Literature DB >> 21754322

catena-Poly[[dinitratocopper(II)]-μ-4,4''-bis-(1H-benzimidazol-1-yl)-1,1':4',1''-terphen-yl].

Hong-Shi Jiang1, Hui Li, Jian Wang, Hui-Xuan Ma, Zhe Zhang.   

Abstract

In the title one-dimensional coordination polymer, [Cu(NO(3))(2)(C(32)H(22)N(4))](n), the Cu(2+) ion (site symmetry 2) is coordinated by two nitrate O atoms and two N atoms from two 4,4'-bis-(benzoimidazol-1-yl)terphenyl (L) ligands in a distorted cis-CuN(2)O(2) square-planar coordination geometry. An alternative description of the metal coordination geometry, if long Cu-O contacts to the bonded nitrate anions are considered, is an extremely distorted cis-CuN(2)O(4) octa-hedron. The complete L ligand is generated by crystallographic twofold symmetry and connects the metal ions into infinite chains propagating in [10[Formula: see text]]. The dihedral angle between the benzimidazole ring system and the adjacent benzene (B) ring is 51.12 (11)° and the dihedral angle between the B ring and the central ring is 19.45 (13)°.

Entities:  

Year:  2011        PMID： 21754322      PMCID： PMC3089250          DOI： 10.1107/S1600536811013596

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


Related literature

For background to benzimidazole-derived ligands in coordin­ation polymers, see: Jin et al. (2006 ▶); Li et al. (2010 ▶); Su et al. (2003 ▶).

Experimental

Crystal data

[Cu(NO3)2(C32H22N4)] M = 650.10 Monoclinic, a = 14.960 (3) Å b = 15.237 (3) Å c = 12.139 (2) Å β = 103.94 (3)° V = 2685.7 (9) Å3 Z = 4 Mo Kα radiation μ = 0.88 mm−1 T = 293 K 0.20 × 0.18 × 0.15 mm

Data collection

Rigaku Mercury CCD diffractometer Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2005 ▶) T min = 0.839, T max = 0.877 13493 measured reflections 2371 independent reflections 2181 reflections with I > 2σ(I) R int = 0.044

