Home Crystal structure of catena-poly[aqua-(methanol-κO)-bis(μ2-4-(pyridin-4-yl)benzoato-κ2N:O)-bis(triphenylphospine-κP)disilver(I)], C61H52Ag2N2O6P2
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Crystal structure of catena-poly[aqua-(methanol-κO)-bis(μ2-4-(pyridin-4-yl)benzoato-κ2N:O)-bis(triphenylphospine-κP)disilver(I)], C61H52Ag2N2O6P2

  • Ning Zhu , Yan Ma , Jian-Ming Liu , Yue-Xue Li , Min Liu , Xiu-Lan Xin and Qiong-Hua Jin EMAIL logo
Published/Copyright: April 5, 2018

Abstract

C61H52Ag2N2O6P2, orthorhombic, P212121 (no. 19), a = 14.4634(11) Å, b = 17.7866(18) Å, c = 20.5509(19) Å, V = 5286.8(8) Å3, Z = 4, Rgt(F) = 0.0424, wRref(F2) = 0.0997, T = 298(2) K.

CCDC no.:: 890651

A part of the title crystal structure is shown in the figure. Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Colorless block
Size:0.40 × 0.32 × 0.21 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:0.86 mm−1
Diffractometer, scan mode:Bruker SMART, φ and ω-scans
θmax, completeness:26.3°, >99%
N(hkl)measured, N(hkl)unique, Rint:29489, 10668, 0.065
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 6633
N(param)refined:660
Programs:Bruker programs [1], SHELX [2]
Table 2:

