Literature DB >> 21836948

Tris(1,10-phenanthroline)cobalt(II) bis-(trichloro-acetate).

Li-Min Li, Yu-Feng Li, Li Liu, Zeng-Hui Zhang.   

Abstract

In the title complex, [Co(C(12)H(8)N(2))(3)](C(2)Cl(3)O(2))(2), the Co(II) ion lies on a twofold rotation axis and is coordinated by six N atoms from three bis-chelating 1,10-phenanthroline ligands in a distorted octa-hedral environment. The crystal structure is stabilized by weak inter-molecular C-H⋯O hydrogen bonds.

Entities:  

Year:  2011        PMID： 21836948      PMCID： PMC3152094          DOI： 10.1107/S160053681102410X

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


Related literature

For background to metal-organic framework coordination polymers, see: Chen et al. (2001 ▶); Fang et al. (2005 ▶). For a related structure, see: Harding et al. (2008 ▶).

Experimental

Crystal data

[Co(C12H8N2)3](C2Cl3O2)2 M = 924.28 Monoclinic, a = 18.367 (4) Å b = 10.753 (2) Å c = 19.020 (4) Å β = 100.94 (3)° V = 3688.2 (13) Å3 Z = 4 Mo Kα radiation μ = 0.95 mm−1 T = 293 K 0.26 × 0.20 × 0.12 mm

Data collection

Bruker SMART CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.837, T max = 0.923 17083 measured reflections 4215 independent reflections 3364 reflections with I > 2σ(I) R int = 0.092

