Startseite Naturwissenschaften Crystal structure of catena-poly[diaqua-bis(μ2-2-(2-((2,6-dichlorophenyl)amino)phenyl)acetato-κ3O,O′:O′)calcium(II)], C56H48N4Ca2Cl8O12
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Crystal structure of catena-poly[diaqua-bis(μ2-2-(2-((2,6-dichlorophenyl)amino)phenyl)acetato-κ3O,O′:O′)calcium(II)], C56H48N4Ca2Cl8O12

  • Ying Duan EMAIL logo und Shi-Hui Li
Veröffentlicht/Copyright: 7. Februar 2018

Abstract

C56H48N4Ca2Cl8O12, monoclinic, P21/c, a = 16.776(8) Å, b = 24.193(12) Å, c = 7.657(4) Å, β = 101.110(7)°, V = 3050(3) Å3, Z = 2, Rgt(F) = 0.0685, wRref(F2) = 0.1663, T = 296(2) K.

CCDC no.: 980387

The 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:Block, colorless
Size:0.32 × 0.22 × 0.19 mm
Wavelength:Mo radiation (0.71073 Å)
μ:0.60 mm−1
Diffractometer, scan mode:Bruker SMART, φ and ω-scans
2θmax, completeness:25.5°, >98%
N(hkl)measured, N(hkl)unique, Rint:15005, 5585, 0.106
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2669
N(param)refined:372
Programs:Bruker programs [1], SHELX [2]
Table 2:

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

AtomxyzUiso*/Ueq
Ca10.31716(6)0.23340(4)0.32629(13)0.0275(3)
Cl10.59735(10)0.37297(7)1.2470(2)0.0635(5)
Cl20.60015(11)0.53917(7)0.7758(2)0.0739(6)
Cl30.05177(12)0.27575(8)0.6306(3)0.0852(7)
Cl4−0.09075(11)0.41390(9)0.1081(2)0.0862(7)
N10.0511(3)0.35264(19)0.3265(6)0.0465(13)
H10.07550.32390.29710.056*
N20.5660(3)0.42473(19)0.8782(6)0.0502(14)
H20.51850.43420.82270.060*
O10.2301(2)0.16215(16)0.1639(5)0.0498(11)
H1A0.24980.13020.19410.075*
H1B0.22760.16670.05240.075*
O20.4218(2)0.17453(15)0.4898(4)0.0473(11)
H2A0.41200.14080.45940.071*
H2B0.42220.17790.60110.071*
O30.3765(2)0.29091(15)0.5873(4)0.0375(10)
O40.4172(2)0.30954(15)0.3395(5)0.0468(11)
O50.2108(2)0.30595(14)0.3095(5)0.0415(10)
O60.2511(2)0.29626(15)0.0551(5)0.0419(10)
C10.6811(3)0.3602(3)0.8970(7)0.0467(16)
H1C0.71310.38320.97930.056*
C20.7120(4)0.3112(3)0.8482(8)0.0508(17)
H2C0.76480.30090.89910.061*
C30.6661(4)0.2776(3)0.7263(8)0.0511(17)
H30.68640.24370.69800.061*
C40.5889(4)0.2943(2)0.6446(7)0.0433(15)
H40.55910.27210.55630.052*
C50.5546(3)0.3434(2)0.6906(6)0.0321(13)
C60.6015(3)0.3754(2)0.8225(7)0.0364(14)
C70.6049(3)0.4584(2)1.0187(7)0.0391(14)
C80.6234(3)0.5132(3)0.9907(8)0.0468(16)
C90.6597(4)0.5473(3)1.1273(9)0.0598(19)
H90.67120.58401.10490.072*
C100.6787(4)0.5264(3)1.2967(9)0.066(2)
H100.70500.54881.38880.079*
C110.6594(4)0.4729(3)1.3326(8)0.0596(19)
H110.67110.45951.44860.071*
C120.6225(3)0.4393(2)1.1951(8)0.0423(15)
C130.4734(3)0.3641(2)0.5961(6)0.0335(13)
H13A0.48150.39180.50960.040*
H13B0.44600.38180.68180.040*
C140.4197(3)0.3188(2)0.5021(7)0.0298(13)
C150.1400(3)0.4124(2)0.1981(7)0.0382(14)
C160.0887(3)0.4039(2)0.3199(7)0.0377(14)
C170.0753(4)0.4467(3)0.4332(8)0.0531(17)
H170.04190.44110.51540.064*
C180.1122(4)0.4976(3)0.4225(9)0.065(2)
H180.10340.52590.49870.078*
C190.1613(4)0.5070(3)0.3018(10)0.067(2)
H190.18510.54140.29500.080*
C200.1749(3)0.4645(2)0.1902(8)0.0524(17)
H200.20810.47080.10800.063*
C210.1556(3)0.3681(2)0.0723(6)0.0382(14)
H21A0.17960.3853−0.01970.046*
H21B0.10360.35290.01490.046*
C220.2097(3)0.3207(2)0.1498(7)0.0319(13)
C23−0.0230(4)0.3452(2)0.3773(8)0.0419(15)
C24−0.0330(4)0.3102(3)0.5155(9)0.0564(18)
C25−0.1069(5)0.3013(3)0.5665(10)0.069(2)
H25−0.11080.27670.65790.083*
C26−0.1739(5)0.3291(3)0.4806(10)0.076(2)
H26−0.22350.32400.51520.092*
C27−0.1683(4)0.3649(3)0.3422(9)0.065(2)
H27−0.21360.38440.28530.078*
C28−0.0943(4)0.3711(3)0.2900(8)0.0519(17)

