Startseite Crystal structure of poly[(μ6-ammoniotris(methylene))tris(hydrogen phosphonato)cadmium(II)], C3H10CdNO9P3
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Crystal structure of poly[(μ6-ammoniotris(methylene))tris(hydrogen phosphonato)cadmium(II)], C3H10CdNO9P3

  • Si N. Gu , Zhi Y. Ou , Ting T. Wu , Ting Y. Nie und Yang Liu ORCID logo EMAIL logo
Veröffentlicht/Copyright: 26. September 2023

Abstract

C3H10CdNO9P3, monoclinic, P21/c (no. 14), a = 9.1770(5) Å, b = 8.3742(4) Å, c = 15.4660(6) Å, β = 119.657(2)°, V = 1032.86(9) Å3, Z = 4, R gt (F) = 0.0202, wRref(F2) = 0.0515, T = 296 K.

CCDC no.: 2281782

The molecular structure is shown in the figure. Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal: Colourless block
Size: 0.20 × 0.20 × 0.20 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 2.62 mm−1
Diffractometer, scan mode: Bruker SMART CCD 6000,
θmax, completeness: 27.6°, >99 %
N(hkl)measured, N(hkl)unique, Rint: 12229, 2370, 0.020
Criterion for Iobs, N(hkl)gt: Iobs > 2 σ(Iobs), 2322
N(param)refined: 157
Programs: Bruker [1], OLEX2 [2], SHELX [3]
Table 2:

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

Atom x y z Uiso*/Ueq
Cd1 −0.47676 (2) −0.05304 (2) −0.75041 (2) 0.01582 (6)
P1 −0.42787 (8) −0.29929 (7) −0.55102 (4) 0.01415 (12)
P2 −0.17571 (8) 0.20844 (8) −0.58821 (5) 0.01633 (13)
P3 −0.18609 (7) −0.32297 (7) −0.73982 (4) 0.01392 (12)
O3 −0.4420 (3) −0.1548 (2) −0.61112 (14) 0.0264 (4)
O1 −0.4689 (2) −0.4616 (2) −0.59943 (13) 0.0194 (4)
O2 −0.5359 (2) −0.2676 (2) −0.49969 (14) 0.0227 (4)
H2 −0.5391 −0.3488 −0.4710 0.034*
O4 −0.3566 (2) 0.1922 (2) −0.67055 (13) 0.0187 (4)
O5 −0.1146 (3) 0.1155 (3) −0.49404 (14) 0.0271 (4)
O6 −0.1328 (3) 0.3857 (2) −0.55129 (14) 0.0260 (4)
H6 −0.1710 0.4459 −0.5994 0.039*
O8 −0.2608 (2) −0.1596 (2) −0.76055 (14) 0.0221 (4)
O7 0.0076 (2) −0.3163 (3) −0.66683 (14) 0.0235 (4)
H7 0.0277 −0.2524 −0.6221 0.035*
O9 −0.7324 (2) 0.0571 (2) −0.79548 (14) 0.0222 (4)
N1 −0.1298 (2) −0.1569 (2) −0.40785 (14) 0.0131 (4)
H1 −0.1546 −0.0853 −0.4636 0.016*
C1 −0.2094 (3) −0.3143 (3) −0.45269 (18) 0.0177 (5)
H1A −0.2034 −0.3829 −0.4005 0.021*
H1B −0.1453 −0.3648 −0.4797 0.021*
C2 −0.0584 (3) 0.1673 (3) −0.65317 (18) 0.0179 (5)
H2A −0.0992 0.0672 −0.6886 0.021*
H2B −0.0858 0.2502 −0.7027 0.021*
C3 −0.2027 (3) −0.4205 (3) −0.84996 (17) 0.0145 (4)
H3A −0.1515 −0.5250 −0.8295 0.017*
H3B −0.3210 −0.4379 −0.8958 0.017*

1 Source of materials

Cd(NO3)2·4H2O (0.3 mmol, 0.093) was dissolved in 8 mL water, followed by the addition of a 50 % solution of nitrilo-tris(methylenephosphonic acid) (0.3 mL). Then the mixture was transferred into a 25 mL Teflon-lined stainless-steel vessel, which was followed by heated at 140 °C under autogenous pressure for 2 days. After the mixture was cooled to room temperature, colorless block crystals were obtained, washed with ethanol, and dried at room temperature.

2 Experimental details

The structures were solved by Direct Methods using the Shelx-97 program incorporated into Olex2. Empirical absorption corrections were applied with Sadabs. The hydrogen atoms bonded to nitrogen and oxygen atoms were included in geometric positions and given thermal parameters equivalent to 1.2 times those of the atom to which they were attached [1], [2], [3].

