (2)	0.035 (2)	0.036 (2)	−0.0044 (17)	0.0074 (16)	0.0038 (16)
C7	0.040 (2)	0.035 (2)	0.0314 (18)	−0.0031 (16)	0.0113 (15)	0.0004 (15)
C8	0.058 (3)	0.045 (2)	0.042 (2)	0.010 (2)	−0.0002 (19)	−0.0038 (19)
C9	0.0336 (19)	0.045 (2)	0.041 (2)	−0.0077 (17)	0.0084 (16)	−0.0029 (18)
C10	0.069 (3)	0.045 (3)	0.047 (2)	0.009 (2)	0.016 (2)	0.004 (2)
C11	0.067 (3)	0.053 (3)	0.059 (3)	0.020 (2)	0.012 (2)	−0.004 (2)
C12	0.051 (3)	0.075 (3)	0.049 (3)	0.013 (2)	0.016 (2)	−0.013 (2)
C13	0.038 (2)	0.057 (3)	0.039 (2)	0.0047 (19)	0.0106 (16)	−0.0069 (19)
C14	0.047 (2)	0.079 (4)	0.045 (2)	0.003 (2)	0.0223 (19)	−0.001 (2)
C15	0.046 (2)	0.071 (3)	0.042 (2)	−0.003 (2)	0.0172 (19)	0.007 (2)
C16	0.0342 (19)	0.051 (2)	0.0332 (19)	−0.0069 (17)	0.0040 (15)	0.0030 (17)
C17	0.052 (2)	0.051 (3)	0.040 (2)	−0.007 (2)	0.0079 (18)	0.0110 (19)
C18	0.061 (3)	0.038 (2)	0.047 (2)	0.003 (2)	0.007 (2)	0.0075 (19)
C19	0.053 (2)	0.041 (2)	0.043 (2)	0.0037 (19)	0.0153 (19)	0.0003 (18)
C20	0.0297 (18)	0.043 (2)	0.0309 (18)	−0.0052 (16)	0.0031 (14)	−0.0026 (16)
C21	0.0360 (19)	0.044 (2)	0.0305 (18)	−0.0016 (16)	0.0050 (15)	−0.0051 (16)

Cd1—O2ⁱ	2.189 (3)	C4—C5	1.391 (5)
Cd1—N2ⁱ	2.211 (3)	C4—H4A	0.930
Cd1—N1	2.236 (3)	C5—C6	1.397 (5)
Cd1—N4	2.327 (3)	C8—C9	1.530 (5)
Cd1—N3	2.405 (3)	C8—H8A	0.970
S1—C7	1.754 (4)	C8—H8B	0.970
S1—C8	1.811 (4)	C10—C11	1.384 (6)
O1—C9	1.225 (5)	C10—H10A	0.930
O2—C9	1.260 (5)	C11—C12	1.360 (7)
O2—Cd1ⁱⁱ	2.189 (3)	C11—H11A	0.930
N1—C7	1.344 (5)	C12—C13	1.400 (6)
N1—C6	1.387 (5)	C12—H12A	0.930
N2—C7	1.334 (5)	C13—C21	1.411 (5)
N2—C5	1.382 (5)	C13—C14	1.427 (6)
N2—Cd1ⁱⁱ	2.211 (3)	C14—C15	1.333 (6)
N3—C10	1.327 (5)	C14—H14A	0.930
N3—C21	1.347 (5)	C15—C16	1.427 (6)
N4—C19	1.323 (5)	C15—H15A	0.930
N4—C20	1.355 (5)	C16—C17	1.396 (6)
C1—C2	1.365 (6)	C16—C20	1.396 (5)
C1—C6	1.387 (5)	C17—C18	1.361 (6)
C1—H1A	0.930	C17—H17A	0.930
C2—C3	1.394 (7)	C18—C19	1.392 (6)
C2—H2A	0.930	C18—H18A	0.930
C3—C4	1.363 (6)	C19—H19A	0.930
C3—H3A	0.930	C20—C21	1.443 (5)

