CN107652436A - A kind of different price double-core manganese（II, III）One-dimensional Dual-band type coordination polymer and preparation method thereof - Google Patents
A kind of different price double-core manganese（II, III）One-dimensional Dual-band type coordination polymer and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to functional complexes material, inorganic organic framework materials and crystal engineering field, more particularly to a kind of one-dimensional Dual-band type coordination polymer of different price double-core manganese (II, III) and preparation method thereof.The compound has below formula：{[Mn(II)2(4,4’‑bpy)2(L)4]2[Mn(III)2(4,4’‑bpy)2(L)4(H 2 O)2].(L)2·8H 2 O}n；Described 4,4 ' bpy are 4,4 ' bipyridyls, and HL is 4 fluobenzoic acids；Advantages of the present invention：The compound has the manganese ion of 2 kinds of different valence states, 2 kinds of different one-dimensional bands is constituted, with 2 between band and band：1 ratio ordered arrangement, three-dimensional network frame structure is constituted, the crystallization water, noncoordinating 4 fluobenzoic acid root are located in pipeline space, have potential application prospect in absorption, ion exchange and catalysis etc..
Description
Technical field
The present invention relates to functional material, crystallography field, more particularly to a kind of different price double-core manganese (I I, III) double-core
One-dimensional Dual-band type coordination polymer of manganese (II, III) and preparation method thereof.
Background technology
Metal organic frame (metal-organic frameworks, MOFs) material is one kind by organic ligand and metal
The material with adjustable aperture being self-assembly of is passed through at center.Compared with traditional inorganic porous material, MOFs materials have
Bigger specific surface area, higher porosity, structure and function are more various, thus be widely used in gas absorption with
It is all in nonlinear optical material, magnetic material, superconductor etc. in the fields such as separation, sensor, medicament slow release, catalytic reaction
Many-side shows fabulous application prospect.Solid material can be predicted using organic bridge ligand and metal ion assembling acquisition
Geometry, wherein coordinate bond or hydrogen bond, π-π aromaticring stackings weak interaction, electrostatic interaction and space support act on tune
Control MOF topological structures and aspect of performance have very important effect.The bridge ligands such as halogenated aromatic acid, 4,4 '-bipyridyl can
One-dimensional, two and three dimensions supermolecule is assembled into various metals, relevant non-linear optical property, catalytic action, photoelectric conversion
The achievement in research of energy has been appeared in the newspapers.
Synthesis, crystal structure and the photoluminescent property of 2,3- difluoro-benzoic acid terbium coordination compounds characterize, Capital Normal University's journal
(natural science edition) the 2nd phase of volume 31, in April, 2010, P28~31, disclose and double-core terbium coordination compound has been synthesized using solwution method
[Tb (2,3-DFBA) 3 (2,2 '-bipy)] 2 (2,3-DFBA=2,3- difluoro-benzoic acid root, 2,2 '-bipy=2,2 '-connection pyrrole
Pyridine), and the complexs are determined with X-ray single crystal diffraction to its crystal structure and belong to monoclinic system, P2 (1)/n spaces
Group is in complex, 2 Tb3+Ion is connected by 42,3- difluoro-benzoic acids roots in a manner of bridging bidentate；Each Tb3+From
Son ligancy be 8, respectively with 4 bridging bidentates 2,4 oxygen atoms of 3- difluoro-benzoic acid roots, the 2,3- of 1 chelating bidentate
2 oxygen atoms of difluoro-benzoic acid root and 12,2 nitrogen-atoms coordination of 2 '-bipyridyl complexs are in ultra violet lamp
Under send strong green glow, there are 4 spectral lines at 489,545,583 and 618nm in its fluorescence spectrum, and this is by Tb3+Ion
Caused by 5D4 → 7Fj (j=6~3) transition.