3 Comment

Organophosphonate-based complexes have received continuous attention owing to their structural diversity and potential applications in catalysis, absorption, separation, and so on [4], [5], [6], [7], [8], [9]. Nitrilo-tris(methylenephosphonic acid) (NTMP) is known as a functionalized flexible triphosphonate ligand with a promising ligation ability due to the large number and steric availability of donor oxygen atoms.

Crystal structure analysis reveals that the asymmetric unit contains one central Cd(II) atom and one ligand. Each Cd atom is octahedrally coordinated by six phosphonate oxygen atoms from six different ligands. The Cd–O distances range from 2.1882(18) to 2.5562(18) Å, which are comparable with those of the reported Cd organotriphosphonate analogues [10, 11]. Three phosphonate and the amine groups are uniformly 1H-protonated, guaranteeing electric neutrality of the full moiety. The ligand adopts a m6-hexadentate coordination mode. Two neighboring Cd atoms are triply bridged by two {PO3} groups and the μ2–O atom (O4) of another {PO3} group, leading to a densely compact 3D framework.


Corresponding author: Yang Liu, Key Laboratory of Functional Organometallic Materials, College of Chemistry and Materials Science, Hengyang Normal University, Hengyang City, 421008, Hunan Province, People’s Republic of China, E-mail:

Funding source: the Foundation of Key Laboratory of Functional Metal-Organic Compounds of Hunan Province 2022HSKFJJ027

  1. Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Research funding: Foundation of Key Laboratory of Functional Metal-Organic Compounds of Hunan Province (2022HSKFJJ027).

  3. Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

References

1. Bruker. SAINT and SADABS; Bruker AXS Inc.: Madison, Wisconsin, USA, 2000.Suche in Google Scholar

2. Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K., Puschmann, H. OLEX2: a Complete structure solution, refinement and analysis program. J. Appl. Crystallogr. 2009, 42, 339–341; https://doi.org/10.1107/s0021889808042726.Suche in Google Scholar

3. Sheldrick, G. M. Crystal structure refinement with SHELXL. Acta Crystallogr. 2015, C71, 3; https://doi.org/10.1107/s2053229614024218.Suche in Google Scholar

4. Wang, G. M., Li, J. H., Pan, J., Xue, Z. Z., Wei, L., Han, S. D., Bao, Z. Z., Wang, Z. H. Two hybrid transition metal triphosphonates decorated with a tripodal imidazole ligand: synthesis, structures and properties. Dalton Trans. 2017, 46, 808–813; https://doi.org/10.1039/c6dt04363a.Suche in Google Scholar PubMed

5. Xu, Q., Xu, B., Kong, H., He, P., Wang, J., Kannan, T., Ma, P., Wang, J., Niu, J. Synthesis and characterization of a crown-shaped 36-molybdate cluster and application in catalyzing knoevenagel condensation. Inorg. Chem. 2020, 59, 10665–10672.10.1021/acs.inorgchem.0c01122Suche in Google Scholar PubMed

6. Chausov, F. F., Lomova, N. V., Somov, N. V., Kazantseva, I. S., Kholzakov, A. V., Sapozhnikov, G. V., Zakirova, R. M. Competitive formation of crystalline phases and its structural properties within the system [CuxNi(1−x){N(CH2PO3)3}]Na4·nH2O (x= 0…1). J. Cryst. Growth 2019, 4, 125187; https://doi.org/10.1016/j.jcrysgro.2019.125187.Suche in Google Scholar

7. Mao, J. G., Wang, Z., Clearfield, A. Hydrothermal synthesis, characterization and crystal structures of two new zinc (ii) phosphonates: Zn2[(O3PCH2)2NHCH2CO2] and Zn2[HO3PCH2NH(CH2PO3)2]. New J. Chem. 2002, 26, 1010–1014; https://doi.org/10.1039/b202096n.Suche in Google Scholar

8. Fu, R., Hu, S., Wu, X. Syntheses, structures, thermal stabilities and luminescence of two new 3D zinc phosphonates. J. Solid State Chem. 2011, 184, 159–163; https://doi.org/10.1016/j.jssc.2010.11.013.Suche in Google Scholar

9. Silva, P., Vieira, F., Gomes, A. C., Ananias, D., Fernandes, J. A., Bruno, S. M., Soares, R., Valente, A. A., Rocha, J., Paz, F. A. A. Thermal transformation of a layered multifunctional network into a metal–organic framework based on a polymeric organic linker. J. Am. Chem. Soc. 2011, 133, 15120–15138; https://doi.org/10.1021/ja205243w.Suche in Google Scholar PubMed