Source of material

A mixture of Ca(OAc)2⋅H2O (0.1 mmol, 0.0176 g), 2-(2-((2,6-dichlorophenyl)amino)phenyl)acetic acid (0.1 mmol, 891 mg), 4-(1H-pyrazol-3-yl)-pyridine (0.1 mmol, 55 mg) and distilled water (10 mL) was heated in a 25 mL steel reactor with a Teflon liner 403 K for 36 h, followed by slow cooling to room temperature. Colorless crystals of the title compound had formed.

Experimental details

Hydrogen atoms were placed in calculated positions and were included using the riding model, with Uiso(H) set to 1.2Ueq(C).

Discussion

The design and construction of metal-organic frameworks (MOFs) with well-regulated network structures has been provoked significant interest [3], [4], [5], [6]. The organic ligands, which have their differences in the size, the flexibility, the coordination ability, the number of the carboxylate groups, the positions of the carboxylate groups, play crucial roles in the construction of frameworks with interesting properties [7], [8], [9]. N-containing auxiliary ligands are known to be ideal connectors for the propagation of coordination networks [10].

The asymmetric unit of the title structure contain one Ca(II), two anionic ligands and two water molecules. The calcium atom is eight-coordinated [CdO8] by six oxygen atoms from several ligands (cf. the figure). The Ca—O bond lengths range from 2.322(4) to 2.639(4) Å, respectively. The Ca—O bond lengths of the water ligands are 2.439(4) Å and 2.414(4) Å. The bond angles of O—Ca—O are in the range of 50.57(11)°–156.20(12)°. The hydrogen bonding between carboxylate oxygen atoms and the NH group of the organic ligands are: (d(N⋯O): 2.933(6) Å, and the (d(N⋯Cl): 3.451(5) Å.

Acknowledgements

This work was supported by the Institutions of higher learning key scientific research project of Henan Province (18B150015).

References

Bruker: APEX2, SAINT and SADABS. Brucker AXS Inc., Madison, WI, USA (2009).Suche in Google Scholar

Sheldrick, G. M.: SHELXT-Integrated space-group and crystal-structure determination. Acta Crystallogr. C71 (2015) 3–8.10.1107/S2053273314026370Suche in Google Scholar PubMed PubMed Central

Li, X. L.; Liu, G. Z.; Xin, L. Y.; Wang, L. Y.: Three Zn(II) metal-organic frameworks assembled from a versatile tecton 5-ethyl-pyridine-2,3-dicarboxylate and dipyridyl-type coligand. CrystEngComm 14 (2012) 1729–1736.10.1039/C1CE06050CSuche in Google Scholar

Li, S. H.; Han, M. L.; Liu, G. Z.; Ma, L. F.; Wang, L. Y.: Guest-induced single-crystal-to-single-crystal transformations of a new 4-connected 3D cadmium(II) metal–organic framework. RSC Adv. 5 (2015) 17588–17591.10.1039/C5RA00621JSuche in Google Scholar

Yoneda, K.; Adachi, K.; Nishio, K.; Yamasaki, M.; Fuyuhiro, A.; Katada, M.; Kaizaki, S.; Kawata, S.: Organocatalytic highly enantioselective antioselective -arylation of -ketoesters/asymmetric organocatalytic -arylation of aldehydes. Angew. Chem. Int. Ed. 45 (2006) 5459–5461.10.1002/anie.200602067Suche in Google Scholar PubMed