Refinement

R[F 2 > 2σ(F 2)] = 0.048 wR(F 2) = 0.142 S = 0.89 4215 reflections 258 parameters H-atom parameters constrained Δρmax = 0.81 e Å−3 Δρmin = −0.45 e Å−3 Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); 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 datablock(s) global, I. DOI: 10.1107/S160053681102410X/lh5253sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681102410X/lh5253Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Co(C12H8N2)3](C2Cl3O2)2F(000) = 1868
Mr = 924.28Dx = 1.665 Mg m−3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 3364 reflections
a = 18.367 (4) Åθ = 3.3–27.5°
b = 10.753 (2) ŵ = 0.95 mm−1
c = 19.020 (4) ÅT = 293 K
β = 100.94 (3)°Block, yellow
V = 3688.2 (13) Å30.26 × 0.20 × 0.12 mm
Z = 4
Bruker SMART CCD diffractometer4215 independent reflections
Radiation source: fine-focus sealed tube3364 reflections with I > 2σ(I)
graphiteRint = 0.092
Detector resolution: 9 pixels mm-1θmax = 27.5°, θmin = 3.3°
φ and ω scansh = −23→23
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)k = −13→13
Tmin = 0.837, Tmax = 0.923l = −22→24
17083 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)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.142H-atom parameters constrained
S = 0.89w = 1/[σ2(Fo2) + (0.1P)2] where P = (Fo2 + 2Fc2)/3
4215 reflections(Δ/σ)max < 0.001
258 parametersΔρmax = 0.81 e Å−3
0 restraintsΔρmin = −0.45 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
Co10.00000.08051 (4)0.25000.01371 (15)
N10.08711 (11)0.05924 (18)0.19106 (10)0.0166 (4)
N2−0.04713 (11)−0.05011 (17)0.16840 (10)0.0171 (4)
N30.05538 (10)0.23619 (17)0.30672 (9)0.0139 (4)
C10.15367 (13)0.1115 (2)0.20262 (13)0.0219 (5)
H1A0.16710.16140.24290.026*
C20.20463 (14)0.0959 (2)0.15766 (14)0.0244 (5)
H2A0.25110.13300.16860.029*
C30.18537 (14)0.0252 (2)0.09727 (13)0.0230 (5)
H3A0.21740.01750.06510.028*
C40.11654 (13)−0.0354 (2)0.08449 (12)0.0199 (5)
C50.06900 (12)−0.0155 (2)0.13273 (11)0.0163 (4)
C6−0.00237 (13)−0.0750 (2)0.12096 (12)0.0158 (4)
C7−0.02363 (13)−0.1525 (2)0.06160 (12)0.0209 (5)
C80.02684 (15)−0.1718 (2)0.01384 (13)0.0264 (5)
H8A0.0134−0.2243−0.02530.032*
C90.09337 (15)−0.1153 (3)0.02451 (13)0.0260 (5)
H9A0.1248−0.1286−0.00770.031*
C10−0.09434 (13)−0.2060 (2)0.05130 (13)0.0234 (5)
H10A−0.1101−0.25930.01290.028*
C11−0.13996 (13)−0.1790 (2)0.09837 (14)0.0239 (5)
H11A−0.1876−0.21200.09180.029*
C12−0.11401 (13)−0.1013 (2)0.15618 (13)0.0209 (5)
H12A−0.1453−0.08430.18810.025*
C130.11155 (12)0.2351 (2)0.36144 (12)0.0179 (5)
H13A0.13080.15860.37860.022*
C140.14369 (13)0.3426 (2)0.39495 (12)0.0208 (5)
H14A0.18320.33710.43350.025*
C150.11645 (13)0.4560 (2)0.37044 (12)0.0217 (5)
H15A0.13600.52850.39310.026*
C160.05858 (12)0.4615 (2)0.31049 (12)0.0173 (5)
C170.02949 (12)0.3489 (2)0.28041 (11)0.0149 (4)
C180.02748 (14)0.5754 (2)0.27896 (14)0.0225 (5)
H18A0.04570.65080.29890.027*
Cl10.18800 (5)0.41813 (7)0.18548 (4)0.0414 (2)
Cl20.06670 (4)0.51120 (9)0.07856 (5)0.0454 (2)
Cl30.17181 (4)0.67933 (6)0.15928 (4)0.0368 (2)
O10.25779 (11)0.59450 (19)0.05738 (11)0.0341 (5)
O20.19590 (11)0.41976 (17)0.02240 (10)0.0292 (4)
C200.16126 (14)0.5325 (2)0.11741 (13)0.0245 (5)
C190.21116 (12)0.5134 (2)0.05881 (12)0.0215 (5)
U11U22U33U12U13U23
Co10.0146 (2)0.0140 (2)0.0126 (2)0.0000.00274 (17)0.000
N10.0169 (9)0.0178 (9)0.0155 (9)−0.0009 (7)0.0041 (8)−0.0021 (7)
N20.0195 (9)0.0134 (9)0.0174 (9)0.0003 (7)0.0010 (8)−0.0002 (7)
N30.0144 (8)0.0157 (9)0.0111 (8)−0.0005 (7)0.0013 (7)−0.0017 (6)
C10.0217 (12)0.0256 (12)0.0189 (12)−0.0045 (10)0.0054 (10)−0.0047 (9)
C20.0184 (11)0.0283 (13)0.0276 (13)−0.0051 (10)0.0071 (10)−0.0035 (10)
C30.0237 (12)0.0279 (13)0.0198 (12)0.0033 (10)0.0101 (10)0.0014 (9)
C40.0246 (12)0.0207 (11)0.0153 (11)0.0041 (9)0.0060 (9)0.0025 (8)
C50.0186 (10)0.0160 (10)0.0140 (10)0.0028 (9)0.0025 (9)0.0009 (8)
C60.0180 (10)0.0154 (10)0.0132 (10)0.0015 (8)0.0009 (9)0.0018 (8)
C70.0260 (12)0.0181 (11)0.0164 (11)0.0019 (9)−0.0018 (10)−0.0018 (8)
C80.0363 (14)0.0254 (13)0.0174 (12)0.0043 (11)0.0047 (11)−0.0051 (9)
