Literature DB >> 21203028

catena-Poly[[(2,9-dieth-oxy-1,10-phen-anthroline-κN,N')cadmium(II)]-di-μ-dicyan-amido-κN:N].

Xian-Fu Zheng¹, Cao-Yuan Niu, Cao-Ling Feng, Xin-Sheng Wan, Chun-Hong Kou.

Abstract

In the title polymer, [Cd(C(2)N(3))(2)(C(16)H(16)N(2)O(2))](n), the Cd(II) ion is coordinated by two N atoms from one 2,9-dieth-oxy-1,10-phenanthroline mol-ecule and four N atoms from four symmetry-related dicyanamide ions in a distorted octa-hedral geometry. In the 2,9-dieth-oxy-1,10-phenanthroline ligand, the O and C atoms of the eth-oxy groups are located almost in the plane defined by the phenanthroline ring system. Two dicyanamide ions bridge two Cd(II) ions, which are located on a twofold axis, forming a one-dimensional zigzag chain along the [001] direction. The 2,9-dieth-oxy-1,10-phenanthroline mol-ecules act as bidentate terminal ligands. There are π-π inter-actions between polymeric chains, characterized by a centroid-centroid distance of 3.7624 (2) Å between the phenanthroline rings of two neighbouring chains.

Entities: CellLine Chemical Disease Species

Year: 2008 PMID： 21203028 PMCID： PMC2961958 DOI： 10.1107/S1600536808021727

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

Related literature

For related literature, see: Brammer (2004 ▶); Chao et al. (2000 ▶); Fletcher et al. (2001 ▶); Lan et al. (2005 ▶); Luo et al. (2002 ▶); Jensen et al. (2002 ▶); Pijper et al. (1984 ▶); Karmakar et al. (2006 ▶); Triki et al. (2001 ▶); Wang et al. (2004 ▶); Bing et al. (2004 ▶).

Experimental

Crystal data

[Cd(C2N3)2(C16H16N2O2)] M = 512.81 Monoclinic, a = 14.3605 (9) Å b = 12.4386 (8) Å c = 11.7582 (7) Å β = 106.676 (1)° V = 2012.0 (2) Å3 Z = 4 Mo Kα radiation μ = 1.12 mm−1 T = 173 (2) K 0.48 × 0.22 × 0.12 mm

Data collection

Siemens SMART CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Siemens, 1996 ▶) T min = 0.615, T max = 0.877 6910 measured reflections 2607 independent reflections 2481 reflections with I > 2σ(I) R int = 0.013

Refinement

R[F 2 > 2σ(F 2)] = 0.019 wR(F 2) = 0.051 S = 1.04 2607 reflections 142 parameters H-atom parameters constrained Δρmax = 0.35 e Å−3 Δρmin = −0.33 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/S1600536808021727/bh2180sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808021727/bh2180Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Cd(C₂N₃)₂(C₁₆H₁₆N₂O₂)]	Z = 4
M_r = 512.81	F₀₀₀ = 1024
Monoclinic, C2/c	D_x = 1.693 Mg m⁻³
Hall symbol: -C 2yc	Mo Kα radiation λ = 0.71073 Å
a = 14.3605 (9) Å	θ = 2.2–29.0º
b = 12.4386 (8) Å	µ = 1.12 mm⁻¹
c = 11.7582 (7) Å	T = 173 (2) K
β = 106.6760 (10)º	Block, colourless
V = 2012.0 (2) Å³	0.48 × 0.22 × 0.12 mm

Siemens SMART CCD area-detector diffractometer	2607 independent reflections
Radiation source: fine-focus sealed tube	2481 reflections with I > 2σ(I)
Monochromator: graphite	R_int = 0.013
T = 173(2) K	θ_max = 29.0º
φ and ω scans	θ_min = 2.2º
Absorption correction: multi-scan(SADABS; Siemens, 1996)	h = −19→18
T_min = 0.615, T_max = 0.877	k = −14→16
6910 measured reflections	l = −15→15