Banerjee, A.; Singh, R.; Colacio, E.; Razak, K. K.: Binuclear copper(II) chelates with heptadentate ligands: synthesis, structure, magnetic properties, DFT studies, and catecholase and hydrolytic DNA cleavage activity. Eur. J. Inorg. Chem. 2 (2009) 277–284.10.1002/ejic.200800937Suche in Google Scholar

Li, K.; Olson, D. H.; Seidel, J.; Emge, T. J.; Gong, H.; Zeng, H.; Li, J.: Zeolitic imidazolate frameworks for kinetic separation of propane and propene. J. Am. Chem. Soc. 131 (2009) 10368–10369.10.1021/ja9039983Suche in Google Scholar PubMed

Li, S. H.; Wu, H. X.; Chai, N.: A cobalt(II) complex based on 5-methoxyisophthalic acid and 1,6-bis(1,2,4-triazol-1-yl)hexane: synthesis, crystal structure and magnetic properties. Synth. React. Inorg. Met-Org. Nan-Met. Chem. 43 (2013) 1487–1491.10.1080/15533174.2012.757750Suche in Google Scholar

Li, S. H.; Li, X. L.: A cadmium complex based on 5-methylisophthalic acid and 1,6-bis(imidazol-1-yl)hexane: synthesis, crystal structure, and photoluminescence properties. Synth. React. Inorg. Met-Org. Nan-Met. Chem. 43 (2013) 710–713.10.1080/15533174.2012.753630Suche in Google Scholar

Pachfule, P.; Panda, T.; Dey, C.; Banerjee, R.: Structural diversity in a series ofmetal-organic frameworks (MOFs) composed of divalent transition metals, 4,4′-bipyridine and a flexible carboxylic acid. CrystEngComm 12 (2010) 2381–2389.10.1039/c000723dSuche in Google Scholar

Received: 2017-6-23
Accepted: 2018-1-10
Published Online: 2018-2-7
Published in Print: 2018-3-28