Binuclear Europium and 2,5- difluoro-benzoic acid and 2, synthesis, crystal structure and the sign of 2 '-bipyridyl complex are inorganization
Journal is learned, the 10th phase of volume 24, in October, 2008, P1621~1625, discloses and has synthesized mixed ligand coordination compound [Eu with solwution method
(2,5-DFBA) 3 (2,2 '-bipy)] 2 (2,5-DFBA=2,5- difluoro-benzoic acid roots, 2,2 '-bipy=2,2 '-bipyridyl),
And determine its crystal structure.The crystal belongs to anorthic system, P1 space groups.In complex, 2 Eu3+Ion is by 4 2,5-
Difluoro-benzoic acid root connects in a manner of bidentate bridging and three bridge works join 2 kinds；Each Eu3+The ligancy of ion be 9, respectively with 4
5 oxygen atoms of bridging 2,5- difluoro-benzoic acid roots, 2 oxygen atoms of 1 bidentate chelating 2,5- difluoro-benzoic acid roots and 1
2 nitrogen-atoms coordination of bipy 2,2' bipyridyl molecule.The complex sends strong feux rouges under ultra violet lamp, in fluorescence light
Occur 5 spectral lines at 580,591,613,648 and 693nm of spectrum, be by Eu respectively3+5D0 → 7Fj (j=0~4) jumps of ion
Caused by moving.
The content of the invention
, should it is an object of the present invention to provide a kind of one-dimensional Dual-band type coordination polymer of different price double-core manganese (II, III)
Polymer, for part, the ion centered on transition metal, tool is assembled into by coordination bonding with 4,4 '-bipyridyl and halogenated aromatic acid
There is the supermolecule of one-dimensional Dual-band type structure.Another object of the present invention is to provide above-mentioned different price double-core manganese (II, III)
The preparation method of one-dimensional Dual-band type coordination polymer；
In order to realize first above-mentioned purpose, present invention employs following technical scheme：
A kind of one-dimensional Dual-band type coordination polymer of different price double-core manganese (II, III), its structural formula are as follows：
Described 4,4 '-bpy are 4,4'-Bipyridine, and HL is 4- fluobenzoic acids；
Described different price double-core manganese (II, III) coordination polymer is by two kinds of one-dimensional bands, the 4- fluobenzoic acids not being coordinated
Root and crystalline water molecules composition, bivalent manganese and Manganic ion have respectively constituted the one-dimensional banding coordination polymerization of two kinds of different double-cores
Chain；
In the one-dimensional band that bivalent manganese is formed, each Mn (II) atoms and 4 oxygen atoms from 3 4- fluobenzoic acid roots
It is coordinated with 2 nitrogen-atoms from 24,4 '-bpy, constitutes the hexa-coordinate MnN slightly to distort2O4Octahedral coordination environment；
2 4- fluobenzoic acid radical ion bridging Mn (1) (II), Mn (2) (II) atomic building double-core manganese node,2 4,4'-Bipyridine molecules distinguish 2 Mn (II) nodes of bridging, form edge
[100] the one-dimensional condensation zone that direction infinitely extends；Its bond distance and bond angle are ∠ (N-Mn-N)=174.33 (9) -179.04 (10) °；
Manganic form one-dimensional band in, each Mn (III) atoms except with 3 from 3 4- fluobenzoic acid roots
Oxygen atom and from 24,4 '-bpy 2 nitrogen-atoms coordination is outer, is also coordinated, constitutes slightly abnormal with 1 water of coordination molecule oxygen
The hexa-coordinate MnN of change2O4Octahedral coordination environment；
2 4- fluobenzoic acid radical ions bridgings 2 Mn (III) atomic buildings double-core manganese node,2 4,4'-Bipyridine molecule difference bridgings, 2 Mn
(III) node, another one-dimensional condensation zone infinitely extended along [100] direction is formd；Its bond distance and bond angle be d (Mn-O)=∠ (N-Mn-N)=178.29 (9) °,
Bivalent manganese is with the band A of manganic composition and with B with 2：1 ratio simultaneously mutually staggers by AABAAB form, passes through
Water of coordination, the crystallization water, coordination and noncoordinating 2- fluobenzoic acids root oxygen atom (fluorine atom) between strong hydrogen bonding act on forming three
Tie up supramolecular network structure,∠ (O-H ... O)=111-172 °, d (O-H ... F)=∠ (O-H ... F)=112-138 °.