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.019	H-atom parameters constrained
wR(F²) = 0.051	w = 1/[σ²(F_o²) + (0.0307P)² + 0.6141P] where P = (F_o² + 2F_c²)/3
S = 1.04	(Δ/σ)_max = 0.001
2607 reflections	Δρ_max = 0.35 e Å⁻³
142 parameters	Δρ_min = −0.33 e Å⁻³
Primary atom site location: structure-invariant direct methods	Extinction correction: none

	x	y	z	U_iso*/U_eq
Cd1	0.0000	0.307814 (10)	0.7500	0.03578 (6)
N1	0.05844 (9)	0.15137 (10)	0.86539 (10)	0.0365 (2)
N2	−0.11504 (13)	0.31300 (11)	0.85824 (15)	0.0536 (4)
N3	−0.13259 (16)	0.38101 (13)	1.04474 (15)	0.0721 (5)
N4	0.08778 (13)	0.44432 (13)	0.86321 (13)	0.0594 (4)
O1	0.13134 (9)	0.24924 (10)	1.02404 (9)	0.0502 (3)
C1	0.11272 (11)	0.15105 (13)	0.97734 (13)	0.0404 (3)
C2	0.14741 (12)	0.05560 (14)	1.04063 (15)	0.0515 (4)
H2	0.1877	0.0582	1.1203	0.062*
C3	0.12161 (13)	−0.03999 (14)	0.98457 (17)	0.0538 (4)
H3	0.1445	−0.1051	1.0252	0.065*
C4	0.06132 (12)	−0.04351 (13)	0.86703 (16)	0.0463 (3)
C5	0.03113 (10)	0.05547 (11)	0.81033 (13)	0.0369 (3)
C6	0.02939 (14)	−0.14182 (13)	0.80563 (18)	0.0570 (4)
H6	0.0502	−0.2083	0.8444	0.068*
C7	0.19439 (13)	0.26036 (16)	1.14355 (14)	0.0510 (4)
H7A	0.2605	0.2345	1.1481	0.061*
H7B	0.1691	0.2175	1.1992	0.061*
C8	0.19725 (16)	0.37679 (18)	1.17551 (16)	0.0649 (5)
H8A	0.2262	0.4179	1.1231	0.097*
H8B	0.2365	0.3863	1.2581	0.097*
H8C	0.1310	0.4025	1.1663	0.097*
C9	−0.12079 (12)	0.35044 (12)	0.94474 (14)	0.0431 (3)
C10	0.10564 (12)	0.52463 (13)	0.91050 (14)	0.0458 (3)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.04617 (9)	0.02954 (8)	0.02878 (8)	0.000	0.00622 (6)	0.000
N1	0.0399 (6)	0.0341 (6)	0.0338 (6)	0.0023 (5)	0.0077 (5)	0.0046 (5)
N2	0.0593 (9)	0.0558 (9)	0.0474 (8)	0.0004 (6)	0.0180 (7)	−0.0080 (6)
N3	0.1294 (16)	0.0418 (8)	0.0601 (10)	−0.0173 (9)	0.0510 (11)	−0.0091 (7)
N4	0.0826 (11)	0.0477 (8)	0.0417 (7)	−0.0154 (7)	0.0078 (7)	−0.0055 (6)
O1	0.0608 (7)	0.0476 (7)	0.0316 (5)	0.0014 (5)	−0.0036 (5)	0.0019 (4)
C1	0.0405 (7)	0.0436 (8)	0.0349 (7)	0.0025 (6)	0.0076 (6)	0.0077 (6)
C2	0.0524 (9)	0.0539 (10)	0.0445 (8)	0.0078 (7)	0.0081 (7)	0.0176 (7)
C3	0.0557 (9)	0.0449 (9)	0.0606 (10)	0.0115 (7)	0.0163 (8)	0.0223 (8)
C4	0.0481 (8)	0.0364 (7)	0.0583 (9)	0.0058 (6)	0.0211 (7)	0.0097 (7)
C5	0.0387 (7)	0.0319 (7)	0.0423 (7)	0.0009 (5)	0.0149 (6)	0.0034 (5)
C6	0.0689 (11)	0.0301 (8)	0.0776 (12)	0.0042 (7)	0.0300 (9)	0.0068 (7)
C7	0.0488 (8)	0.0679 (11)	0.0296 (7)	−0.0070 (8)	0.0004 (6)	0.0052 (7)
C8	0.0750 (12)	0.0754 (13)	0.0376 (8)	−0.0053 (10)	0.0056 (8)	−0.0110 (8)
C9	0.0521 (8)	0.0338 (7)	0.0437 (8)	0.0000 (6)	0.0142 (7)	0.0006 (6)
C10	0.0589 (9)	0.0430 (8)	0.0351 (7)	−0.0022 (7)	0.0128 (6)	0.0022 (6)