10. Chausov, F. F., Kazantseva, I. S., Reshetnikov, S. M., Lomova, N. V., Maratkanova, A. N., Somov, N. V. Zinc and cadmium nitrilotris (methylenephosphonate) s: a comparative study of different coordination Structures for corrosion inhibition of steels in neutral aqueous media. ChemistrySelect 2020, 5, 13711–13719; https://doi.org/10.1002/slct.202003255.Suche in Google Scholar

11. Wang, B., Man, X. Crystal structure of poly[triaqua-(di(2,2′-bipyridine-κ2N,N′)-μ4-silanetetrayltetrakis(benzene-4,1-diyl)tetrakis (hydrogen phosphonato)-κ4O:O′:O′′:O′′′) dicadmium(II)], C44H42N4O15P4Cd2Si. Z. Kristallogr. N. Cryst. Struct. 2020, 235, 1361–1363; https://doi.org/10.1016/j.jssc.2010.11.013.Suche in Google Scholar

Received: 2023-07-18
Accepted: 2023-08-20
Published Online: 2023-09-26
Published in Print: 2023-12-15

© 2023 the author(s), published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution 4.0 International License.

Artikel in diesem Heft

  1. Frontmatter
  2. New Crystal Structures
  3. Crystal structure of bis(dimethylammonium) poly[(μ4-1,1′-(1,4-phenylenebis(methylene))bis(1H-pyrazole-3,5-dicarboxylato))-κ6O1, N2:O2:O3:O1′,N2′]nickel (II)], C22H26N6NiO8
  4. Hydrothermal synthesis and crystal structure of catena-poly[diaqua-bis(μ2-4-((pyridin-4-ylmethyl)amino)benzoato-κ2N:O)cobalt(II)] 4,4′-bipyridine – water (1/2/2)
  5. Crystal structure of (2S,3S,4S,5S, Z)-2,3,5,6-tetrakis(benzyloxy)-4-hydroxyhexanal oxime, C34H37NO6
  6. The crystal structure of hexakis(3-thiophenecarboxylato-κ2O,O″)-bis(1,10-phenanthroline-κ2N,N′) trimanganese(II), C54H34N4O12S6Mn3
  7. Crystal structure of catena-poly[(μ2-1,4-di(pyridin-4-yl)benzene-κ2N:N′)-(4-bromobenzoate-κ2O:O′)-(μ-2-bromobenzoate-κ2O,O′)nickel(II)] – water (2/1), C30H21Br2N2NiO4.5
  8. The crystal structure of poly[(μ3-1,3-phenylenedioxydiacetate-κ5O,O,O′,O″,O‴)-bis(4′-(4-(1H-imidazol-1-yl)phenyl)-4,2′:6′,4″-terpyridine-kN) cadmium(II)], C58H42CdN10O6
  9. The crystal structure of 5-chloro-6′-methyl-3-(4-(methylsulfonyl)phenyl)-[2,3′-bipyridin]-1′-ium 4-methylbenzenesulfonate
  10. Crystal structure of poly[(μ-benzoato)-(μ-cis-4–hydroxy-D-proline)lithium], C12H14LiNO5
  11. The crystal structure of catena-poly[aqua-(4-iodopyridine-2,6-dicarboxylato-κ3N,O,O)-copper(II)] monohydrate, C7H6NO6ICu
  12. The crystal structure of catena-[diaqua-(4-acetylphenoxyacetato-κ2O,O)-bis(4-acetylphenoxyacetato-κ3O,O:O)-dihydrate-lanthanum(III)]–4,4′-bipyridine (2/1), C35H35NO14La
  13. The crystal structure of catena-poly[(4-iodopyridine-2,6-dicarboxylato-κ4 O,N,O′,O′′)(4-imidazol-1-yl-pyridine-κN)copper(II)], C15H9N4O4ICu
  14. Crystal structure of polybis(μ 4-3,5-dicarboxylatopyrazol-1-yl)-bis(N,N-dimethylformamide)tri-copper(II)–acetonitrile (1/2), C20H22Cu3N8O10
  15. Crystal structure of poly[(μ2-5-hydroxy-isophthalato-κ4O,O′:O″,O‴)-(μ2-1,5-bis(imidazol-2-methyl)pentane-κ2N:N′)cadmium(II)], C21H24CdN4O5
  16. The crystal structure of poly[bis(μ2-1,4-bi(1-imidazolyl)benzene-κ2N:N′)bis(μ2-4,4′-methylenebis(3-hydroxy-2-naphthoate)-κ2O:O′)cobalt(II)], C35H24CoN4O6
