Abstract
C30H29MnN6 O7V2, triclinic, P
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.

Data collection and handling.
| Crystal: | Red block |
| Size: | 0.22 × 0.21 × 0.20 mm |
| Wavelength: μ: |
Mo Kα radiation (0.71073 Å) 1.03 mm−1 |
| Diffractometer, scan mode: θ max, completeness: |
Bruker APEX-II, φ and ω
29.6°, 99 % |
| N(hkl)measured, N(hkl)unique, R int: | 20461, 8754, 0.040 |
| Criterion for I obs, N(hkl)gt: | I obs > 2 σ(I obs), 7493 |
| N(param)refined: | 418 |
| Programs: | Bruker, 1 Olex2, 2 SHELX 3 , 4 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).
| Atom | x | y | z | U iso*/U eq |
|---|---|---|---|---|
| Mn1 | 0.08351 (2) | 0.43771 (2) | 0.07793 (2) | 0.00901 (6) |
| V1 | 0.41899 (3) | 0.31707 (2) | 0.04087 (2) | 0.01094 (6) |
| V2 | 0.73956 (3) | 0.54233 (2) | 0.10127 (2) | 0.00932 (6) |
| O1 | 0.29237 (13) | 0.36147 (11) | 0.09690 (8) | 0.0154 (2) |
| O2 | 0.41738 (14) | 0.16744 (11) | 0.02952 (9) | 0.0213 (3) |
| O3 | 0.60607 (13) | 0.40293 (11) | 0.08941 (9) | 0.0204 (3) |
| O4 | 0.81290 (14) | 0.59937 (12) | 0.20145 (8) | 0.0208 (3) |
| O5 | 0.64009 (13) | 0.65512 (11) | 0.06354 (8) | 0.0177 (2) |
| O6 | 0.87633 (12) | 0.51279 (10) | 0.04525 (7) | 0.0110 (2) |
| N1 | 0.21646 (15) | 0.61824 (12) | 0.15768 (8) | 0.0121 (2) |
| N2 | 0.41141 (15) | 0.77252 (12) | 0.21469 (8) | 0.0116 (2) |
| N3 | 0.92245 (15) | 1.05943 (12) | 0.91941 (8) | 0.0129 (3) |
| N4 | 0.96379 (15) | 1.25359 (12) | 0.99559 (8) | 0.0116 (2) |
| N5 | 0.02485 (15) | 0.39073 (13) | 0.19559 (9) | 0.0140 (3) |
| N6 | −0.08807 (16) | 0.31673 (13) | 0.28808 (9) | 0.0159 (3) |
| C1 | 0.36340 (17) | 0.65715 (14) | 0.16324 (10) | 0.0128 (3) |
| H1 | 0.426803 | 0.609820 | 0.134634 | 0.015* |
| C2 | 0.28751 (18) | 0.80997 (15) | 0.24399 (11) | 0.0156 (3) |
| H2 | 0.285649 | 0.887051 | 0.281380 | 0.019* |
| C3 | 0.16845 (18) | 0.71454 (15) | 0.20868 (10) | 0.0151 (3) |
| H3 | 0.067798 | 0.714018 | 0.217628 | 0.018* |
| C4 | 0.56659 (18) | 0.84452 (15) | 0.23587 (10) | 0.0151 (3) |
| H4A | 0.564222 | 0.926067 | 0.221738 | 0.018* |
| H4B | 0.630226 | 0.799788 | 0.201123 | 0.018* |
| C5 | 0.63577 (17) | 0.86426 (15) | 0.32979 (10) | 0.0144 (3) |
| C6 | 0.6971 (2) | 0.76987 (18) | 0.35942 (12) | 0.0256 (4) |
| H6 | 0.700655 | 0.695135 | 0.319997 | 0.031* |
| C7 | 0.7531 (2) | 0.78448 (19) | 0.44643 (12) | 0.0288 (4) |
| H7 | 0.792763 | 0.718825 | 0.465979 | 0.035* |
| C8 | 0.7518 (2) | 0.89435 (16) | 0.50530 (11) | 0.0188 (3) |
