Home Physical Sciences The crystal structure of hexaaquamagnesium(II) bis-3-(1,2,3,4-tetrahydrobenzo[4,5]imidazo[1,2-α]pyridin-1-yl)benzoate, C36H42N4O10Mg
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The crystal structure of hexaaquamagnesium(II) bis-3-(1,2,3,4-tetrahydrobenzo[4,5]imidazo[1,2-α]pyridin-1-yl)benzoate, C36H42N4O10Mg

  • Zhao Zeng-Bing , Cheng Lan-Xing , Yang Shu-Cheng , Chai Yong-Li EMAIL logo and Tai Xi-Shi ORCID logo EMAIL logo
Published/Copyright: May 27, 2024
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Zeitschrift für Kristallographie - New Crystal Structures
From the journal Zeitschrift für Kristallographie - New Crystal Structures Volume 239 Issue 4

Abstract

C36H42N4O10Mg, monoclinic, C2/c (no. 15), a = 16.4977(12) Å, b = 16.3866(10) Å, c = 12.5814(10) Å, β = 101.922(8)°, V = 3327.9(4) Å3, Z = 4, Rgt (F) = 0.0794, wRref (F 2) = 0.2021, T = 260 K.

CCDC no.: 2354775

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: 0.16 × 0.13 × 0.11 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 0.12 mm−1
Diffractometer, scan mode: SuperNova, ω
θ max, completeness: 25.0°, >99 %
N(hkl)measured, N(hkl)unique, R int: 7457, 2931, 0.027
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 2335
N(param) refined: 258
Programs: Bruker, 1 Olex2, 2 SHELX, 3 Diamond 4
Table 2:

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

Atom x y z U iso*/U eq
C1 0.2728 (2) 0.9015 (2) 0.5441 (3) 0.0350 (7)
C2 0.2566 (3) 0.9455 (3) 0.6322 (3) 0.0449 (9)
H2 0.210328 0.979081 0.624943 0.054*
C3 0.3113 (3) 0.9376 (3) 0.7306 (4) 0.0502 (10)
H3 0.301527 0.966463 0.790323 0.060*
C4 0.3809 (3) 0.8875 (3) 0.7430 (4) 0.0494 (10)
H4 0.416557 0.883711 0.810531 0.059*
C5 0.3979 (3) 0.8432 (3) 0.6563 (3) 0.0457 (9)
H5 0.444160 0.809510 0.663986 0.055*
C6 0.3427 (2) 0.8515 (2) 0.5577 (3) 0.0369 (8)
C7 0.2722 (2) 0.8472 (2) 0.3877 (3) 0.0410 (8)
C8 0.2515 (3) 0.8198 (3) 0.2726 (4) 0.0540 (11)
H8AAa 0.238107 0.865882 0.223618 0.065*
H8ABa 0.205269 0.782083 0.260385 0.065*
H8BCb 0.193428 0.80483 0.254665 0.065*
H8BDb 0.259265 0.865428 0.226465 0.065*
C9Ab 0.2988 (6) 0.7534 (6) 0.2482 (7) 0.0389 (19)
H9AAb 0.289902 0.747255 0.169939 0.047*
H9ABb 0.279626 0.703848 0.277396 0.047*
C9a 0.3386 (7) 0.7738 (6) 0.2558 (8) 0.043 (2)
H9Aa 0.326533 0.744979 0.186955 0.051*
H9Ba 0.378909 0.815782 0.250031 0.051*
C10Ab 0.3870 (5) 0.7631 (5) 0.2921 (8) 0.034 (2)
H10Ab 0.406290 0.813538 0.265576 0.040*
H10Bb 0.417164 0.718264 0.267984 0.040*
C10a 0.3758 (4) 0.7184 (4) 0.3363 (6) 0.0281 (16)
H10Ca 0.335602 0.678997 0.350858 0.034*
H10Da 0.420735 0.689456 0.313894 0.034*
C11 0.4047 (2) 0.7646 (3) 0.4254 (4) 0.0519 (10)
H11a 0.412884 0.723786 0.483538 0.062*
H11Ab 0.406608 0.710125 0.457936 0.062*
C12 0.4885 (2) 0.8068 (2) 0.4454 (3) 0.0331 (7)
C13 0.4925 (3) 0.8892 (2) 0.4187 (4) 0.0520 (10)
H13 0.443578 0.917179 0.391495 0.062*
C14 0.5668 (3) 0.9302 (3) 0.4315 (4) 0.0626 (11)
H14 0.567712 0.985141 0.413202 0.075*
C15 0.6389 (3) 0.8900 (3) 0.4712 (4) 0.0605 (11)
H15 0.689197 0.917529 0.480850 0.073*
C16 0.6371 (3) 0.8087 (3) 0.4968 (3) 0.0461 (9)
H16 0.686749 0.781600 0.523054 0.055*
C17 0.5627 (2) 0.7654 (2) 0.4845 (3) 0.0296 (7)
C18 0.5704 (3) 0.6764 (2) 0.5129 (3) 0.0514 (9)
Mg1 0.500000 0.52137 (10) 0.250000 0.0309 (4)
N1 0.22938 (19) 0.8973 (2) 0.4367 (3) 0.0416 (7)
N2 0.3412 (2) 0.8185 (2) 0.4560 (3) 0.0466 (8)
O1 0.6369 (2) 0.6420 (2) 0.5048 (3) 0.0849 (12)
O2 0.5121 (3) 0.6408 (2) 0.5415 (3) 0.0719 (10)
O3 0.500000 0.6451 (2) 0.250000 0.0355 (8)
H3Ac 0.544952 0.673469 0.289958 0.053*
H3Bc 0.455048 0.673469 0.210042 0.053*
O4 0.61544 (17) 0.52157 (17) 0.3526 (2) 0.0472 (7)
H4A 0.630963 0.557062 0.401866 0.071*
H4B 0.643356 0.479211 0.375514 0.071*
O5 0.500000 0.3966 (2) 0.250000 0.0578 (12)
H5Ac 0.513301 0.368000 0.307278 0.087*
H5Bc 0.514482 0.367960 0.200766 0.087*
O6 0.44228 (16) 0.52030 (16) 0.3832 (2) 0.0383 (6)
H6A 0.447426 0.473110 0.412051 0.058*
H6B 0.468228 0.551762 0.432433 0.058*

  1. aOccupancy: 0.507(10). bOccupancy: 0.493(10). cOccupancy: 0.5.

1 Source of materials

An amount of 0.0585 g 2-(1H-benzo[d]imidazol-2-y)ethanamine dihydrochloride (0.25 mmol), 0.0375 g 2-carboxybenzaldehyde (0.25 mmol), 0.030 g NaOH (0.75 mmol), and 0.0508 g magnesium chloride hexahydrate (0.25 mmol) were dissolved to the 20 ml ethanol-water (v:v = 3:1) solution under stirring. The above solution was heated and stirred for 4 h at 85 °C. The solution was then stirred for an additional 3 h at room temperature. The colorless block crystals were received from the filtrate after 10 days.

2 Experimental details

The hydrogen atoms were positioned geometrically (C–H = 0.93–0.97 Å, O–H = 0.85–0.93 Å). Their U iso values were set to 1.2U eq or 1.5U eq of the parent atoms.