  17. The crystal structure of a cobalt-vanadium-oxido hydrate
  18. The crystal structure of catena-poly[(μ 2-2H-1,2,3-triazole-4,5-dicarboxylato-κ 2 O, O′)-(μ 2-1,3-bis((1H-imidazol-1-yl)methyl)benzene-κ 2 N,N′) zinc(II)], C18H15N7O4Zn
  19. Crystal structure of poly[diaqua-(bis(m2-1,4-bis(imidazol-1-ylmethyl)benzene)-κ2N,N′-manganese] dichloride, C28H32MnN8O2Cl2
  20. The crystal structure of 9,10-dimethoxy-5,6-dihydro-[1,3]dioxolo[4,5-g]isoquinolino [3,2-a]isoquinolin-7-ium (E)-3-(4-nitrophenyl)acrylate pentahydrate, C29H34N2O13
  21. Crystal structure of poly[(μ6-ammoniotris(methylene))tris(hydrogen phosphonato)cadmium(II)], C3H10CdNO9P3
  22. Crystal structure of Zn2[(1,1′-(hexane-1,6-diyl)bis(3-(pyridin-3-yl)urea))·(H2O)2·(DMF)2·(SO4)2], C24H50N8O18S2Zn2
  23. The crystal structure of 2-anilino-1,4-naphthoquinone, C10H11NO2
  24. Crystal structure of (E)-2-(2-(4-(diethylamino)styryl)-1-ethyl-1,4-dihydroquinolin-4-yl) malononitrile, C26H26N4
  25. Crystal structure of ethyl 2-((2,6-dichloro-4-(cyanomethyl)phenyl) amino)benzoate, C17H14Cl2N2O2
  26. Synthesis and crystal structure of 2-(3-oxo-3-phenylpropyl)isoindoline-1,3-dione, C17H13NO3
  27. The crystal structure of bis(acetonitrile-κ1N)tetrakis(μ2-2,6-difluorobenzoato-κ2O:O′)rhodium(II) (Rh–Rh), C32H18F8O8N2Rh2
  28. The crystal structure of a new polymorph of 6-hydroxy-2-naphthoic acid, C11H8O3
  29. The crystal structure of [(8-carboxymethoxy-quinoline-2-carboxylate-κ4N,O,O,O)-2,2′-bipyridine-κ2N-copper(II)] tetrahydrate, C22H23N3O9Cu
  30. The crystal structure of ethyl 4-hydroxy-2-(4-methoxyphenyl)-5-oxo-1-(2-oxo-2H-chromen-6-yl)-2,5-dihydro-1H-pyrrole-3-carboxylate, C23H19NO7
  31. Crystal structure of 7-hydroxy-3,4-dihydronaphthalen-1(2H)-one, C10H10O2
  32. Crystal structure of bis(tetrapropylammonium) dodecacarbonyltetratelluridotetraferrate(2-), (Pr4N)2[Fe4Te4(CO)12]
  33. The crystal structure of poly[bis(μ2−3−aminopyridine−4−carboxylatoκ2N:O)Zinc(II)], [Zn(C6H5N2O2)2] n
  34. The crystal structure of methyl 5-nitro-2-(tosyloxy)benzoate, C15H13NO7S
  35. The crystal structure of 18-crown-6 ― tetraaqua-dichlorido-di-μ2-chloridodicopper(II) (2/1), C12H32O10Cu2Cl4
  36. Crystal structure of 6,6a,7,8,9,10-hexahydro-5H-pyrazino [2,3-e]pyrido[1,2-a]pyrazine, C10H14N4
  37. Crystal structure of catena-poly-{diaqua-bis[μ-(((4-chlorophenyl)sulfonyl)glycinato-κO)](μ2-4, 4′-bipyridine-κ2N:N′)cobalt(II)} dihydrate, C26H30Cl2CoN4O12S2
  38. Crystal structure of bis{N′-[1,3-diphenylprop-2-en-1-ylidene]-N-phenylcarbamohydrazonothioato}zinc(II), C44H36N6S2Zn
  39. Crystal structure of tetraaqua-bis(((4-chlorophenyl)sulfonyl)glycinato-κO)cobalt(II) dihydrate, C16H26Cl2CoN2O14S2
  40. Crystal structure of 2-(5-phenyl-1-(quinolin-2-yl)-4,5-dihydro-1H-pyrazol-3-yl)phenol, C24H19N3O
  41. Crystal structure of 2-((2-fluoro-4-(trifluoromethyl)phenyl)(hydroxy)methyl)-7-methoxy-3,4-dihydronaphthalen-1((2H))-one, C19H16F4O3