©2018 Ying Duan et al., published by De Gruyter, Berlin/Boston

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

Artikel in diesem Heft

  1. Cover and Frontmatter
  2. Crystal structure and optical properties of diaqua-tris(nitrato-κ2O,O′)-bis(4,4,5,5-tetramethyl-2-(p-pyridyl)imidazoline-1-oxyl 3-oxide-κN)praseodymium(III), C24H36N9O15Pr
  3. Crystal structure of dimethanol-bis(μ2-methanol-κ2O:O)-bis{3-((4-methoxy-2-oxidobenzylidene)amino)-2-oxo-2H-chromen-4-olato-κ3O,N,O′}dimanganese(II), C38H38Mn2N2O14
  4. Crystal structure of catena-poly[diaqua-bis(μ2-2-(2-((2,6-dichlorophenyl)amino)phenyl)acetato-κ3O,O′:O′)calcium(II)], C56H48N4Ca2Cl8O12
  5. Crystal structure of catena-poly[triaqua-(isophthalato-κO)-(μ2-1,6-di(1H-imidazol-1-yl)hexane-κ2N:N′)]nickel(II), C20H28N4NiO7
  6. Crystal structure of cyclo[hexaqua-bis[1-[(2-ethyl-1H-imidazol-1-yl) methyl]-1H-benzotriazole-κ2N:N′]-bis(sulfato-κ1O)dicadmium(II)] monohydrate, C24H42Cd2N10O16S2
  7. Crystal Structure of bis(2-fluorbenzoato-κO)-bis(1,10-phenanthroline-κ2N,N′)manganese(II) dihydrate, C38H28F2MnN4O6
  8. Crystal structure of tetrapropylammonium 5-hydroxyisophthalate tetrahydrate, C20H41NO9
  9. Crystal structural of 2-amino-4-(3-bromophenyl)-3-cyano-7,7-dimethyl-5-oxo-4H-5,6,7,8-tetrahydrobenzo[b]pyran, C18H17BrN2O2
  10. Crystal structural of 2-amino-4-(4-methoxyphenyl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C17H16N2O3
  11. Crystal structure of catena-poly[aqua(μ2-1,3-bis(1H-benzo[d]imidazol-1-yl)propane-κ2N:N′)-(μ2-5-(tert-butyl)isophthalate-κ3O,O′:O′′)nickel(II)], C29H30N4NiO5
  12. Crystal structure of catena-poly[(μ2-dicyanamido-κ2N:N′)-(μ2-2-(pyridin-2-yl)ethan-1-olato-κ3N,O:O′)copper(II)], C9H8CuN4O
  13. Crystal structure of bis(5,5′-((butane-1,4-diylbis(azanylylidene))bis(methanylylidene))bis(3-(ethoxycarbonyl)-2,4-dimethylpyrrol-1-ido-k4N,N′,N′′,N′′′)copper(II), C24H32CuN4O4
  14. The crystal structure of the formamide solvate of (17b)-estra-1,3,5(10)-triene-3,17diol, C19H27NO3
  15. Crystal structure of catena-poly[diaqua-bis(μ2-1H-benzo[d]imidazole-5-carboxylato-κ2N:O)nickel(II)] dihydrate, C16H18N4NiO8
  16. Crystal structure of dibromido[(1,2-bis(diisopropylphosphino)-1,2-dicarba-closo-dodecaborane-κ2P,P′]nickel(II), C14H38B10NiBr2P2
  17. The crystal structure of catena-poly[aquachlorido(3,3′-([4,4′-bipyridine]-1,1′-diium-1,1′-diylbis(methylene))dibenzoato-κ2O:O′)copper(II)] chloride dihydrate, C26H26Cl2CuN2O7
  18. The crystal structure of N′-(2-nitrobenzylidene)-2-phenylacetohydrazide, C15H13N3O3
  19. Crystal structure of dichlorido bis[1-[(2-methyl-1H-benzoimidazol-1-yl)methyl]-1H-benzotriazole-κ1N]cadmium(II), C30H26CdCl2N10
  20. Crystal structure of aqua-bis(3-(2-pyridyl)-5-(4-pyridyl)-1H-1,2,4-triazole-κ2N,N′)copper(II) sulfate tetrahydrate, C24H28CuN10O9S
  21. Crystal structure of dibromido-carbonyl-(η6-p-cymene)osmium(II), C11H14Br2OOs
  22. Crystal structure of catena-poly[chlorido-(μ2-chlorido)-bis(imidazole-κN)copper(II)] C6H8Cl2CuN4
  23. Crystal structure of [(1,2-bis(dicyclohexylphosphino)-1,2-dicarba-closo-dodecaborane-κ2P,P′]dibromidonickel(II)), C26H54B10NiBr2P2
  24. Crystal structure of dichlorido[1,1′-bis(diphenylphosphanyl)ferrocene-κ2P,P′]zinc(II), C34H28FeCl2P2Zn
  25. Crystal structure of tris(μ2-2-(pyridin-2-yl)ethan-1-olato-κ3N,O:O)-trithiocyanato-κN-dicobalt(III), C24H24Co2N6O3S3
  26. The crystal structure of diaqua-2,2′-((cyclohexane-1,2-diylbis(azanylylidene))bis(methanylylidene))diphenolato-κ4N,N′,O,O′)manganese(III) perchlorate, C20H24MnClN2O4
  27. Crystal structure of bis(μ3-chlorido)-bis(μ2-chlorido)-tetrakis(μ2-2,6-bis (diphenylmethyl)-4-t-butylphenolato)tetralithium(I)dicobalt(II) toluene solvate, C75.5H70Cl2CoLi2O2
  28. The crystal structure of hexaaqua-bis(μ2-3-(3-(pyridin-4-yl)-1,2,4-oxadiazol-5-yl)propanoato-κ2O:O′)-tetrakis(3-(3-(pyridin-4-yl)-1,2,4-oxadiazol-5-yl)propanoato-κO)dierbium(III) octahydrate, C60H76N18O32Er2
