Startseite Crystal structure of catena-poly[(5,5′-dimethyl-2,2′-bipyridine-κ 2 N,N′)-(μ 3-hydrogen-1,1′,1″-(1,3,5-triazine-2,4,6-triyl)tris(piperidine-4-carboxylato)- κ 5 O:O,O′:O″,O‴)-cadmium(II)], C33H40CdN8O6
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Crystal structure of catena-poly[(5,5′-dimethyl-2,2′-bipyridine-κ 2 N,N′)-(μ 3-hydrogen-1,1′,1″-(1,3,5-triazine-2,4,6-triyl)tris(piperidine-4-carboxylato)- κ 5 O:O,O′:O″,O‴)-cadmium(II)], C33H40CdN8O6

  • Hua-Xiang Zhang ORCID logo EMAIL logo
Veröffentlicht/Copyright: 5. September 2022

Abstract

C33H40CdN8O6, triclinic, P 1 (no. 2), a = 10.6468(11) Å, b = 11.6739(9) Å, c = 14.5312(9) Å, α = 93.976(5)°, β = 102.005(7)°, γ = 111.827(8)°, V = 1618.4(2) Å3, Z = 2, R gt(F) = 0.0480, wR ref(F 2) = 0.1102, T = 293(2) K.

CCDC no.: 2166150

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 × 0.10 × 0.10 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 0.73 mm−1
Diffractometer, scan mode: Bruker D8 Advance, φ and ω
θ max, completeness: 25.0°, >99%
N(hkl)measured, N(hkl)unique, R int: 10151, 5699, 0.046
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 4293
N(param)refined: 449
Programs: Bruker [1], Olex2 [2], SHELX [3, 4]
Table 2:

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

Atom x y z U iso*/U eq
Cd1 0.64004 (3) 0.49225 (3) 0.44780 (2) 0.03877 (13)
O1a −0.5068 (12) 0.4547 (9) −0.1090 (6) 0.089 (3)
O2 −0.3998 (5) 0.4152 (4) −0.2100 (3) 0.0797 (14)
O3 −0.6320 (4) −0.3048 (3) 0.4685 (3) 0.0791 (12)
O4 −0.4601 (4) −0.3669 (3) 0.4867 (2) 0.0476 (9)
O5 0.5792 (4) 0.3139 (3) 0.3246 (3) 0.0738 (11)
O6 0.4547 (4) 0.4251 (3) 0.3060 (2) 0.0484 (8)
N1 0.8190 (4) 0.6012 (3) 0.3773 (3) 0.0383 (9)
N2 0.8491 (4) 0.5829 (3) 0.5641 (3) 0.0382 (9)
N3 0.0576 (4) 0.0522 (3) 0.1551 (2) 0.0396 (9)
N4 −0.1285 (4) 0.1031 (3) 0.0958 (2) 0.0367 (9)
N5 −0.3050 (4) 0.0740 (3) 0.1817 (3) 0.0397 (9)
N6 −0.1071 (4) 0.0244 (3) 0.2428 (3) 0.0391 (9)
N7 −0.2763 (4) 0.0005 (4) 0.3245 (3) 0.0498 (11)
N8 −0.3137 (4) 0.1587 (3) 0.0422 (3) 0.0452 (10)
C1 −0.4422 (6) 0.3979 (5) −0.1335 (4) 0.0543 (14)
C2 −0.4270 (5) 0.2884 (4) −0.0901 (3) 0.0445 (12)
H2A −0.500564 0.212431 −0.130104 0.053*
C3 −0.2878 (5) 0.2790 (4) −0.0893 (3) 0.0465 (12)
H3A −0.275475 0.275950 −0.153577 0.056*
H3B −0.211998 0.352537 −0.049915 0.056*
C4 −0.2828 (6) 0.1644 (5) −0.0514 (3) 0.0518 (13)
H4A −0.350216 0.090770 −0.095707 0.062*
H4B −0.190628 0.164143 −0.046250 0.062*
C5 −0.4427 (6) 0.1717 (5) 0.0479 (4) 0.0521 (14)
H5A −0.448220 0.177364 0.113783 0.063*
H5B −0.522120 0.098430 0.011402 0.063*
C6 −0.4488 (6) 0.2871 (5) 0.0097 (4) 0.0571 (15)
H6A −0.377239 0.360903 0.051711 0.068*
H6B −0.539012 0.289763 0.008864 0.068*
C7 −0.2472 (5) 0.1091 (4) 0.1086 (3) 0.0356 (11)
C8 −0.2270 (5) 0.0344 (4) 0.2470 (3) 0.0380 (11)
C9 −0.4044 (5) 0.0072 (4) 0.3407 (3) 0.0453 (12)
H9A −0.453706 0.028008 0.284689 0.054*
H9B −0.381430 0.072203 0.394128 0.054*
C10 −0.4980 (5) −0.1186 (4) 0.3615 (3) 0.0400 (11)
H10A −0.578307 −0.111009 0.378497 0.048*
H10B −0.532048 −0.180763 0.304413 0.048*
C11 −0.4196 (5) −0.1624 (4) 0.4425 (3) 0.0371 (11)
H11 −0.394831 −0.100645 0.499555 0.045*
C12 −0.5114 (5) −0.2884 (4) 0.4653 (3) 0.0431 (12)
C13 −0.2844 (5) −0.1590 (4) 0.4257 (3) 0.0479 (13)
H13A −0.304093 −0.224299 0.373268 0.057*
H13B −0.232046 −0.176360 0.482115 0.057*
C14 −0.1958 (5) −0.0349 (5) 0.4031 (3) 0.0513 (13)
H14A −0.162918 0.028831 0.459002 0.062*
H14B −0.114781 −0.040634 0.385846 0.062*
C15 −0.0628 (5) 0.0607 (3) 0.1654 (3) 0.0346 (11)
C16 0.1336 (5) 0.1210 (4) 0.0902 (3) 0.0433 (12)
H16A 0.070481 0.141107 0.042088 0.052*
H16B 0.170054 0.069292 0.058285 0.052*
C17 0.2538 (5) 0.2411 (4) 0.1447 (3) 0.0408 (11)
H17A 0.305529 0.284166 0.101142 0.049*
H17B 0.216796 0.295672 0.172444 0.049*
C18 0.3514 (5) 0.2122 (4) 0.2233 (3) 0.0394 (11)
H18 0.391479 0.160894 0.193482 0.047*
C19 0.2680 (5) 0.1366 (4) 0.2881 (3) 0.0402 (11)
H19A 0.328897 0.112295 0.334667 0.048*
H19B 0.233947 0.188519 0.322241 0.048*
C20 0.1453 (5) 0.0208 (4) 0.2320 (3) 0.0428 (12)
H20A 0.179660 −0.036786 0.205260 0.051*
H20B 0.089899 −0.020562 0.274335 0.051*
C21 0.4707 (5) 0.3263 (5) 0.2854 (3) 0.0427 (12)
C22 0.7981 (5) 0.6121 (4) 0.2853 (3) 0.0454 (12)
H22 0.706795 0.576738 0.247542 0.055*
C23 0.9046 (6) 0.6730 (4) 0.2417 (4) 0.0505 (13)
C24 1.0380 (6) 0.7162 (4) 0.2993 (4) 0.0523 (14)
H24 1.113099 0.754193 0.273224 0.063*
C25 1.0640 (5) 0.7051 (4) 0.3940 (4) 0.0488 (13)
H25 1.155146 0.735037 0.431710 0.059*
C26 0.9504 (5) 0.6478 (4) 0.4327 (3) 0.0368 (11)
C27 0.9676 (5) 0.6339 (4) 0.5344 (3) 0.0377 (11)
C28 1.0966 (5) 0.6671 (4) 0.5977 (4) 0.0456 (12)
H28 1.177928 0.701554 0.577237 0.055*
C29 1.1047 (5) 0.6492 (4) 0.6910 (4) 0.0486 (13)
H29 1.191658 0.670596 0.733090 0.058*
C30 0.9837 (5) 0.5993 (4) 0.7228 (3) 0.0436 (12)
C31 0.8587 (5) 0.5676 (4) 0.6547 (4) 0.0464 (12)
H31 0.776055 0.533387 0.673696 0.056*
C32 0.9851 (6) 0.5761 (5) 0.8236 (3) 0.0570 (14)
H32A 0.899858 0.508176 0.824102 0.085*
H32B 0.993239 0.650120 0.861918 0.085*
H32C 1.063218 0.555311 0.849041 0.085*
C33 0.8719 (7) 0.6877 (5) 0.1391 (4) 0.0772 (19)
H33A 0.875462 0.770473 0.134698 0.116*
H33B 0.779943 0.627442 0.107205 0.116*
H33C 0.939190 0.674579 0.109607 0.116*
H2 −0.408 (12) 0.477 (6) −0.233 (7) 0.22 (5)*
O1Ab −0.393 (6) 0.500 (3) −0.073 (2) 0.096 (10)
  1. aOccupancy: 0.815 (18), bOccupancy: 0.185 (18).