Refinement

R[F 2 > 2σ(F 2)] = 0.044 wR(F 2) = 0.124 S = 1.09 2371 reflections 204 parameters H-atom parameters constrained Δρmax = 0.37 e Å−3 Δρmin = −0.77 e Å−3 Data collection: CrystalClear (Rigaku/MSC, 2005 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; 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/S1600536811013596/hb5843sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536811013596/hb5843Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cu(NO3)2(C32H22N4)]F(000) = 1332
Mr = 650.10Dx = 1.608 Mg m−3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 4661 reflections
a = 14.960 (3) Åθ = 1.9–28.7°
b = 15.237 (3) ŵ = 0.88 mm−1
c = 12.139 (2) ÅT = 293 K
β = 103.94 (3)°Block, green
V = 2685.7 (9) Å30.20 × 0.18 × 0.15 mm
Z = 4
Rigaku Mercury CCD diffractometer2371 independent reflections
Radiation source: fine-focus sealed tube2181 reflections with I > 2σ(I)
graphiteRint = 0.044
Detector resolution: 9 pixels mm-1θmax = 25.0°, θmin = 1.9°
ω scansh = −17→17
Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2005)k = −18→18
Tmin = 0.839, Tmax = 0.877l = −14→14
13493 measured reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.124H-atom parameters constrained
S = 1.09w = 1/[σ2(Fo2) + (0.0735P)2 + 6.1716P] where P = (Fo2 + 2Fc2)/3
2371 reflections(Δ/σ)max = 0.001
204 parametersΔρmax = 0.37 e Å−3
0 restraintsΔρmin = −0.77 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.
xyzUiso*/Ueq
Cu11.00001.08431 (3)0.75000.0158 (2)
N10.90976 (16)1.00076 (15)0.7873 (2)0.0147 (5)
N20.79830 (16)0.95918 (15)0.8684 (2)0.0127 (5)
N31.00584 (19)1.19959 (17)0.5927 (2)0.0228 (6)
C10.86254 (19)1.01906 (19)0.8646 (2)0.0149 (6)
H1A0.87331.06840.91100.018*
C20.87224 (19)0.92203 (18)0.7368 (2)0.0124 (6)
C30.89502 (19)0.87094 (19)0.6515 (2)0.0144 (6)
H3A0.94230.88720.61800.017*
C40.8443 (2)0.79544 (19)0.6192 (2)0.0176 (6)
H4A0.85870.75940.56410.021*
C50.7707 (2)0.77168 (19)0.6684 (3)0.0177 (6)
H5A0.73650.72170.64230.021*
C60.74853 (18)0.82031 (18)0.7533 (2)0.0135 (6)
H6A0.70090.80410.78620.016*
C70.80152 (19)0.89544 (18)0.7875 (2)0.0119 (6)
C80.73918 (18)0.96045 (18)0.9471 (2)0.0114 (6)
C90.7327 (2)0.8866 (2)1.0116 (3)0.0189 (7)
H9A0.76670.83651.00550.023*
C100.6748 (2)0.88846 (19)1.0852 (3)0.0180 (6)
H10A0.66960.83861.12730.022*
C110.62384 (18)0.96369 (18)1.0978 (2)0.0113 (6)
C120.63268 (18)1.03720 (18)1.0321 (2)0.0112 (6)
H12A0.60001.08801.03910.013*
C130.68927 (19)1.03586 (18)0.9565 (2)0.0116 (6)
H13A0.69371.08500.91270.014*
C140.56072 (18)0.96408 (18)1.1761 (2)0.0108 (6)
C150.52982 (19)1.04264 (18)1.2139 (2)0.0129 (6)