  42. Crystal structure of 2-amino-4-(2-fluoro-3-(trifluoromethyl)phenyl)-9-methoxy-1,4,5,6-tetrahydrobenzo[h]quinazolin-3-ium chloride, C20H18ClF4N3O
  43. Crystal structure of (2-phenylimino methylquinoline-κ 2 N,N′)-bis(1–phenylpyrazole-κ 2 C,N)-iridium(III) hexafluorophosphate, C34H26F6IrN6P
  44. Crystal structure of (3-hydroxy-4-methoxyphenyl)(pyrrolidin-1-yl)methanone, C12H15NO3
  45. The crystal structure of bis(trimethylsulfoxonium) catena-poly[µ2-hexabromido-indium(III)sodium(I)] C6H18O2S2NaInBr6
  46. Crystal structure of N-cyclopropyl-3-hydroxy-4-methoxybenzamide, C11H13NO3
  47. The crystal structure of (bis(benzimidazol-2-yl-methyl)amine-κ3N,N,N )-(dihydrogen L-malate-κ2O,O )copper(II) perchlorate dihydrate, CuC20H24ClN5O12
  48. Crystal structure of (1E,1′E)-4,4′-(9,9-diethyl-9H-fluorene-2,7-diyl)dibenzaldehyde dioxime, C31H28N2O2
  49. Crystal structure of diethyl 1,9-bis(4-fluorophenyl)-4,6-diphenylhexahydro-3H-2,7,3,5-(epimethanetriyliminomethanetriyl)cyclopenta [b]pyridine-3,7(2H)-dicarboxylate, C40H36F2N2O4
  50. Crystal structure of bis(benzene-1 carboxylato-O 3,5-carboxyl-κ1O)-[(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ4N,N′,N′′,N′′′)nickel(II) ─ benzene-1,3,5-tricarboxylic acid ─ water (1/2/4), C52H66N4NiO28
  51. Crystal structure of 1,4-dibromo-2,5-bis(2-methoxyethoxy)benzene-1,4-diol, C12H16Br2O4
  52. Crystal structure of dicarbonyl[N,N′-(1,2-dimethyl-1,2-ethanediylidene)bis[2,6-bis(1-methylethyl)benzenamine]-N,N′]nickel(0), C30H40N2NiO2
  53. Crystal structure of 1,4-dibromo-2,5-bis(prop-2-yn-1-yloxy)benzene, C12H8Br2O2
  54. Crystal structure of O-(3-(benzo[d]thiazol-2-yl)naphthalen-2-yl) O-phenyl carbonothioate, C24H15NO2S2
  55. The crystal structure of (E)-4-fluoro-N′-(1-(4-hydroxyphenyl)propylidene)benzohydrazide, C16H15FN2O2
  56. Crystal structure of (E)-1-(benzo[d]thiazol-2-yl)-N-(4,5-dihydropyren-2-yl)methanimine, C24H16N2S
  57. Crystal structure of 3-((4-bromophenyl)thio)-1H-indole, C14H10BrNS
  58. Synthesis and crystal structure of 1-((7-hydroxy-3-(4-hydroxy-3-nitrophenyl)-4-oxo-4H-chromen-8-yl)methyl)piperidin-1-ium-4-carboxylate monohydrate, C22H22N2O9
  59. Synthesis and crystal structure of (3E,5S,10S,13S,14S,17Z)-17-ethylidene-10,13-dimethylhexadecahydro-3H-cyclopenta[α]phenanthren-3-one O-(methacryloyl) oxime, C50H74N2O4
  60. Crystal structure of the hydrogen storage active phase La12Mg46LiMn
  61. The crystal structure of the salt: 4-((1,3-dioxoisoindolin-2-yl)carbamoyl)pyridine-1-ium 2-carboxybenzoate, C14H10N3O3·C8H5O4
  62. Crystal structure of (2-(2-pyridine)-benzimidazole-κ2 N,N′)-bis(1-phenylpyrazole-κ2 C,N)iridium(III) hexafluorophosphate, C30H22F6IrN7P
  63. Crystal structure of dichlorido-bis[2-(2,4-difluorophenyl)pyridine-κ1N]platinum(II), C22H14Cl2F4N2Pt
  64. Crystal structure of (5R,8R,9R,10R,12R,13R,14R, 17S,17Z)-2-((3-fluoropyridin-4-yl)methylene)-12-hydroxy-4,4,8,10,14-pentamethyl-17-((R)-2,6,6-trimethyltetrahydro-2H-pyran-2-yl)hexadecahydro-3H-cyclopenta[a]phenanthren-3-one, C36H52FNO3
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