  29. Crystal structure of dimethylammonium bis(naphthalene-2,3-diolato)borate, C22H20BNO4
  30. Crystal structure of 2-amino-4-(4-nitro-phenyl)-7,7-dimethyl-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C18H17N3O4
  31. The crystal structure of (E)-4-chloro-2-(((5-methylpyridin-2-yl)imino)methyl)phenol, C13H11ClN2O
  32. Crystal structure of bis(N,N,N-trimethylbutanaminium) poly[heptaselenidotristannate(IV)], C14H36N2Se7Sn3
  33. The crystal structure of N-((3,5-di-tert-butyl-4-hydroxyphenyl)(phenyl)methyl)-4-methylbenzenesulfonamide, C28H35N3S
  34. Crystal structure of 2-(4-chlorophenyl)-2,3-dihydro-1H-perimidine, C17H13Cl1N2
  35. The Crystal structure of 2-iodo-1-(p-tolyl)propan-1-one, C10H11IO
  36. Crystal structure of ethyl 1-(4-bromobenzyl)-3-phenyl-1H-pyrazole-5-carboxylate, C19H17BrN2O2
  37. Crystal structure of ethyl 1-(4-fluorobenzyl)-3-phenyl-1H-pyrazole-5-carboxylate, C19H17FN2O2
  38. Crystal structure of catena-poly[diaqua-(μ2-2,5-dihydroxyterephthalato-κ4O,O′:O′′,O′′′)cadmium(II)], C8H8O8Cd
  39. Crystal structure of tetraaqua-bis[6-(1H-imidazol-1-yl-κN)nicotinato]zinc(II), C18H20N6O8Zn
  40. Crystal structure of dichlorido-bis(N-phenyl-2-(quinolin-8-yloxy)acetamide-κ2N,O) – acetone (2/1), C35.5H31N4O4.5Cl2Cu
  41. Crystal Structure of ethyl (E)-3,4-dimethyl-5-((2-(4-methylbenzoyl)hydrazono)methyl)-1H-pyrrole-2-carboxylate — water — ethanol (1/1/1), C20H29N3O5
  42. Crystal structure of 5-((4-(1H-benzo[d]imidazol-2-yl)-2-methoxyphenoxy)methyl)-2-chlorothiazole - trichloromethane - methanol (1/1/1), C20H19Cl4N3O3S
  43. The crystal structure of a matrine derivative: 41S,7aS,12S,13aR,13bR)-12-(4-methylpiperazin-1-yl)dodecahydro-1H,5H,10H-dipyrido[2,1-f:3′,2′,1′-ij][1,6]naphthyridin-10-one, C20H34N4O
  44. Crystal structure of cesium beryllophosphate, Be3Cs2P4O14
  45. Crystal Structure of 3-((3-hydroxybenzyl)ammonio)-3-phenylpropanoate, C16H17NO3
  46. Crystal structure of 9,10-dimethoxy-5,6-dihydro-[1,3]dioxolo[4,5-g]isoquinolino[3,2-a]isoquinolin-7-ium chloride — 4-hydroxy-3-methoxybenzoic acid — water (2/1/5), C48H54N2Cl2O17
  47. The crystal structure of (1R, 2R)-N1,N2-diferrocenyl-1,2-cyclohexanedicarboxamide, C28H30Fe2N2O2
  48. Crystal structure of N-(2-methylphenyl)ethoxycarbothioamide, C10H13NOS
  49. Crystal Structure of ethyl (E)-2,4-dimethyl-5-((2-tosylhydrazono)methyl)-1H-pyrrole-3-carboxylate monohydrate, C17H23N3O5
  50. Crystal structure of Diiodo-(N′-((quinolin-8-yl)methylene)isonicotinohydrazide κ3N,N′,O)cadium(II) – dimethylformamide (1/1), C19H19N5O2CdI2
  51. Crystal structure of dinitrato-(N′-((quinolin-8-yl)methylene)isonicotinohydrazide κ3-N,N′,O)copper(II), C16H12N6O7Cu
  52. Crystal structure of benzoato-κO-bis(1,3,5-triaza-7-phosphaadamantane-κP)silver(I) monohydrate C19H31AgN6O3P2
  53. Crystal structure of (E)-2-(anthracen-9-ylmethylene)hydrazine-1-carbothioamide, C16H13N3S
  54. The crystal structure of 8-chloro-7-ethyl-1,3-dimethyl-1H-purine-2,6(3H,7H)-dione, C9H11ClN4O2
  55. Crystal structure of {5,5′-((propane-1,3-diylbis(azanylylidene))bis(methanylylidene))bis(3-(ethoxycarbonyl)-2,4-dimethylpyrrol-1-ido)-κ4N,N′,N′′,N′′′}zinc(II), C23H30N4O4Cu
  56. Crystal structure of bis(4-dimethylamino-pyridin-1-ium)tetrafluorosuccinate, C18H22F4N4O4
  57. Crystal structure of dimethyl 3,9-dibenzyl-6,12-dicyclohexyl-3,9-diazahexacyclo [6.4.0.02,7.04,11.05,10]-dodecane-1,11-dicarboxylate, C40H50N2O4
  58. Crystal structure of diethyl 3,9-diphenyl-6,12-bis(3-methoxyphenyl)-3,9-diazahexacyclo[6.4.0.02,7.04,11.05,10]dodecane-1,11-dicarboxylate, C42H42N2O6
  59. Crystal structure of bis(acetato-κO)-bis(1-(pyridin-2-yl)ethan-1-one oxime-κ2N,N′)nickel(II), C18H22N4NiO6
  60. Crystal structure of (N-(3-ethoxy-2-oxidobenzylidene)-4-fluorobenzohydrazonato-κ3N,O,O′)-diphenyltin(IV), C28H23FN2O3Sn
  61. Crystal structure of {N-(3-ethoxy-2-oxidobenzylidene)-4-fluorobenzohydrazonato-κ3O,N,O′}dimethyltin(IV), C18H19FN2O3Sn
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