H15A0.54941.09581.19030.015*
C160.52938 (19)0.88512 (19)1.2128 (2)0.0126 (6)
H16A0.54780.83201.18750.015*
O11.06322 (14)1.18409 (14)0.68862 (19)0.0224 (5)
O21.01639 (19)1.26531 (16)0.5384 (2)0.0373 (6)
O30.94347 (17)1.14482 (17)0.5587 (2)0.0352 (6)
U11U22U33U12U13U23
Cu10.0152 (3)0.0149 (3)0.0202 (3)0.0000.0099 (2)0.000
N10.0161 (12)0.0147 (12)0.0160 (12)−0.0024 (10)0.0092 (10)−0.0034 (10)
N20.0140 (12)0.0135 (12)0.0132 (12)0.0014 (9)0.0084 (10)−0.0008 (9)
N30.0290 (15)0.0182 (14)0.0267 (15)0.0031 (11)0.0172 (13)0.0032 (12)
C10.0163 (14)0.0151 (14)0.0151 (14)−0.0004 (11)0.0070 (12)−0.0004 (12)
C20.0091 (13)0.0161 (14)0.0119 (14)−0.0013 (10)0.0024 (11)0.0011 (11)
C30.0115 (13)0.0217 (15)0.0117 (14)0.0037 (11)0.0061 (11)0.0003 (12)
C40.0203 (15)0.0170 (15)0.0152 (15)0.0047 (12)0.0037 (12)−0.0035 (12)
C50.0196 (15)0.0118 (14)0.0202 (16)−0.0010 (12)0.0020 (12)−0.0021 (12)
C60.0097 (13)0.0134 (13)0.0182 (15)0.0005 (11)0.0050 (12)0.0044 (11)
C70.0130 (13)0.0130 (13)0.0108 (14)0.0031 (11)0.0053 (11)0.0014 (11)
C80.0100 (13)0.0145 (14)0.0127 (14)−0.0015 (11)0.0085 (11)−0.0011 (11)
C90.0200 (16)0.0161 (15)0.0262 (17)0.0077 (12)0.0164 (13)0.0053 (13)
C100.0199 (15)0.0145 (15)0.0239 (16)0.0048 (12)0.0140 (13)0.0085 (12)
C110.0103 (13)0.0148 (14)0.0097 (13)−0.0005 (11)0.0040 (11)0.0004 (11)
C120.0112 (13)0.0119 (14)0.0113 (13)0.0003 (10)0.0044 (11)−0.0013 (11)
C130.0140 (13)0.0118 (13)0.0100 (13)−0.0020 (11)0.0048 (11)0.0015 (11)
C140.0096 (13)0.0156 (14)0.0086 (13)0.0006 (10)0.0046 (11)0.0010 (11)
C150.0134 (13)0.0118 (14)0.0156 (14)−0.0011 (11)0.0078 (12)0.0019 (11)
C160.0142 (13)0.0130 (14)0.0129 (14)0.0015 (11)0.0080 (12)−0.0003 (11)
O10.0206 (11)0.0194 (11)0.0294 (12)−0.0026 (9)0.0102 (10)−0.0009 (9)
O20.0480 (16)0.0246 (13)0.0474 (16)0.0038 (11)0.0273 (13)0.0133 (12)
O30.0337 (14)0.0330 (14)0.0357 (14)−0.0083 (11)0.0020 (12)0.0044 (11)
Cu1—N11.985 (2)C5—C61.373 (4)
Cu1—N1i1.985 (2)C5—H5A0.9300
Cu1—O1i2.025 (2)C6—C71.398 (4)
Cu1—O12.025 (2)C6—H6A0.9300
Cu1—O32.452 (3)C8—C91.388 (4)
Cu1—O3i2.452 (3)C8—C131.390 (4)
N1—C11.333 (4)C9—C101.386 (4)
N1—C21.401 (4)C9—H9A0.9300
N2—C11.334 (4)C10—C111.406 (4)
N2—C71.390 (4)C10—H10A0.9300
N2—C81.450 (3)C11—C121.400 (4)
N3—O21.230 (3)C11—C141.493 (4)
N3—O31.246 (4)C12—C131.390 (4)
N3—O11.291 (4)C12—H12A0.9300
C1—H1A0.9300C13—H13A0.9300
C2—C31.401 (4)C14—C151.400 (4)
C2—C71.406 (4)C14—C161.402 (4)
C3—C41.382 (4)C15—C15ii1.394 (5)
C3—H3A0.9300C15—H15A0.9300
C4—C51.420 (4)C16—C16ii1.404 (5)
C4—H4A0.9300C16—H16A0.9300
N1—Cu1—N1i100.24 (14)C7—C6—H6A121.9