| C9 | 0.6942 (2) | 0.98926 (17) | 0.47547 (11) | 0.0227 (4) |
| H9 | 0.694665 | 1.065377 | 0.514610 | 0.027* |
| C10 | 0.6353 (2) | 0.97389 (16) | 0.38825 (11) | 0.0211 (3) |
| H10 | 0.594572 | 1.039185 | 0.368801 | 0.025* |
| C11 | 0.8066 (2) | 0.90785 (16) | 0.59862 (11) | 0.0191 (3) |
| C12 | 0.7295 (2) | 0.83149 (18) | 0.64066 (12) | 0.0264 (4) |
| H12 | 0.643439 | 0.770985 | 0.609327 | 0.032* |
| C13 | 0.7776 (2) | 0.84310 (17) | 0.72790 (12) | 0.0244 (4) |
| H13 | 0.723396 | 0.791203 | 0.755812 | 0.029* |
| C14 | 0.9040 (2) | 0.92978 (15) | 0.77443 (10) | 0.0173 (3) |
| C15 | 0.98291 (19) | 1.00514 (17) | 0.73286 (11) | 0.0197 (3) |
| H15 | 1.070567 | 1.063956 | 0.764207 | 0.024* |
| C16 | 0.9342 (2) | 0.99486 (17) | 0.64556 (11) | 0.0202 (3) |
| H16 | 0.988128 | 1.047322 | 0.617883 | 0.024* |
| C17 | 0.9525 (2) | 0.94305 (15) | 0.86946 (11) | 0.0193 (3) |
| H17A | 0.897255 | 0.871849 | 0.885326 | 0.023* |
| H17B | 1.062586 | 0.941062 | 0.883761 | 0.023* |
| C18 | 1.02595 (18) | 1.16323 (14) | 0.95613 (10) | 0.0135 (3) |
| H18 | 1.130644 | 1.170999 | 0.954099 | 0.016* |
| C19 | 0.81080 (18) | 1.20369 (15) | 0.98190 (10) | 0.0134 (3) |
| H19 | 0.735864 | 1.246565 | 1.002139 | 0.016* |
| C20 | 0.78400 (18) | 1.08347 (15) | 0.93489 (10) | 0.0150 (3) |
| H20 | 0.689258 | 1.027969 | 0.916670 | 0.018* |
| C21 | −0.08954 (18) | 0.31159 (15) | 0.20501 (11) | 0.0144 (3) |
| H21 | −0.163420 | 0.257891 | 0.158880 | 0.017* |
| C22 | 0.1027 (2) | 0.44954 (17) | 0.27777 (11) | 0.0197 (3) |
| H22 | 0.190973 | 0.512198 | 0.291844 | 0.024* |
| C23 | 0.0348 (2) | 0.40481 (17) | 0.33563 (11) | 0.0210 (3) |
| H23 | 0.065715 | 0.429224 | 0.396212 | 0.025* |
| C24 | −0.1961 (2) | 0.24075 (16) | 0.32138 (12) | 0.0208 (4) |
| H24A | −0.140246 | 0.193135 | 0.356930 | 0.025* |
| H24B | −0.267847 | 0.180564 | 0.272993 | 0.025* |
| C25 | −0.2845 (2) | 0.31965 (16) | 0.37462 (12) | 0.0188 (3) |
| C26 | −0.2784 (2) | 0.31846 (18) | 0.45943 (12) | 0.0251 (4) |
| H26 | −0.215352 | 0.269417 | 0.485018 | 0.030* |
| C27 | −0.3631 (2) | 0.38800 (18) | 0.50815 (12) | 0.0255 (4) |
| H27 | −0.358404 | 0.383916 | 0.565953 | 0.031* |
| C28 | −0.45434 (19) | 0.46311 (15) | 0.47394 (12) | 0.0184 (3) |
| C29 | −0.4576 (3) | 0.4645 (3) | 0.38850 (16) | 0.0439 (7) |
| H29 | −0.518269 | 0.515261 | 0.363173 | 0.053* |
| C30 | −0.3754 (3) | 0.3942 (2) | 0.33934 (15) | 0.0415 (6) |
| H30 | −0.381254 | 0.397052 | 0.281242 | 0.050* |