Source of material

The raw materials were purchased from Shanghai Aladdin Biochemical Technology Co., Ltd. For the reaction Cd(NO3)2 ⋅ 4H2O (0.0308 g, 0.1 mmol), 1,1′,1″-(1,3,5-triazine-2,4,6-triyl)tris(piperidine-4-carboxylic acid) (H3L, 0.0139 g, 0.03 mmol), 5,5′-dimethyl-2,2′-bipyridine (DMBPY, 0.0092 g, 0.05 mmol), DMF (8 mL) and two drops of concentrated hydrochloric acid were mixed in a 20 mL capped vial and transferred to an 100 °C oven for 72 h, After the system cooled to room temperature, clear light colourless block crystals were obtained, yielding 37%, based on the metal-salt.

Experimental details

The following steps are operated via the OLEX2 software. The initial structure of the complex was solved by SHELXT. Refinement process was performed by SHELXL program. The hydrogen atoms were placed in their idealized positions with isotropic thermal parameters. Note that the oxygen atom belonging to C=O of the undeprotonated carboxylic group is disordered.

Comment

As a tridentate carboxylic acid cotaining triazine centre, 1,1′,1″-(1,3,5-triazine-2,4,6-triyl)tris(piperidine-4-carboxylic acid) (H3L) has been used to build complexes with metal salts [5], [6], [7], [8], [9]. However, almost all of the reported structures are based on only the H3L ligand which greatly limited the quantity of the H3L-complexes. Mixed-ligand strategy has been proved to be a effective way for preparation of valuable functional complexes with diversiform structures [10], [11], [12]. With this in mind, we introduced 5,5′-dimethyl-2,2′-bipyridine (DMBPY) as an auxiliary ligand, combined with cadmium salt to build metal complexes. As a result, the title complex was synthesized through one-pot synthesis method.

The complex crystallizes in the triclinic system within the space group P 1 . The asymmetric unit contains one partial deprotonated H3L ligand (two of the three carboxylic groups are deprotonated), one DMBPY ligand and one Cd(II) ion. The Cd(II) ion is seven-coordinated with five oxygen atoms (O31, O41, O42, O5, O6) derived from three different H3L ligands and two DMBPY nitrogen atoms (N1, N2). The distances of Cd–N and Cd–O bonds are within the range of 2.316(4)–2.559(4) Å, parallel to the reported Cd(II)-based complexes with similar environment [13], [14], [15]. Two Cd(II) ions, two H3L and two DMBPY ligands formed a Cd2(H3L)2(DMBPY)2 binuclear unit. These units are bridged by carboxylic oxygen atoms with the Cd(II) ions to generate a infinite one-dimensional (1D) structure. As a result, the 1D structures are further expended by hydrogen bonding (O2–H2—O63) and π-π stacking interactions between the ligand rings, centroid-centroid distance: 3.748(3) Å, to form a three-dimensional (3D) supramolecular network (symmetry code: #1: −x, −y, 1 − z; #2: 1 + x, 1 + y, z; #3: −x, 1 − y, −z).


Corresponding author: Hua-Xiang Zhang, College of Chemistry and Chemical Engineering, Weifang University, Weifang, Shandong 261061, P. R. China, E-mail:

Funding source: College of Chemistry and Chemical Engineering, Weifang University

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

  2. Research funding: This work was supported by College of Chemistry and Chemical Engineering, Weifang University.

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

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Received: 2022-07-10
Accepted: 2022-08-26
Published Online: 2022-09-05
Published in Print: 2022-12-16