N1—Cu1—O1i89.66 (9)N2—C7—C6131.9 (3)
N1i—Cu1—O1i165.63 (9)N2—C7—C2105.4 (2)
N1—Cu1—O1165.63 (9)C6—C7—C2122.6 (3)
N1i—Cu1—O189.66 (9)C9—C8—C13120.8 (3)
O1i—Cu1—O182.68 (12)C9—C8—N2119.8 (2)
C1—N1—C2105.2 (2)C13—C8—N2119.4 (2)
C1—N1—Cu1122.08 (19)C10—C9—C8119.1 (3)
C2—N1—Cu1132.22 (19)C10—C9—H9A120.5
C1—N2—C7107.8 (2)C8—C9—H9A120.5
C1—N2—C8124.9 (2)C9—C10—C11121.8 (3)
C7—N2—C8127.2 (2)C9—C10—H10A119.1
O2—N3—O3123.4 (3)C11—C10—H10A119.1
O2—N3—O1119.3 (3)C12—C11—C10117.5 (3)
O3—N3—O1117.3 (2)C12—C11—C14121.4 (2)
N1—C1—N2112.9 (3)C10—C11—C14121.0 (2)
N1—C1—H1A123.5C13—C12—C11121.4 (3)
N2—C1—H1A123.5C13—C12—H12A119.3
C3—C2—N1131.0 (3)C11—C12—H12A119.3
C3—C2—C7120.4 (3)C8—C13—C12119.4 (3)
N1—C2—C7108.6 (2)C8—C13—H13A120.3
C4—C3—C2117.2 (3)C12—C13—H13A120.3
C4—C3—H3A121.4C15—C14—C16117.9 (3)
C2—C3—H3A121.4C15—C14—C11121.4 (2)
C3—C4—C5121.4 (3)C16—C14—C11120.7 (2)
C3—C4—H4A119.3C15ii—C15—C14121.21 (16)
C5—C4—H4A119.3C15ii—C15—H15A119.4
C6—C5—C4122.0 (3)C14—C15—H15A119.4
C6—C5—H5A119.0C14—C16—C16ii120.89 (16)
C4—C5—H5A119.0C14—C16—H16A119.6
C5—C6—C7116.3 (3)C16ii—C16—H16A119.6
C5—C6—H6A121.9N3—O1—Cu1101.61 (16)
N1i—Cu1—N1—C1147.7 (3)N1—C2—C7—C6178.1 (2)
O1i—Cu1—N1—C1−21.8 (2)C1—N2—C8—C9−128.1 (3)
O1—Cu1—N1—C1−79.4 (4)C7—N2—C8—C949.3 (4)
N1i—Cu1—N1—C2−41.6 (2)C1—N2—C8—C1352.2 (4)
O1i—Cu1—N1—C2148.9 (3)C7—N2—C8—C13−130.4 (3)
O1—Cu1—N1—C291.3 (4)C13—C8—C9—C100.6 (4)
C2—N1—C1—N20.1 (3)N2—C8—C9—C10−179.1 (3)
Cu1—N1—C1—N2173.00 (18)C8—C9—C10—C11−1.2 (5)
C7—N2—C1—N1−0.3 (3)C9—C10—C11—C120.7 (4)
C8—N2—C1—N1177.6 (2)C9—C10—C11—C14179.0 (3)
C1—N1—C2—C3−179.0 (3)C10—C11—C12—C130.4 (4)
Cu1—N1—C2—C39.1 (5)C14—C11—C12—C13−178.0 (3)
C1—N1—C2—C70.1 (3)C9—C8—C13—C120.4 (4)
Cu1—N1—C2—C7−171.8 (2)N2—C8—C13—C12−179.9 (2)
N1—C2—C3—C4−179.9 (3)C11—C12—C13—C8−0.9 (4)
C7—C2—C3—C41.0 (4)C12—C11—C14—C15−19.7 (4)
C2—C3—C4—C51.5 (4)C10—C11—C14—C15161.9 (3)
C3—C4—C5—C6−2.7 (4)C12—C11—C14—C16159.3 (3)
C4—C5—C6—C71.0 (4)C10—C11—C14—C16−19.0 (4)
C1—N2—C7—C6−177.8 (3)C16—C14—C15—C15ii0.4 (5)
C8—N2—C7—C64.5 (5)C11—C14—C15—C15ii179.4 (3)
C1—N2—C7—C20.3 (3)C15—C14—C16—C16ii−1.5 (5)
C8—N2—C7—C2−177.4 (3)C11—C14—C16—C16ii179.5 (3)
C5—C6—C7—N2179.4 (3)O2—N3—O1—Cu1170.1 (2)
C5—C6—C7—C21.6 (4)O3—N3—O1—Cu1−11.7 (3)
C3—C2—C7—N2179.0 (3)N1—Cu1—O1—N3−28.9 (4)
N1—C2—C7—N2−0.2 (3)N1i—Cu1—O1—N3105.01 (17)
C3—C2—C7—C6−2.7 (4)O1i—Cu1—O1—N3−87.19 (17)
Table 1

Selected bond lengths (Å)

Cu1—N11.985 (2)
Cu1—O12.025 (2)
Cu1—O32.452 (3)
  3 in total

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  3 in total

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