3 Comment

Because the nitrogen and oxygen atoms of some ligands exhibit a variety of coordination modes, 5 , 6 and the complexes also show potential applications in many aspects for example antitumor chemodynamic therapy agent, 7 fluorescent property, 8 dual functional luminescent sensors, 9 and ion sensing and dye adsorption. 10 In our previous work, we have synthesized and structurally characterized some metal complexes with nitrogen heterocarboxylic acid ligands. 11 – 14 To further enrich the structure of metal complexes with nitrogen heterocarboxylic acid ligands. Thus, we synthesized and structurally characterized a Mg(II) complex using 2-(1H-benzo[d]imidazol-2-y)ethanamine dihydrochloride, 2-carboxybenzaldehyde, NaOH, and magnesium chloride hexahydrate as materials. The molecular structure of the title complex is shown in the figure. The title complex is made up of one [Mg(H2O)6]2+ cation and 3-(1,2,3,4-tetrahydrobenzo[4,5]imidazo[1,2-α]pyridin-1-yl)benzoate anion. The asymmetric unit Mg(II) complex contains one half of a Mg2+, one 3-(1,2,3,4-tetrahydrobenzo[4,5]imidazo[1,2-α]pyridin-1-yl)benzoate ligand, and six coordinated H2O molecules. And the Mg2+ is six-coordinated with six O atoms (O3, O4, O41, O5, O6, O61) of six coordinated H2O molecules, which form a distorted MgO6 octahedral coordination geometry (figure). And the bond angle of O3–Mg1–O5 is 180.0°, showing that the O3 and O5 atoms are at the axial positions, and the O4, O41, O6, O61 atoms are at the equatorial plane. The bond lengths of Mg are in the range of 2.027(4)–2.092(2) Å, which are coincident with that reported in reference. 15 The angles around the Mg2+ range from 89.27(11) to 90.73(11)° in the basal plane. Unfortunately, the carboxy oxygen atoms of 3-(1,2,3,4-tetrahydrobenzo[4,5]imidazo[1,2-α]pyridin-1-yl)benzoate ligand do not take part in coordination with Mg2+. The [Mg(H2O)6]2+ cation unit and 3-(1,2,3,4-tetrahydrobenzo[4,5]imidazo[1,2-α]pyridin-1-yl)benzoate anion unit are linked together by O–H⋯O and C–H⋯O hydrogen bonds.

Corresponding authors: Chai Yong-Li, Henan Academy of Sciences, Zhengzhou, 450046, P.R. China; and Henan Chemical Industry Research Institute Co., Zhengzhou, 450052, P.R. China, E-mail: ; and Tai Xi-Shi, College of Chemistry and Chemical Engineering, Weifang University, Weifang, Shandong 261061, P.R. China, E-mail:

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

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

  3. Research funding: talent training support of Henan Academy of Sciences (220608035, 231508001, 242208025) and the National Natural Science Foundation of China (No. 21171132, https://doi.org/10.13039/501100001809).

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Received: 2024-03-18
Accepted: 2024-05-12
Published Online: 2024-05-27
Published in Print: 2024-08-27

© 2024 the author(s), published by De Gruyter, Berlin/Boston

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

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  54. Crystal structure of ((benzyl(hydroxy)-amino)(4-chlorophenyl)methyl)-diphenylphosphine oxide, C26H23ClNO2P
  55. The crystal structure of ethyl 3-(1-methyl-1H-indole-2-carbonyl)-2-phenylquinoline-4-carboxylate, C28H22N2O3
  56. The crystal structure of 1,4-bis(1H-imidazol-3-ium-1-yl)benzene dinitrate, C12H12N4 2+·2(NO3 −)
  57. Crystal structure of tris(hexafluoroacetylacetonato-κ2O,O′) bis(triphenylphosphine oxide-κ1O)samarium(III), C51H33F18O8P2Sm
  58. Crystal structure of 1-(4-(dimethylamino)phenyl)-2,3-bis(diphenylphosphoryl)propan-1-one, C35H33NO3P2
  59. Crystal structure of diaqua[bis(μ 2-pyridine 2,6-dicarboxylato) bismuth(III) potassium(I)], C14H10BiKN2O10
  60. Crystal structure of (R)-N, N ′-dimethyl-[1, 1′-binaphthalene]-2, 2′-diamine, C22H20N2
  61. Crystal structure of 1-phenyl-4-(2-furoyl)-3-furyl-1H-pyrazol-5-ol, C18H12N2O4
  62. Crystal structure of bis(14,34-dimethyl[11,21:23,31-terphenyl]-22-yl)diselane, C40H34Se2
https://doi.org/10.1515/ncrs-2024-0134
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Articles in the same Issue