O2ⁱ—Cd1—N2ⁱ	104.44 (11)	C9—C8—S1	120.2 (3)
O2ⁱ—Cd1—N1	102.73 (12)	C9—C8—H8A	107.3
N2ⁱ—Cd1—N1	99.99 (11)	S1—C8—H8A	107.3
O2ⁱ—Cd1—N4	100.86 (11)	C9—C8—H8B	107.3
N2ⁱ—Cd1—N4	147.43 (11)	S1—C8—H8B	107.3
N1—Cd1—N4	94.03 (11)	H8A—C8—H8B	106.9
O2ⁱ—Cd1—N3	93.88 (12)	O1—C9—O2	124.8 (4)
N2ⁱ—Cd1—N3	87.71 (11)	O1—C9—C8	114.9 (4)
N1—Cd1—N3	159.18 (12)	O2—C9—C8	120.3 (4)
N4—Cd1—N3	70.30 (11)	N3—C10—C11	123.5 (4)
C7—S1—C8	102.5 (2)	N3—C10—H10A	118.2
C9—O2—Cd1ⁱⁱ	131.8 (3)	C11—C10—H10A	118.2
C7—N1—C6	103.6 (3)	C12—C11—C10	118.8 (4)
C7—N1—Cd1	123.9 (2)	C12—C11—H11A	120.6
C6—N1—Cd1	130.9 (2)	C10—C11—H11A	120.6
C7—N2—C5	104.4 (3)	C11—C12—C13	120.1 (4)
C7—N2—Cd1ⁱⁱ	119.8 (2)	C11—C12—H12A	120.0
C5—N2—Cd1ⁱⁱ	135.0 (3)	C13—C12—H12A	120.0
C10—N3—C21	118.2 (3)	C12—C13—C21	117.2 (4)
C10—N3—Cd1	126.8 (3)	C12—C13—C14	123.7 (4)
C21—N3—Cd1	114.9 (2)	C21—C13—C14	119.1 (4)
C19—N4—C20	117.9 (3)	C15—C14—C13	121.6 (4)
C19—N4—Cd1	124.2 (3)	C15—C14—H14A	119.2
C20—N4—Cd1	117.8 (2)	C13—C14—H14A	119.2
C2—C1—C6	117.7 (4)	C14—C15—C16	121.1 (4)
C2—C1—H1A	121.2	C14—C15—H15A	119.5
C6—C1—H1A	121.2	C16—C15—H15A	119.5
C1—C2—C3	121.8 (4)	C17—C16—C20	117.8 (4)
C1—C2—H2A	119.1	C17—C16—C15	122.6 (4)
C3—C2—H2A	119.1	C20—C16—C15	119.5 (4)
C4—C3—C2	121.3 (4)	C18—C17—C16	119.7 (4)
C4—C3—H3A	119.4	C18—C17—H17A	120.1
C2—C3—H3A	119.4	C16—C17—H17A	120.1
C3—C4—C5	117.5 (4)	C17—C18—C19	118.7 (4)
C3—C4—H4A	121.2	C17—C18—H18A	120.7
C5—C4—H4A	121.2	C19—C18—H18A	120.7
N2—C5—C4	130.7 (4)	N4—C19—C18	123.4 (4)
N2—C5—C6	108.1 (3)	N4—C19—H19A	118.3
C4—C5—C6	121.2 (4)	C18—C19—H19A	118.3
N1—C6—C1	131.0 (4)	N4—C20—C16	122.4 (4)
N1—C6—C5	108.5 (3)	N4—C20—C21	118.0 (3)
C1—C6—C5	120.5 (4)	C16—C20—C21	119.7 (3)
N2—C7—N1	115.5 (3)	N3—C21—C13	122.3 (4)
N2—C7—S1	122.9 (3)	N3—C21—C20	118.7 (3)
N1—C7—S1	121.5 (3)	C13—C21—C20	119.0 (4)

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(2)-1,2-bis-[4-(3-pyrid-yl)pyrimidin-2-ylsulfan-yl]ethane}di-μ(2)-cyanido-dicopper(I)].

Authors: Ya-Wen Zhang; Hua-Ze Dong; Lin Cheng
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2008-06-07

2 in total

1 in total

1. Bis[2-(benzimidazol-2-ylsulfan-yl)acetato]bis-(2,2'-bipyridine)cadmium(II).

Authors: Lin Cheng; Yan-Yan Sun; Jian-Quan Wang; Ya-Wen Zhang
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2009-10-13

1 in total