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

AtomxyzUiso*/Ueq
Ag10.74447(4)0.52780(4)0.60076(3)0.04366(18)
Ag20.01417(4)0.02818(4)0.57824(3)0.04327(18)
N10.6348(4)0.4342(4)0.6128(3)0.0399(18)
N20.1310(4)0.9452(3)0.5934(3)0.0372(17)
O10.1115(4)0.1341(3)0.5870(3)0.0502(16)
O20.1299(4)0.1272(3)0.6947(3)0.0551(17)
O30.6351(4)0.6245(3)0.6041(3)0.0518(17)
O40.5913(4)0.6091(3)0.7064(3)0.0550(18)
O50.7537(4)0.5421(3)0.7235(2)0.0568(16)
H5B0.71310.57320.73650.068*
H5C0.80670.55880.73410.068*
O6−0.0199(5)0.0454(4)0.7039(3)0.072(2)
H6C0.02730.07060.70070.086*
P10.89828(12)0.52371(13)0.56126(9)0.0327(5)
P2−0.14252(13)0.02221(13)0.54702(10)0.0342(5)
C10.1533(6)0.1497(5)0.6383(5)0.043(2)
C20.2369(6)0.2008(4)0.6348(4)0.036(2)
C30.2828(5)0.2229(4)0.6903(4)0.040(2)
H30.26040.20850.73090.048*
C40.3623(6)0.2663(5)0.6861(4)0.042(2)
H40.39230.28050.72420.051*
C50.3978(5)0.2889(4)0.6274(4)0.034(2)
C60.3503(6)0.2665(4)0.5715(4)0.043(2)
H60.37250.28110.53100.052*
C70.2714(6)0.2236(4)0.5749(4)0.044(2)
H70.24100.20970.53690.053*
C80.5901(6)0.4241(5)0.6691(4)0.047(2)
H80.61070.45020.70560.057*
C90.5140(6)0.3763(4)0.6758(4)0.041(2)
H90.48540.37070.71600.049*
C100.4813(6)0.3374(4)0.6220(4)0.035(2)
C110.5297(6)0.3466(5)0.5644(4)0.043(2)
H110.51150.32080.52720.052*
C120.6051(6)0.3941(5)0.5624(4)0.046(2)
H120.63710.39830.52330.055*
C130.5830(6)0.6372(5)0.6509(5)0.036(2)
C140.5024(6)0.6910(4)0.6407(4)0.034(2)
C150.4480(6)0.7130(5)0.6913(4)0.046(2)
H150.46060.69470.73280.055*
C160.3750(6)0.7614(5)0.6826(4)0.048(2)
H160.33950.77600.71820.058*
C170.3539(5)0.7888(4)0.6208(4)0.035(2)
C180.4087(5)0.7662(4)0.5695(4)0.040(2)
H180.39610.78410.52790.048*
C190.4820(6)0.7173(4)0.5786(4)0.044(2)
H190.51760.70200.54330.053*
C200.1743(6)0.9389(5)0.6505(4)0.047(2)
H200.15500.96900.68490.056*
C210.2462(6)0.8898(4)0.6607(4)0.042(2)
H210.27450.88800.70130.050*
C220.2772(5)0.8429(4)0.6114(4)0.037(2)
C230.2320(6)0.8512(4)0.5520(4)0.041(2)
H230.25080.82270.51650.049*
C240.1598(6)0.9009(5)0.5451(4)0.042(2)
H240.12980.90380.50520.051*
C250.9656(5)0.6043(4)0.5886(4)0.035(2)
C260.9186(6)0.6682(5)0.6068(5)0.052(2)
H260.85440.66900.60630.062*
C270.9674(9)0.7312(5)0.6259(5)0.073(3)
H270.93550.77390.63910.087*
C281.0623(9)0.7317(6)0.6256(6)0.077(4)
H281.09440.77480.63770.092*
C291.1088(7)0.6689(6)0.6076(4)0.060(3)
H291.17310.66900.60740.071*
C301.0611(6)0.6045(5)0.5895(4)0.045(2)
H301.09360.56140.57790.054*
C310.9557(5)0.4425(4)0.5987(4)0.034(2)
C320.9506(7)0.4358(5)0.6649(4)0.058(3)
H320.92200.47370.68880.070*
C330.9863(8)0.3751(6)0.6971(5)0.070(3)
H330.98290.37230.74230.084*
C341.0272(8)0.3183(6)0.6624(6)0.068(3)
H341.05060.27650.68400.082*
C351.0336(7)0.3229(5)0.5971(6)0.062(3)
H351.06160.28450.57360.074*
C360.9977(6)0.3860(5)0.5648(4)0.052(2)
H361.00270.38940.51980.063*
C370.9250(5)0.5144(4)0.4748(4)0.0339(19)
C380.9926(6)0.5550(4)0.4436(4)0.044(2)
H381.02680.59050.46650.052*
C391.0098(6)0.5431(5)0.3783(4)0.055(3)
H391.05520.57130.35750.066*
C400.9613(7)0.4907(5)0.3438(4)0.058(3)
H400.97550.48150.30040.070*
C410.8918(7)0.4520(5)0.3738(4)0.057(3)
H410.85760.41690.35050.069*
C420.8720(5)0.4651(5)0.4387(4)0.050(2)
H420.82250.44040.45820.061*
C43−0.2084(5)0.1004(4)0.5806(4)0.035(2)
C44−0.1624(6)0.1663(5)0.5949(4)0.047(2)
H44−0.09910.16980.58760.057*
C45−0.2099(7)0.2270(5)0.6203(5)0.058(3)
H45−0.17880.27150.62930.070*
C46−0.3036(8)0.2214(6)0.6320(5)0.069(3)
H46−0.33550.26240.64900.082*
C47−0.3491(7)0.1571(6)0.6192(5)0.069(3)
H47−0.41210.15400.62790.083*
C48−0.3038(6)0.0958(5)0.5932(5)0.059(3)
H48−0.33610.05180.58410.071*
C49−0.1995(5)−0.0607(4)0.5804(4)0.035(2)
C50−0.1862(7)−0.0758(5)0.6459(5)0.059(3)
H50−0.1494−0.04410.67090.070*
C51−0.2276(7)−0.1381(5)0.6745(5)0.064(3)
H51−0.2206−0.14690.71880.076*
C52−0.2790(8)−0.1870(5)0.6369(6)0.061(3)
H52−0.3061−0.22900.65590.074*
C53−0.2901(6)−0.1741(5)0.5722(6)0.057(3)
H53−0.3239−0.20770.54690.069*
C54−0.2512(6)−0.1106(4)0.5435(4)0.046(2)
H54−0.2599−0.10170.49940.055*
C55−0.1698(5)0.0195(5)0.4605(4)0.0356(19)
C56−0.2466(6)0.0555(4)0.4336(4)0.049(2)
H56−0.28620.08290.46020.059*
C57−0.2640(6)0.0506(5)0.3679(4)0.053(3)
H57−0.31550.07450.35040.064*
C58−0.2055(7)0.0104(5)0.3279(4)0.058(3)
H58−0.21700.00780.28340.069*
C59−0.1304(6)−0.0254(6)0.3541(4)0.060(2)
H59−0.0918−0.05370.32740.072*
C60−0.1116(6)−0.0200(5)0.4200(4)0.051(2)
H60−0.0594−0.04320.43710.061*
C61−0.0840(8)0.0833(8)0.7429(5)0.097(4)
H61A−0.05990.13180.75430.146*
H61B−0.09500.05470.78180.146*
H61C−0.14090.08920.71950.146*

Source of material

The title compound was obtained by the reaction of silver(I) sulfate (0.0624 g, 0.2 mmol) and triphenylphosphine (PPh3) (0.0525 g, 0.2 mmol) in the presence of 4-pyridin-4-yl-benzoic acid (0.0398 g, 0.2 mmol) in the mixed solution of CH3OH (5 mL) and CH2Cl2 (5 mL) for 6 h at ambient temperature. The insoluble residues were removed by filtration, and the filtrate was evaporated slowly at room temperature for about 1 week to yield transparent and colorless crystals. Crystals suitable for single-crystal X-ray diffraction were selected directly from the sample as prepared.