C90.0323 (13)0.0300 (13)0.0179 (12)0.0043 (11)0.0104 (11)−0.0027 (10)
C100.0255 (11)0.0203 (11)0.0204 (12)−0.0014 (10)−0.0059 (10)−0.0024 (9)
C110.0206 (11)0.0164 (12)0.0318 (14)−0.0016 (9)−0.0022 (10)0.0017 (9)
C120.0176 (11)0.0179 (11)0.0264 (13)−0.0005 (9)0.0023 (10)0.0006 (9)
C130.0184 (10)0.0208 (11)0.0138 (11)0.0038 (9)0.0009 (9)−0.0003 (8)
C140.0160 (10)0.0305 (13)0.0135 (10)−0.0014 (9)−0.0033 (9)−0.0025 (9)
C150.0248 (12)0.0210 (12)0.0191 (11)−0.0033 (10)0.0041 (10)−0.0047 (9)
C160.0149 (10)0.0187 (11)0.0184 (11)−0.0006 (9)0.0037 (9)−0.0009 (8)
C170.0147 (10)0.0169 (11)0.0140 (10)0.0009 (8)0.0053 (9)−0.0002 (8)
C180.0270 (12)0.0141 (11)0.0247 (12)−0.0015 (9)0.0007 (10)−0.0019 (9)
Cl10.0599 (5)0.0325 (4)0.0382 (4)0.0076 (3)0.0255 (4)0.0144 (3)
Cl20.0190 (3)0.0604 (5)0.0581 (5)−0.0049 (3)0.0110 (3)−0.0155 (4)
Cl30.0469 (4)0.0273 (4)0.0337 (4)0.0072 (3)0.0007 (3)−0.0071 (3)
O10.0268 (10)0.0393 (12)0.0367 (11)−0.0156 (8)0.0074 (9)−0.0009 (8)
O20.0271 (10)0.0328 (10)0.0277 (10)−0.0036 (8)0.0049 (8)−0.0083 (7)
C200.0221 (11)0.0250 (13)0.0258 (13)−0.0022 (10)0.0033 (10)−0.0008 (9)
C190.0148 (10)0.0309 (13)0.0176 (11)−0.0020 (9)0.0001 (9)0.0034 (9)
Co1—N1i2.1330 (19)C8—H8A0.9300
Co1—N12.1330 (19)C9—H9A0.9300
Co1—N32.1411 (18)C10—C111.368 (4)
Co1—N3i2.1411 (18)C10—H10A0.9300
Co1—N22.1497 (19)C11—C121.391 (3)
Co1—N2i2.1497 (19)C11—H11A0.9300
N1—C11.325 (3)C12—H12A0.9300
N1—C51.359 (3)C13—C141.396 (3)
N2—C121.326 (3)C13—H13A0.9300
N2—C61.358 (3)C14—C151.366 (3)
N3—C131.319 (3)C14—H14A0.9300
N3—C171.362 (3)C15—C161.405 (3)
C1—C21.393 (3)C15—H15A0.9300
C1—H1A0.9300C16—C171.401 (3)
C2—C31.366 (4)C16—C181.434 (3)
C2—H2A0.9300C17—C17i1.427 (4)
C3—C41.402 (3)C18—C18i1.345 (5)
C3—H3A0.9300C18—H18A0.9300
C4—C51.398 (3)Cl1—C201.786 (3)
C4—C91.428 (3)Cl2—C201.769 (3)
C5—C61.438 (3)Cl3—C201.762 (3)
C6—C71.398 (3)O1—C191.226 (3)
C7—C101.400 (3)O2—C191.224 (3)
C7—C81.431 (3)C20—C191.585 (3)
C8—C91.345 (4)
N1i—Co1—N1167.69 (10)C10—C7—C8123.2 (2)
N1i—Co1—N398.69 (7)C9—C8—C7121.2 (2)
N1—Co1—N390.95 (7)C9—C8—H8A119.4
N1i—Co1—N3i90.95 (7)C7—C8—H8A119.4
N1—Co1—N3i98.69 (7)C8—C9—C4121.1 (2)
N3—Co1—N3i77.14 (10)C8—C9—H9A119.4
N1i—Co1—N294.01 (8)C4—C9—H9A119.4
N1—Co1—N277.87 (7)C11—C10—C7119.2 (2)
N3—Co1—N2164.22 (7)C11—C10—H10A120.4
N3i—Co1—N293.40 (7)C7—C10—H10A120.4
N1i—Co1—N2i77.87 (7)C10—C11—C12119.0 (2)
N1—Co1—N2i94.01 (8)C10—C11—H11A120.5
N3—Co1—N2i93.40 (7)C12—C11—H11A120.5
N3i—Co1—N2i164.22 (7)N2—C12—C11123.7 (2)
N2—Co1—N2i98.40 (10)N2—C12—H12A118.1
C1—N1—C5117.5 (2)C11—C12—H12A118.1
C1—N1—Co1128.87 (16)N3—C13—C14123.5 (2)
C5—N1—Co1113.61 (15)N3—C13—H13A118.2
C12—N2—C6117.3 (2)C14—C13—H13A118.2
C12—N2—Co1129.10 (17)C15—C14—C13119.2 (2)
C6—N2—Co1113.39 (15)C15—C14—H14A120.4
C13—N3—C17117.65 (19)C13—C14—H14A120.4
C13—N3—Co1128.03 (16)C14—C15—C16119.1 (2)
C17—N3—Co1114.28 (14)C14—C15—H15A120.4
N1—C1—C2123.6 (2)C16—C15—H15A120.4
N1—C1—H1A118.2C17—C16—C15117.8 (2)
C2—C1—H1A118.2C17—C16—C18118.5 (2)
C3—C2—C1119.1 (2)C15—C16—C18123.8 (2)
C3—C2—H2A120.4N3—C17—C16122.7 (2)
C1—C2—H2A120.4N3—C17—C17i117.15 (12)
C2—C3—C4119.0 (2)C16—C17—C17i120.20 (13)
C2—C3—H3A120.5C18i—C18—C16121.32 (14)
C4—C3—H3A120.5C18i—C18—H18A119.3
C5—C4—C3118.0 (2)C16—C18—H18A119.3
C5—C4—C9119.2 (2)C19—C20—Cl3113.91 (17)
C3—C4—C9122.7 (2)C19—C20—Cl2110.03 (16)
N1—C5—C4122.6 (2)Cl3—C20—Cl2108.66 (14)
N1—C5—C6117.7 (2)C19—C20—Cl1107.71 (17)
C4—C5—C6119.6 (2)Cl3—C20—Cl1107.33 (13)
N2—C6—C7122.9 (2)Cl2—C20—Cl1109.08 (14)
N2—C6—C5117.3 (2)O2—C19—O1131.2 (2)
C7—C6—C5119.9 (2)O2—C19—C20113.8 (2)
C6—C7—C10117.9 (2)O1—C19—C20115.0 (2)
C6—C7—C8118.9 (2)
D—H···AD—HH···AD···AD—H···A
C9—H9A···O1ii0.932.543.401 (3)154
C10—H10A···O2iii0.932.353.120 (3)140
C13—H13A···O1iv0.932.283.004 (3)134
C14—H14A···O1v0.932.603.455 (3)154
C15—H15A···O2v0.932.563.266 (3)133
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
C9—H9A⋯O1i0.932.543.401 (3)154
C10—H10A⋯O2ii0.932.353.120 (3)140
C13—H13A⋯O1iii0.932.283.004 (3)134
C14—H14A⋯O1iv0.932.603.455 (3)154
C15—H15A⋯O2iv0.932.563.266 (3)133