  1. Frontmatter
  2. New Crystal Structures
  3. The crystal structure of hexaquazinc(II) poly[hexakis(μ2-4-methylbenzenesulfinato-κ2O:O′) dizinc(II)]
  4. The crystal structure of poly[((2-(4,5-dihydro-1H-pyrazol-4-yl)-1,3-dioxoisoindoline-5-carbonyl)oxy)(1-(dimethylamino)ethoxy)zinc[II]], C16H14ZnN4O5
  5. Crystal structure of bis[(triaqua-4-iodopyridine-2,6-dicarboxylato-κ 3 N,O,O ″)cobalt(II)] trihydrate, C14H22N2O17I2Co2
  6. Crystal structure of bis(methanol-κO)-bis(nitrato-kO)-bis(1-((2-(2-chloro-4-(4-chlorophenoxy)phenyl)-4-methyl-1,3-dioxolan-2-yl)methyl)-1H-1,2,4-triazole-κN)cadmium(II), C40H42O14N8Cl4Cd
  7. Crystal structure of poly[μ2-dichlorido-(μ2-1-[(2,4-dimethyl-1H-triazole-1-yl)methyl]-1H-benzotriazole-κ2N:N′)cadmium(II)], C11H12CdN6Cl2
  8. The crystal structure of (3aS, 4R, 7S, 7aR)-hexahydro-4, 7-methano-1H-isoindole-1, 3-(2H)-dione, C9H11NO2
  9. The crystal structure of N-(acridin-9-yl)-4-chloro-N-(4-chloro-butanoyl) butanamide, C21H20Cl2N2O2
  10. Crystal structure of 3,3′-dimethoxy-4,4′-oxy-di-benzaldehyde, C16H14O5
  11. The crystal structure of tetrakis(μ 2-2-amino-3,5-dibromobenzoate-κ 2 O:O′)-octakis(n-butyl-κ 1 C)-bis(μ 3-oxo)tetratin(II), C60H92Br8N4O10Sn4
  12. Crystal structure of methyl-1-(naphthalen-1-yl)-2,3,4,9-tetrahydro-1H-pyrido[3,4-b] indole-3-carboxylate, C23H20N2O2
  13. Crystal structure of tetrapropylammonium bicarbonate–1-(diaminomethylene)thiourea(1/1)
  14. Crystal structure of 6,6′-((1E,1′E)-((2-phenylpyrimidine-4,6-diyl)bis(hydrazin-2-yl-1-ylidene))bis(methaneylylidene))bis(2-methoxyphenol)monohydrate, C26H26N6O5
  15. Crystal structure of bis(N,N,N-trimethylbutanaminium) tetrathiotungstate(VI), (BuMe3N)2[WS4]
  16. The crystal structure of 2,3,9-triphenyl-9-(2-phenylbenzofuran-3-yl)-9H-9λ 5-benzo[4,5][1,2]oxaphospholo[2,3-b][1,2,5]oxadiphosphole 2-oxide, C40H28O4P2
  17. Crystal structure of 1–methyl-3-propyl-4-nitro-1H-pyrazole-5-carboxylic acid, C8H11N3O4
  18. Crystal structure of N-(benzo[d]thiazol-2-yl)-2-chloroacetamide, C9H7ClN2OS
  19. The crystal structure of N-benzyl-2-chloro-N-(p-tolyl) acetamide, C16H16ClNO
  20. Crystal structure of 3,4-dimethoxybenzyl 2-(6-methoxynaphthalen-2-yl)propanoate, C23H24O5
  21. Crystal structure of 2,5-bis(2,5-dimethoxybenzyl)-3,6-dimethyl-2,5-dihydropyrrolo[3,4-c]pyrrole-1,4-dione, C26H28N2O6
  22. Crystal structure of poly[(μ3-5-bromoisophthalato-κ4 O,O′ :O″,O‴)-(μ2-1,2-bis(1,2,4-triazole-1-ylmethyl)benzene-κ2 N:N′)cobalt(II)], C20H15BrCoN6O4