Cd1—N4	2.2980 (15)	C2—H2	0.9500
Cd1—N4ⁱ	2.2980 (15)	C3—C4	1.405 (3)
Cd1—N2ⁱ	2.3580 (16)	C3—H3	0.9500
Cd1—N2	2.3580 (16)	C4—C5	1.408 (2)
Cd1—N1ⁱ	2.3829 (12)	C4—C6	1.427 (3)
Cd1—N1	2.3829 (12)	C5—C5ⁱ	1.444 (3)
N1—C1	1.3234 (18)	C6—C6ⁱ	1.338 (4)
N1—C5	1.3602 (19)	C6—H6	0.9500
N2—C9	1.143 (2)	C7—C8	1.494 (3)
N3—C9	1.292 (2)	C7—H7A	0.9900
N3—C10ⁱⁱ	1.299 (2)	C7—H7B	0.9900
N4—C10	1.136 (2)	C8—H8A	0.9800
O1—C1	1.334 (2)	C8—H8B	0.9800
O1—C7	1.4434 (17)	C8—H8C	0.9800
C1—C2	1.414 (2)	C10—N3ⁱⁱ	1.299 (2)
C2—C3	1.358 (3)

N4—Cd1—N4ⁱ	84.73 (9)	C1—C2—H2	120.9
N4—Cd1—N2ⁱ	86.54 (6)	C2—C3—C4	120.65 (15)
N4ⁱ—Cd1—N2ⁱ	91.14 (6)	C2—C3—H3	119.7
N4—Cd1—N2	91.14 (6)	C4—C3—H3	119.7
N4ⁱ—Cd1—N2	86.54 (6)	C3—C4—C5	117.23 (15)
N2ⁱ—Cd1—N2	176.87 (7)	C3—C4—C6	122.82 (15)
N4—Cd1—N1ⁱ	168.02 (6)	C5—C4—C6	119.94 (16)
N4ⁱ—Cd1—N1ⁱ	103.21 (5)	N1—C5—C4	122.27 (14)
N2ⁱ—Cd1—N1ⁱ	84.37 (5)	N1—C5—C5ⁱ	118.71 (8)
N2—Cd1—N1ⁱ	98.21 (5)	C4—C5—C5ⁱ	119.01 (10)
N4—Cd1—N1	103.21 (5)	C6ⁱ—C6—C4	121.04 (10)
N4ⁱ—Cd1—N1	168.02 (6)	C6ⁱ—C6—H6	119.5
N2ⁱ—Cd1—N1	98.21 (5)	C4—C6—H6	119.5
N2—Cd1—N1	84.37 (5)	O1—C7—C8	107.58 (15)
N1ⁱ—Cd1—N1	70.51 (6)	O1—C7—H7A	110.2
C1—N1—C5	118.54 (13)	C8—C7—H7A	110.2
C1—N1—Cd1	125.41 (10)	O1—C7—H7B	110.2
C5—N1—Cd1	116.03 (9)	C8—C7—H7B	110.2
C9—N2—Cd1	137.07 (14)	H7A—C7—H7B	108.5
C9—N3—C10ⁱⁱ	122.21 (15)	C7—C8—H8A	109.5
C10—N4—Cd1	160.44 (17)	C7—C8—H8B	109.5
C1—O1—C7	118.95 (13)	H8A—C8—H8B	109.5
N1—C1—O1	113.44 (13)	C7—C8—H8C	109.5
N1—C1—C2	122.96 (15)	H8A—C8—H8C	109.5
O1—C1—C2	123.59 (14)	H8B—C8—H8C	109.5
C3—C2—C1	118.28 (15)	N2—C9—N3	172.45 (18)
C3—C2—H2	120.9	N4—C10—N3ⁱⁱ	172.66 (19)