In order to realize second above-mentioned purpose, present invention employs following technical scheme：
A kind of preparation method for preparing the above-mentioned one-dimensional banding coordination polymer of different price double-core manganese (II, III), this method include
Following step：Freshly prepared MnCO3, 4- fluobenzoic acids F6H4COOH, 4,4-Bipyridine, with CH3OH/H2O(v:V=1:2)
Mixed solvent 15mL mix stirring a few hours, then the khaki suspension of gained is enclosed the stainless steel of inner liner polytetrafluoroethylene
In reactor, reactor is finally placed in 160 DEG C of temperature programmed control of baking oven inside holding one week by compactedness 60-85%.Naturally it is cold
But to room temperature, it is filtered to remove khaki insoluble matter.Gained pale yellow filtrate is placed in natural evaporation at room temperature, is fitted after one month
Yellow crystals for monocrystalline test；With distillation water washing after spontaneously dry.
The features of the present invention：First, crystal structure is by 2 kinds of different polymeric chains and noncoordinating 4- fluobenzoic acids radical ion, knot
Brilliant hydrone composition, the coordination mode of different price double-core manganese node is different, then by 4,4-bipyridyl molecule bridging forms 2 kinds of differences
Polymeric chain, O-H ... O, O-H ... F hydrogen bond actions of interband and interlayer form Three-dimensional Supramolecular Network structure, constituted by more
The three-dimensional tube of kind micropore composition；Second, 2 kinds of different polymeric chains are by 2：1 ratio is closely staggeredly accumulated, and accounts for total amount 12%
The crystallization water, noncoordinating 4- fluobenzoic acids radical ion in micropore, be heated to 200 DEG C or so, polymer can form porous network
Framework, and with exchange of solvent, the possibility of anion exchange, absorption, catalysis and ion exchange material in terms of etc. tool
There is application prospect.
Brief description of the drawings
Fig. 1 is the construction unit (coordination environment) of the compounds of this invention.
Fig. 2 is 2 kind coordination polymerization chains of the compounds of this invention along the extension of [100] direction.
Fig. 3 is accumulation graph of the compounds of this invention along [100] direction.
Fig. 4 is the infrared spectrum of the compounds of this invention.
Fig. 5 is the TG curves of the compounds of this invention.
Fig. 6 is the powder diagram of the compounds of this invention.
Embodiment
1.1 reagents and instrument
Agents useful for same is ommercially available AR, VarioIII types elemental analyser (German Elementar companies), FT-IR
Instrument (Nicolet companies of U.S. EXUS670 types)；TGA/SDTA 851eInstrument (Meltter-Toludo companies of Switzerland)；BIUKER is public
Take charge of APEX CCD II type single crystal diffractometers；SQUID Quantum Design Model MPMS -7 type magnetometers
The synthesis of 1.2 complexs
Weigh MnCl2H2O 0.189g (1.50mmol) are dissolved in appropriate distilled water, then add enough saturated sodium carbonates
Solution, centrifuge and wash MnCO35 times, take freshly prepared MnCO3, then add 4- fluobenzoic acids FC6H4COOH0.072g
(0.50mmol), 4,4-Bipyridine 0.160g (0.65mmol), with CH3OH/H2O(v:V=1:2) mixed solvent 15mL
Stirring 2.0 hours is mixed, then the khaki suspension of gained is enclosed in the stainless steel cauldron of inner liner polytetrafluoroethylene, filling
60-90% is spent, reactor is finally placed in 160 DEG C of temperature programmed control of baking oven inside holding one week.Room temperature is naturally cooled to, is filtered
Remove colour of loess insoluble matter.Gained pale yellow filtrate is placed in natural evaporation at room temperature, obtains being applied to monocrystalline test after one month
Yellow bulk crystals.With distillation water washing after spontaneously dry.