  23. The crystal structure of bis(2-(piperidin-1-ium-4-yl)-1Hbenzo[d]imidazol-3-ium) dihydrogen decavanadate, C24H36N6O28V10
  24. Crystal structure of diaqua-bis(1-(3-carboxyphenyl)-5-methyl-4-oxo-1,4-dihydropyridazine3-carboxylato-O,O′)-cobalt(ii)dihydrate, C26H36N4O14Co
  25. Crystal structure of poly[(μ2-5-bromoisophthalato-κ4 O,O ′:O ″,O ‴)-(μ2-1,4-bis(2-methylimidazol-1-ylmethyl)benzene-N:N′)cadmium(II)], C24H21BrCdN4O4
  26. The crystal structure of dimethyl 8-(3-methoxy-2-(methoxycarbonyl)-3-oxoprop-1-en-1-yl)-4-methyl-1-(p-tolyl)-1,3a,4,8b-tetrahydro-3H-furo[3,4-b]indole-3,3-dicarboxylate. C28H29NO9
  27. Crystal structure of (3R)-1-(3,5-dimethoxyphenyl)-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole-3-carboxylate chloride, C21H23ClN2O4
  28. Synthesis and crystal structure of 3-(4,5-dihydroisoxazol-3-yl)-2-methyl-4-(methylsulfonyl)benzoic acid, C12H13NO5S
  29. The crystal structure of hexaaquamagnesium(II) bis-3-(1,2,3,4-tetrahydrobenzo[4,5]imidazo[1,2-α]pyridin-1-yl)benzoate, C36H42N4O10Mg
  30. Crystal structure of 4-formyl-2-methoxyphenyl 2-acetoxybenzoate, C17H14O6
  31. Crystal structure of poly[octakis(μ-oxido)-tris(μ-1,1′-[[1,1′-biphenyl]-4,4′-diylbis(methylene)]bis(1H-imidazole))-tetrakis(oxido)-tetra-vanadium-dimanganese(II)dihydrate], C30H29MnN6O7V2
  32. Crystal structure of 4,8a-bis(4-chlorophenyl)-1,5,6-tris(4-fluorobenzyl)-1,4,4a,4b,5,6,8a,8b-octahydrocyclobuta[1,2-b:3,4-c′]dipyridine-3,8-dicarbonitrile, C45H33Cl2F3N4
  33. Crystal structure of benzo[d][1,3]dioxol-5-ylmethyl 2-(6-methoxynaphthalen-2-yl)propanoate, C22H20O5
  34. Crystal structure of N-benzoyl-N-phenylhydroxylaminato-dicarbonylrhodium(I), [Rh(BNA)CO2]
  35. The crystal structure of N-(2-((2-methoxynaphthalen-1-yl)ethynyl)phenyl)-4-methylbenzenesulfonamide, C26H21NO3S
  36. The crystal structure of methyl ((4-aminobenzyl)sulfonyl)-d-prolinate, C13H18N2O4S
  37. The crystal structure of dichlorido-(N-isopropyl-N-(pyridin-2-ylmethyl)propan-2-amine-κ 2 N, N′)palladium(II), C12H20N2PdCl2
  38. Crystal structure of poly[(μ 2-5-hydroxyisophthalato-κ4 O,O′:O″,O‴)-(μ 2-1,4-bis(2-methylimidazolyl)-1-butene-N:N′)nickel(II)], C20H20NiN4O5
  39. The crystal structure of {hexakis(1-methyl-1H-imidazole-κ 1 N)cobalt(II)}(μ 2-oxido)-hexaoxido-dimolybdenum(VI)— 1-methyl-1H-imidazole (1/2), C32H48CoMo2N16O7
  40. Synthesis, crystal structure and nonlinear optical property of 1-((propan-2-ylideneamino)oxy)propan-2-yl-4-methylbenzenesulfonate, C13H19O4NS