| O1W | 0.63013 (15) | 1.04705 (12) | 0.11624 (8) | 0.0230 (3) |
| H1WA | 0.570121 | 1.090666 | 0.093043 | 0.034* |
| H1WB | 0.617167 | 0.977710 | 0.077574 | 0.034* |
1 Source of materials
A mixture comprising NaVO3 (0.5 mmol, 61.0 mg) and N2H4·H2O (0.1 mmol, 6.2 μL) in H2O (9.5 mL) was stirred for a duration of 30 min at ambient temperature. The mixture was stirred for an additional hour after being enriched with a solution containing 4,4′-bis(imidazol-1-ylmethyl)biphenyl (bibp; 0.15 mmol, 47.1 mg) in DMF (0.5 mL) and Mn(OAc)2·4H2O (0.1 mmol, 24.5 mg). The pH of this mixture was then adjusted by adding HCl (aq 1.0 M) to 3.42, and the resulting mixture was poured into a 23 mL Teflon-lined autoclave reactor and kept at 393 K for 3 days. The product was obtained as a green crystalline solid after the autoclave was cooled to room temperature.
2 Experimental details
The structure was solved by Direct Methods with the SHELXS-2018 program. All the non–H atoms were refined anisotropically. All H-atoms from C atoms were positioned with idealized geometry and refined isotropic (U iso(H) = 1.2U eq(C)) and (U iso(H) = 1.5U eq(C)) using a riding model with C–H = 0.950 Å (imidazole and phenyl groups) and C–H = 0.990 Å (methylene), respectively. The water H-atom positions were fixed with O–H = 0.870 Å (U iso(H) = 1.5U eq(O)).
3 Comment
Vanadium-based functional complexes have attracted widespread research interest due to their rich topological structural types.
5
–
16
The bibp is a linear bridging ligand containing rigid biphenyls and flexible alkyl groups, and if applied to the synthesis of polyvanadates-based coordination complexes, it may yield very interesting crystal structures. However, to our knowledge, only two polyvanadate based compounds containing bibp ligands have been reported up to now.
9
Here, we prepared a new polyvanadate manganese complex based on bibp ligand using a simple one pot method. Single-crystal X-ray diffraction study shows the title compound crystallizes in the space group P
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Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.
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Research funding: Talent Scientific Research Fund of Liaoning Petrochemical University (2016XJJL-019).
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Competing interests: The authors declare no conflicts of interest regarding this article.