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

  4 in total

1.  Interwoven metal-organic framework on a periodic minimal surface with extra-large pores.

Authors:  B Chen; M Eddaoudi; S T Hyde; M O'Keeffe; O M Yaghi
Journal:  Science       Date:  2001-02-09       Impact factor: 47.728

2.  A metal-organic framework with the zeolite MTN topology containing large cages of volume 2.5 nm3.

Authors:  Qianrong Fang; Guangshan Zhu; Ming Xue; Jinyu Sun; Yen Wei; Shilun Qiu; Ruren Xu
Journal:  Angew Chem Int Ed Engl       Date:  2005-06-20       Impact factor: 15.336

3.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

4.  Tris(phenanthroline-κN,N')cobalt(II) tetra-fluoridoborate acetonitrile solvate.

Authors:  David J Harding; Phimphaka Harding; Harry Adams
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2008-11-13
  4 in total
  1 in total

1.  Crystal structure of bis-[tris-(1,10-phenanthroline-κ(2) N,N')cobalt(II)] tetra-nitrate N,N'-(1,4-phenyl-enedicarbon-yl)diglycine solvate octa-hydrate.

Authors:  Niels-Patrick Pook; Philipp Hentrich; Mimoza Gjikaj
Journal:  Acta Crystallogr E Crystallogr Commun       Date:  2015-07-11
  1 in total

北京卡尤迪生物科技股份有限公司 © 2022-2023.