Experimental details

Multi-scan absorption corrections were applied using SADABS program. All the structures were solved by direct methods using SHELXS program of the SHELX-2014/6 package and refined with SHELXL-2014/6 [2]. The final refinements were performed by full-matrix least-squares methods with anisotropic thermal parameters for non-hydrogen atoms on F2. The hydrogen atoms were generated geometrically and refined with fixed displacement parameters riding on the concerned atoms. The structure was refined as an inversion twin with a 0.22(4)/0.78(4) ratio of the twin components [2].

Discussion

During the past decades, a large number of silver(I) complexes with interesting structures and properties have been reported. The targeted synthesis of silver(I) complexes with designed structures and properties is still a complex task, considering that the structures and properties of complexes can be influenced by many factors, such as organic ligands, metal ions, solvent systems, and metal-to-ligand ratios [3]. These ligands including nitrogen and oxygen atoms have received widespread attention in the study of coordination chemistry. Meanwhile, heterocyclic ligands containing nitrogen and carboxyl groups are employed in many laboratories in recent years. A great deal of attention has been paid on ligands which have heterocyclic nitrogen atoms and carboxylate groups mainly because of their potential applications [4, 5] . As known to all, silver(I) salts are classified as a kind of soft acid. According to the Hard-Soft-Acid-Base (HSAB) theory, P-donor and N-donor ligands can easily coordinate to Ag(I) salts [6].

The asymmetric unit of the title structure is comprised of two Ag(I) atoms, two PPh3 ligands, two 4-pyridin-4-yl-benzoate (4,4-pybz) ligands, one water molecule and one methanol molecule. Both silver(I) metal centers are fourfold coordinated (cf. the figure) to one oxygen atom from a carboxyl fragment of the 4,4-pybz ligand, one N atom from the pyridine ring fragment of the 4,4-pybz ligand, one P atom from one PPh3 and one oxygen atom from one water or methanol molecule to establish a distorted tetrahedral geometry in each case. The metal ions of the silver(I) title complex are bridged by two 4-pyridin-4-yl-benzoate ligands to form the infinite chain structure. The two Ag—P distances are 2.3579(14) and 2.3698(13) Å, which are similar to those in [Ag2((P(C6H5))3)2(C12NO2)2(H2O)2]n (2.3599(9)−2.3686(10) Å). The angles around each Ag atom vary from 86.17(14)° to 136.49(12)°, which are similar to those in [Ag2((P(C6H5))3)2(C12NO2)2(H2O)2]n (86.84(10)°–136.87(8)°) and different from those in [Ag2((P(C6H5))3)2(C12NO2)2]⋅CH3OH (53.38(8)°–136.69(6)°)) [7]. In summary, a new Ag(I) coordination polymer was synthesized and characterized. The result will give an important information for designing and synthesizing new compounds of Ag(I) complexes using pyridylbenzoate ligands. Ag—N and Ag—O bond lengths are all in the expected ranges for such a coordination polymer [8].

Acknowledgements

This work has been supported by the National Natural Science Foundation of China (grant No. 21171119, No. 21376008) and Beijing Natural Science Foundation (grant No. 2172017, No. 2172012).

References

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Received: 2017-12-11
Accepted: 2018-3-15
Published Online: 2018-4-5
Published in Print: 2018-5-24