  41. The crystal structure of N,N-(ethane-1,1-diyl)dibenzamide, C16H16N2O2
  42. Crystal structure of 1-(4-bromophenyl)-3-(diphenylphosphoryl)-3-hydroxypropan-1-one, C21H18BrO3P
  43. The crystal structure of fac-tricarbonyl(bis(3,5-dimethyl-4H-pyrazole)-κ1 N)-((nitrato)-κ1 O)-rhenium(I)— 3,5-dimethyl-4H-pyrazole(1/1), C18H23N7O6Re
  44. The crystal structure of 4′-chloro-griseofulvin: (2S,6′R)-4′,7-dichloro-4,6-dimethoxy-6′-methyl-3H-spiro[benzofuran-2,1′-cyclohexan]-3′-ene-2′,3-dione, C16H14Cl2O5
  45. Crystal structure of tetraethylammonium bicarbonate–1-(diaminomethylene)thiourea(1/1)
  46. Crystal structure of 1-cyclohexyl-4-p-tolyl-1,4-dihydropyridine-3,5-dicarboxylic acid dimethyl ester, C22H27NO4
  47. The crystal structure of catena-poly(μ2-1,4-bis-(1H-imidazol-1-yl)benzene-copper(I)) dichloridocopper(I), {[CuC12H10N4]+[CuCl2]−} n
  48. The crystal structure of propane-1-aminium-2-carbamate, C4H10N2O2
  49. Crystal structure of 5,6,3′,4′,5′-pentamethoxy-flavone dihydrate, C20H24O9
  50. Crystal structure of (E)-N-(2-bromophenyl)-4-(4-(3,5-dimethoxystyryl)phenoxy)pyrimidin-2-amine, C26H22BrN3O3
  51. Crystal structure of methyl (3R)-1-(2-bromo-4-fluorophenyl)-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole-3-carboxylate hydrochloride hydrate, C19H19BrClFN2O3
  52. The crystal structure of 1-(2-chlorophenyl)-3-(p-tolyl)urea, C14H13ClN2O
  53. The crystal structure of 1-cyclohexyl-3-(p-tolyl)urea, C14H20N2O
  54. Crystal structure of ((benzyl(hydroxy)-amino)(4-chlorophenyl)methyl)-diphenylphosphine oxide, C26H23ClNO2P
  55. The crystal structure of ethyl 3-(1-methyl-1H-indole-2-carbonyl)-2-phenylquinoline-4-carboxylate, C28H22N2O3
  56. The crystal structure of 1,4-bis(1H-imidazol-3-ium-1-yl)benzene dinitrate, C12H12N4 2+·2(NO3 −)
  57. Crystal structure of tris(hexafluoroacetylacetonato-κ2O,O′) bis(triphenylphosphine oxide-κ1O)samarium(III), C51H33F18O8P2Sm
  58. Crystal structure of 1-(4-(dimethylamino)phenyl)-2,3-bis(diphenylphosphoryl)propan-1-one, C35H33NO3P2
  59. Crystal structure of diaqua[bis(μ 2-pyridine 2,6-dicarboxylato) bismuth(III) potassium(I)], C14H10BiKN2O10
  60. Crystal structure of (R)-N, N ′-dimethyl-[1, 1′-binaphthalene]-2, 2′-diamine, C22H20N2
  61. Crystal structure of 1-phenyl-4-(2-furoyl)-3-furyl-1H-pyrazol-5-ol, C18H12N2O4
  62. Crystal structure of bis(14,34-dimethyl[11,21:23,31-terphenyl]-22-yl)diselane, C40H34Se2
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