© 2022 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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  40. The crystal structure of N′-[bis(2-hydroxyphenyl)methylidene]pyridine-4-carbohydrazide, C19H15N3O3
  41. Crystal structure of 2-chloro-6-formylphenolato-κ2O,O′-(6,6′-(((2,2-dimethylpropane-1,3-diyl)bis(azaneylylidene))bis(methaneylylidene))bis(2-chlorophenolato)κ4 N,N,O,O′)cobalt(III), C26H22Cl3CoN2O4
  42. The crystal structure of tetrakis(6-phenylpyridine-2-carboxylate-κ 2 N,O)-bis(μ2-6-phenylpyridine-2-carboxylate-κ 2 O:O′)-bis(μ2-6-phenylpyridine-2-carboxylate-κ 3N,O:O)tetralead(II) C48H32N4O8Pb2
  43. The crystal structure of 3,7-dihydroxy-9-methoxy-4a-methyl-4aH-benzo[c] chromene-2,6-dione —dichloromethane (1/1), C16H14Cl2O6
  44. The crystal structure of (Z)-6-(((5-chloro-2-hydroxyphenyl)amino)methylene)- 4-nitrocyclohexa, C13H9ClN2O4
  45. Crystal structure of dichlorido-tetra((E)-(RS)-1-(2,4-dichlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)pent-1-en-3-ol-κ1 N)zinc(II), C60H68O4N12Cl10Zn
  46. The crystal structure of 4-(2-bromoethoxy)-2-hydroxybenzaldehyde, C9H9BrO3
  47. The crystal structure of 5-azido-1-methyl-4-nitroimidazole, C4H4O2N6
  48. Crystal structure of dibromido-tetra((E)-(RS)-1-(2,4-dichlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)pent-1-en-3-ol-κ 1 N)zinc(II), C60H68O4N12Br2Cl8Zn
  49. Crystal structure of tetrasodium-bis(μ 2-oxido)-hexafluoro-didioxo-molybdenum(V), Na2(Mo2O4F6)
  50. Crystal structure of (E)-N′-(2-chloro-6-hydroxybenzylidene)-4- hydroxybenzohydrazide-water (1/1), C14H13Cl1N2O4
  51. Crystal structure of (E)-N-(4-morpholinophenyl)-1-(quinolin-2-yl)methanimine, C20H19N3O
  52. The crystal structure of catena-poly[(1,10-phenanthroline-κ2 N,N′)-(μ3-2-hydroxybenzene-1,3-dicarboxylato-κ5 O,O′:O″,O‴:O‴)cadmium(II)], C20H12CdN2O5
  53. The crystal structure of 2,6-di-tert-butyl-4-(4-(methylthio)benzylidene)cyclohexa-2,5-dien-1-one, C22H28OS
  54. La3.65Mg30Sb1.07 as a disordered derivative of Th2Ni17-type structure
  55. Crystal structure of (E)-N-(4-morpholinophenyl)-1-(quinoxalin-2-yl)methanimine, C19H18N4O
  56. The crystal structure of 2,2′-(1,2-phenylenebis(methylene))bis(1,3-dimethylisothiouronium) bromide, C14H24Br2N4S2
  57. Crystal structure of tetraaqua-bis[4-(1H-1,2,4-triazol-1-yl)benzoato-κ1 N]zinc(II), C18H20ZnN6O8
  58. Crystal structure of bis(tricarbonyl)-{(S)-(tert-butoxycarbonyl)(1-methoxy-1-oxo-3-sulfido-k2 S:S′-propan-2-yl)amido-k2N:N′}diiron(I) (Fe—Fe), C15H15Fe2NO10S
  59. Crystal structure of (E)-3-((4-chlorophenyl)thio)-4-hydroxypent-3-en-2-one, C11H11ClO2S
  60. The crystal structure of (E)-3′,6′-bis(diethylamino)-2-((5-(diethylamino)-2-hydroxybenzylidene)amino)spiro[isoindoline-1,9′-xanthen]-3-one, C39H45N5O3
  61. The crystal structure of 2-(4-methoxynaphthalen-1-yl)-4H-chromen-4-one, C20H14O3
  62. The crystal structure of trans-dichlorido-(ethylenediamine-κ 2 N,N′)-bis(triphenylphosphine-κ 1 P)ruthenium(II), C38H38Cl2N2P2Ru
  63. The double polymeric chain of catena-poly[(μ2-6-bromopyridine-3-carboxylato-κ2 O,O′) (6-bromopyridine-3-carboxylato-κ2 O,O′) (μ2-1,2-bis(4-pyridyl)ethylene-κ2 N:N′)cobalt(II)], C24H16CoBr2N4O4
  64. The crystal structure of tert-butyl 2-(4-(12-bromo [2.2]paracyclophanyl)carbamoyl)pyrrolidine-1-carboxylate, C26H31BrN2O3
  65. The crystal structure of (Z)-2-(2,3-dimethoxybenzylidene)naphtho[1,2-b]furan-3(2H)-one, C21H16O4
  66. Crystal structure of 2-hydroxy-1-tosylindolin-3-yl- 2-naphthoate, C26H21N1S1O5
  67. The crystal structure of 1-methyl-N-(1-methyl-1H-imidazole-2-carbonyl)-1H-imidazole-2-carboxamide, C10H11N5O2
  68. The crystal structure of (E)-2-((5-bromo-2-hydroxybenzylidene)amino)-3′,6′-bis(ethylamino)-2′, 7′-dimethylspiro[isoindoline-1,9′-xanthen]-3-one, C33H31BrN4O3
  69. The crystal structure of dimethanol-5,15-diphenylporphyrin-21,23-diido-κ4 N,Nʹ,Nʺ,Nʹʺ-manganese(III) trans-dicyanido-bis(acetylacetonato-κ2O,Oʹ)ruthenium(III), C46H42N6O6RuMn
  70. Crystal structure of 1,4,8,11-tetraazacyclotetradecane-1,8-diium bis(3,5-dicarboxybenzoate), C28H36N4O12
  71. Bifurcated halogen bonds in the crystal structure of 2,2′-bi(1,8-naphthyridine)—1,4-diiodotetrafluorobenzene (1/1), C22H10F4I2N4
Heruntergeladen am 7.9.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2022-0351/html
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