©2018 Ning Zhu et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

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  38. Crystal structure of 5-methyl-3,3-diphenyl-1-tosyl-1,2,3,4-tetrahydropyridine, C25H25NO2S
  39. Synthesis and crystal structure of μ-[1,1′-di(mesitylphosphanido)ferrocene]bis[η5-cyclopentadienylnickel(II)] tetrahydrofurane solvate, C42H48FeNi2OP2
  40. Synthesis and crystal structure of (E)-1-(4-(((E)-5-chloro-2-hydroxybenzylidene)amino)phenyl)ethan-1-one O-methyl oxime, C16H15ClN2O2
  41. Crystal structure of bis(1-(phenylsulfonyl)-2-(1-(pyrazin-2-yl)ethylidene)hydrazin-1-ido-κ3N,N′,O)nickel(II), C24H22N8O4S2Ni
  42. Crystal Structure of bis(1-(phenylsulfonyl)-2-(1-(pyrazin-2-yl)ethylidene)hydrazin-1-ido-κ3N,N′,O)copper(II), C24H22N8O4S2Cu
  43. Synthesis and crystal structure of poly[aqua{μ3-(1S,2S)-1-((7-hydroxy-3-(4-hydroxy-3-sulfonatophenyl)-4-oxo-4H-chromen-8-yl)methyl)pyrrolidin-1-ium-2-carboxylato-κ4O,O′:O′′:O′′′}sodium(I)] monohydrate, C21H22NNaO11S
  44. Halogen bonds in the crystal structure of 1,4-diiodotetrafluorobenzene–1,2-bis(4-pyridyl)propane (1/1), C19H14F4I2N2
  45. Crystal structure of bis(μ-N-i-propyl-N-n-propyldithiocarbamato-κ2S:S′) bis(N-i-propyl-N-n-propyldithiocarbamato-κ2S,S′)dizinc(II), C28H56N4S8Zn2
  46. Crystal structure of bis(μ-N-i-propyl-N-n-propyldithiocarbamato-κ3S,S′:S)bis(N-i-propyl-N-n-propyldithiocarbamato-κ2S,S′)dicadmium(II), C28H56Cd2N4S8
  47. Crystal structure of bis(μ2-di-n-butyldithiocarbamato-κ3S,S′:S3S:S:S′)-hexacarbonyl-di-rhenium(I), C24H36N2O6Re2
  48. Crystal structure of 7-(4-methylphenyl)imidazo[1,2-a][1,3,5]triazin-4-amine, C12H11N5
  49. Crystal structure of the co-crystal O-isopropyl phenylcarbamothioate – 4,4′-bipyridine (2/1), C15H17N2OS
  50. Crystal structure of the coordination polymer catena-poly[chlorido-{μ2-2-(((3,5-dimethyl-1H-pyrazol-1-yl)methyl)amino)-3-hydroxybutanoato-κ4N,N,O:O′}copper(II)], C11H16ClCuN2O3
  51. Synthesis and crystal structure of bis(μ2-acetato-κ2O:O′)-di(ethanol)-bis{μ2-5-(N,N′-diethylamine)-5′-methoxyl-2,2′-[ethylenediyldioxybis(nitrilomethylidyne)]diphenolato-κ6O:O,N,N,O′:O′}trinickel(II) – ethanol – acetonitrile (1/2/2), C58H86Ni3N8O18
  52. Crystal structure of the bis((E)-O-ethyl-N-phenylthiocarbamate) – 4,4′-bipyridine co-crystal (2/1), C28H30N4O2S2
  53. Crystal structure of the (E)-O-methyl-N-phenyl-thiocarbamate – 4,4′-bipyridine (1/1), C18H17N3OS
  54. Crystal structure of bis(μ2-diethyldithiocarbamato-κ3S,S′:S′)-bis(tricyclohexylphosphane-κP)dicopper(I), C46H86Cu2N2P2S4
  55. Crystal structure of N-(3-chlorophenyl)ethoxycarbothioamide, C9H10ClNOS
  56. Crystal structure of bis(μ2-pyrrolidine-1-carbodithioato-κ3S,S′:S;κ3S:S:S′)-bis(tricyclohexylphosphane-P)-di-copper(I), C46H82Cu2N2P2S4
  57. Crystal structure of N-(2-chlorophenyl)methoxycarbothioamide, C8H8ClNOS
  58. Crystal structure of chlorido-methanol-(N-(2-(oxy)-3-methoxybenzylidene)pyridine-4-carbohydrazonato-κ3O,N,O′)-(4-methylphenyl)methyl-tin(IV), C23H24ClN3O4Sn
  59. Crystal structure of N-(3-chlorophenyl)(propan-2-yloxy)carbothioamide, C10H12ClNOS
  60. Crystal structure of 1-[(Z)-[4-(4-methoxyphenyl)butan-2-ylidene]amino]-3-phenylurea, C18H21N3O2
  61. A triclinic polymorph of bis(μ-N,N-bis(2-hydroxyethyl)dithiocarbamato-κ3S,S′:S′) bis(N,N-bis(2-hydroxyethyl)dithiocarbamato-κ2S:S′)zinc(II), C20H40N4O8S8Zn2
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