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© 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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- The crystal structure of 1-cyclohexyl-3-(p-tolyl)urea, C14H20N2O
- Crystal structure of ((benzyl(hydroxy)-amino)(4-chlorophenyl)methyl)-diphenylphosphine oxide, C26H23ClNO2P
- The crystal structure of ethyl 3-(1-methyl-1H-indole-2-carbonyl)-2-phenylquinoline-4-carboxylate, C28H22N2O3
- The crystal structure of 1,4-bis(1H-imidazol-3-ium-1-yl)benzene dinitrate, C12H12N4 2+·2(NO3 −)
- Crystal structure of tris(hexafluoroacetylacetonato-κ2O,O′) bis(triphenylphosphine oxide-κ1O)samarium(III), C51H33F18O8P2Sm
- Crystal structure of 1-(4-(dimethylamino)phenyl)-2,3-bis(diphenylphosphoryl)propan-1-one, C35H33NO3P2
- Crystal structure of diaqua[bis(μ 2-pyridine 2,6-dicarboxylato) bismuth(III) potassium(I)], C14H10BiKN2O10
- Crystal structure of (R)-N, N ′-dimethyl-[1, 1′-binaphthalene]-2, 2′-diamine, C22H20N2
- Crystal structure of 1-phenyl-4-(2-furoyl)-3-furyl-1H-pyrazol-5-ol, C18H12N2O4
- Crystal structure of bis(14,34-dimethyl[11,21:23,31-terphenyl]-22-yl)diselane, C40H34Se2
Articles in the same Issue
- Frontmatter
- New Crystal Structures
- The crystal structure of hexaquazinc(II) poly[hexakis(μ2-4-methylbenzenesulfinato-κ2O:O′) dizinc(II)]
- 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
- Crystal structure of bis[(triaqua-4-iodopyridine-2,6-dicarboxylato-κ 3 N,O,O ″)cobalt(II)] trihydrate, C14H22N2O17I2Co2
- 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
- Crystal structure of poly[μ2-dichlorido-(μ2-1-[(2,4-dimethyl-1H-triazole-1-yl)methyl]-1H-benzotriazole-κ2N:N′)cadmium(II)], C11H12CdN6Cl2
- The crystal structure of (3aS, 4R, 7S, 7aR)-hexahydro-4, 7-methano-1H-isoindole-1, 3-(2H)-dione, C9H11NO2
- The crystal structure of N-(acridin-9-yl)-4-chloro-N-(4-chloro-butanoyl) butanamide, C21H20Cl2N2O2
- Crystal structure of 3,3′-dimethoxy-4,4′-oxy-di-benzaldehyde, C16H14O5
- 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
- Crystal structure of methyl-1-(naphthalen-1-yl)-2,3,4,9-tetrahydro-1H-pyrido[3,4-b] indole-3-carboxylate, C23H20N2O2
- Crystal structure of tetrapropylammonium bicarbonate–1-(diaminomethylene)thiourea(1/1)
- 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
- Crystal structure of bis(N,N,N-trimethylbutanaminium) tetrathiotungstate(VI), (BuMe3N)2[WS4]
- 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
- Crystal structure of 1–methyl-3-propyl-4-nitro-1H-pyrazole-5-carboxylic acid, C8H11N3O4
- Crystal structure of N-(benzo[d]thiazol-2-yl)-2-chloroacetamide, C9H7ClN2OS
- The crystal structure of N-benzyl-2-chloro-N-(p-tolyl) acetamide, C16H16ClNO
- Crystal structure of 3,4-dimethoxybenzyl 2-(6-methoxynaphthalen-2-yl)propanoate, C23H24O5
- Crystal structure of 2,5-bis(2,5-dimethoxybenzyl)-3,6-dimethyl-2,5-dihydropyrrolo[3,4-c]pyrrole-1,4-dione, C26H28N2O6
- 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
- The crystal structure of bis(2-(piperidin-1-ium-4-yl)-1Hbenzo[d]imidazol-3-ium) dihydrogen decavanadate, C24H36N6O28V10
- Crystal structure of diaqua-bis(1-(3-carboxyphenyl)-5-methyl-4-oxo-1,4-dihydropyridazine3-carboxylato-O,O′)-cobalt(ii)dihydrate, C26H36N4O14Co
- 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
- 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