N4—Cd1—N1—C1	12.39 (13)	C5—N1—C1—C2	3.1 (2)
N4ⁱ—Cd1—N1—C1	−118.3 (2)	Cd1—N1—C1—C2	−178.36 (11)
N2ⁱ—Cd1—N1—C1	100.74 (12)	C7—O1—C1—N1	−176.54 (14)
N2—Cd1—N1—C1	−77.47 (12)	C7—O1—C1—C2	3.4 (2)
N1ⁱ—Cd1—N1—C1	−178.25 (15)	N1—C1—C2—C3	−1.7 (2)
N4—Cd1—N1—C5	−169.00 (10)	O1—C1—C2—C3	178.35 (15)
N4ⁱ—Cd1—N1—C5	60.3 (3)	C1—C2—C3—C4	−0.5 (3)
N2ⁱ—Cd1—N1—C5	−80.65 (10)	C2—C3—C4—C5	1.3 (2)
N2—Cd1—N1—C5	101.15 (10)	C2—C3—C4—C6	−177.76 (17)
N1ⁱ—Cd1—N1—C5	0.36 (7)	C1—N1—C5—C4	−2.2 (2)
N4—Cd1—N2—C9	−13.0 (2)	Cd1—N1—C5—C4	179.08 (11)
N4ⁱ—Cd1—N2—C9	−97.7 (2)	C1—N1—C5—C5ⁱ	177.68 (15)
N1ⁱ—Cd1—N2—C9	159.45 (19)	Cd1—N1—C5—C5ⁱ	−1.0 (2)
N1—Cd1—N2—C9	90.1 (2)	C3—C4—C5—N1	0.1 (2)
N4ⁱ—Cd1—N4—C10	35.8 (4)	C6—C4—C5—N1	179.14 (14)
N2ⁱ—Cd1—N4—C10	127.3 (4)	C3—C4—C5—C5ⁱ	−179.80 (16)
N2—Cd1—N4—C10	−50.6 (4)	C6—C4—C5—C5ⁱ	−0.7 (2)
N1ⁱ—Cd1—N4—C10	167.9 (3)	C3—C4—C6—C6ⁱ	178.8 (2)
N1—Cd1—N4—C10	−135.1 (4)	C5—C4—C6—C6ⁱ	−0.2 (3)
C5—N1—C1—O1	−177.02 (12)	C1—O1—C7—C8	−176.37 (14)
Cd1—N1—C1—O1	1.57 (17)

Cd1—N4	2.2980 (15)
Cd1—N2	2.3580 (16)
Cd1—N1	2.3829 (12)

N4—Cd1—N4ⁱ	84.73 (9)
N4—Cd1—N2ⁱ	86.54 (6)
N4ⁱ—Cd1—N2ⁱ	91.14 (6)
N2ⁱ—Cd1—N2	176.87 (7)
N4—Cd1—N1ⁱ	168.02 (6)
N2—Cd1—N1ⁱ	98.21 (5)
N4—Cd1—N1	103.21 (5)
N2—Cd1—N1	84.37 (5)
N1ⁱ—Cd1—N1	70.51 (6)

Symmetry code: (i) .

4 in total

1. Adsorption dynamics of gases and vapors on the nanoporous metal organic framework material Ni2(4,4'-bipyridine)3(NO3)4: guest modification of host sorption behavior.

Authors: A J Fletcher; E J Cussen; T J Prior; M J Rosseinsky; C J Kepert; K M Thomas
Journal: J Am Chem Soc Date: 2001-10-17 Impact factor: 15.419