- Crystal structure of (3R)-1-(3,5-dimethoxyphenyl)-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole-3-carboxylate chloride, C21H23ClN2O4
- Synthesis and crystal structure of 3-(4,5-dihydroisoxazol-3-yl)-2-methyl-4-(methylsulfonyl)benzoic acid, C12H13NO5S
- The crystal structure of hexaaquamagnesium(II) bis-3-(1,2,3,4-tetrahydrobenzo[4,5]imidazo[1,2-α]pyridin-1-yl)benzoate, C36H42N4O10Mg
- Crystal structure of 4-formyl-2-methoxyphenyl 2-acetoxybenzoate, C17H14O6
- 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
- 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
- Crystal structure of benzo[d][1,3]dioxol-5-ylmethyl 2-(6-methoxynaphthalen-2-yl)propanoate, C22H20O5
- Crystal structure of N-benzoyl-N-phenylhydroxylaminato-dicarbonylrhodium(I), [Rh(BNA)CO2]
- The crystal structure of N-(2-((2-methoxynaphthalen-1-yl)ethynyl)phenyl)-4-methylbenzenesulfonamide, C26H21NO3S
- The crystal structure of methyl ((4-aminobenzyl)sulfonyl)-d-prolinate, C13H18N2O4S
- The crystal structure of dichlorido-(N-isopropyl-N-(pyridin-2-ylmethyl)propan-2-amine-κ 2 N, N′)palladium(II), C12H20N2PdCl2
- 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
- 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
- Synthesis, crystal structure and nonlinear optical property of 1-((propan-2-ylideneamino)oxy)propan-2-yl-4-methylbenzenesulfonate, C13H19O4NS
- The crystal structure of N,N-(ethane-1,1-diyl)dibenzamide, C16H16N2O2
- Crystal structure of 1-(4-bromophenyl)-3-(diphenylphosphoryl)-3-hydroxypropan-1-one, C21H18BrO3P
- 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
- 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
- Crystal structure of tetraethylammonium bicarbonate–1-(diaminomethylene)thiourea(1/1)
- Crystal structure of 1-cyclohexyl-4-p-tolyl-1,4-dihydropyridine-3,5-dicarboxylic acid dimethyl ester, C22H27NO4
- The crystal structure of catena-poly(μ2-1,4-bis-(1H-imidazol-1-yl)benzene-copper(I)) dichloridocopper(I), {[CuC12H10N4]+[CuCl2]−} n
- The crystal structure of propane-1-aminium-2-carbamate, C4H10N2O2
- Crystal structure of 5,6,3′,4′,5′-pentamethoxy-flavone dihydrate, C20H24O9
- Crystal structure of (E)-N-(2-bromophenyl)-4-(4-(3,5-dimethoxystyryl)phenoxy)pyrimidin-2-amine, C26H22BrN3O3
- 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
- The crystal structure of 1-(2-chlorophenyl)-3-(p-tolyl)urea, C14H13ClN2O
- The crystal structure of 1-cyclohexyl-3-(p-tolyl)urea, C14H20N2O
- Crystal structure of ((benzyl(hydroxy)-amino)(4-chlorophenyl)methyl)-diphenylphosphine oxide, C26H23ClNO2P
- The crystal structure of ethyl 3-(1-methyl-1H-indole-2-carbonyl)-2-phenylquinoline-4-carboxylate, C28H22N2O3
- The crystal structure of 1,4-bis(1H-imidazol-3-ium-1-yl)benzene dinitrate, C12H12N4 2+·2(NO3 −)
- Crystal structure of tris(hexafluoroacetylacetonato-κ2O,O′) bis(triphenylphosphine oxide-κ1O)samarium(III), C51H33F18O8P2Sm
- Crystal structure of 1-(4-(dimethylamino)phenyl)-2,3-bis(diphenylphosphoryl)propan-1-one, C35H33NO3P2
- Crystal structure of diaqua[bis(μ 2-pyridine 2,6-dicarboxylato) bismuth(III) potassium(I)], C14H10BiKN2O10
- Crystal structure of (R)-N, N ′-dimethyl-[1, 1′-binaphthalene]-2, 2′-diamine, C22H20N2
- Crystal structure of 1-phenyl-4-(2-furoyl)-3-furyl-1H-pyrazol-5-ol, C18H12N2O4
- Crystal structure of bis(14,34-dimethyl[11,21:23,31-terphenyl]-22-yl)diselane, C40H34Se2