1.3 crystal structure determination
Selection size is 0.410mm × 0.250mm × 0.170mm monocrystalline, is collected on APEX CCD II type single crystal diffractometers
Diffraction data, using MoK alpha raysIn the range of 3.11 °≤θ≤25.00 ° with ω andScan mode
29813 data are collected into altogether, wherein independent point diffraction 13145 [R (int) >=0.0371], 9347 [F0 2≥2σ(F0 2)] can
Observation point diffraction is used for structural modifications, and diffracted intensity data are through the Lp factors and empirical absorption correction.Whole non-hydrogen atoms are using straight
Connection obtains, and non-hydrogen atom coordinate and its anisotropic temperature factor use complete matrix least square method amendment, on carbon atom
Hydrogen atom is obtained by theory hydrogenation.Predominant crystal data is listed in table 1.W=1/ [σ2(F0 2)+(0.0458×P)2+1.71×
P], P=(F0 2+2Fc 2)/3.The S values of last wheel amendment are 1.031, (Δ/σ)maxFor 0.001, in difference Fourier most
Big remaining peak Δ ρmax=378e/nm3, peak Δ ρ more than Minimum Residualmin=-355e/nm3.All calculating use SHELX -97 programs[6 ,7], carried out on PentiumIV 300.≥
The crystallographic data of the complex of table 1
2.1 infrared spectrum
Infrared spectrum (shown in Fig. 4) principal character peak of the compounds of this invention is attributed to：3067cm-1, stretched for C-H on aromatic ring
Contracting absorption of vibrations, 3442cm-1Absorbed for the stretching vibration of water of coordination and crystallization water O-H keys, 1608cm-1,1577cm-1,
1547cm-1, 1412cm-1For aromatic ring frame absorption of vibrations, 1608cm-1,1412cm-1For double coordination carboxylate anion (-
COO–) asymmetric and symmetric stretching vibration absorb, wherein 1608cm-1Absworption peak it is especially strong, be due to aromatic ring frame vibration
Absorb caused by the bimodal degeneracy of asymmetric absorption with carboxylic acid ion.
2.2 differential thermals-thermogravimetric analysis
Differential thermal-thermogravimetric analysis is carried out under nitrogen protection, nitrogen rate 20mLmin–1, heating rate is 10 DEG C of min–1, mark
The TG curves of topic complex sample show (shown in Fig. 5), stablize at normal temperatures, are heated to 200 DEG C or so and successively lose the crystallization water, match somebody with somebody
Position water and noncoordinating 4- fluobenzoic acids radical ion, form the metal organic frame with functions such as absorption, catalysis and ion exchanges
Material.
2.3 crystal structure
Complex of the present invention
The main bond distance of (bpy=Bipyridine, HL=4-fluorobenzoic acid) and bond angle are shown in Table 2, crystal structure
(shown in Fig. 1,2,3).Crystal structure analysis shows that the complex is the one-dimensional biobelt polymerization link that different price double-core manganese is formed
Structure.
In the one-dimensional band that bivalent manganese is formed, each Mn (II) atoms and 4 oxygen atoms from 3 4- fluobenzoic acid roots and
From 24,4 '-bpy 2 nitrogen-atoms are coordinated, and constitute the hexa-coordinate MnN slightly to distort2O4Octahedral coordination environment；
2 4- fluobenzoic acid radical ion bridging Mn (1) (II), Mn (2) (II) atomic building double-core manganese node,2 4,4'-Bipyridine molecules distinguish 2 Mn (II) nodes of bridging, form edge
[100] the one-dimensional condensation zone that direction infinitely extends；Its bond distance and bond angle are ∠ (N-Mn-N)=174.33 (9) -179.04 (10) °；
Manganic form one-dimensional band in, each Mn (III) atoms except with 3 oxygen originals from 3 4- fluobenzoic acid roots
Son and from 24,4 '-bpy 2 nitrogen-atoms coordination is outer, is also coordinated with 1 water of coordination molecule oxygen, constitutes what is slightly distorted
Hexa-coordinate MnN2O4Octahedral coordination environment；
2 4- fluobenzoic acid radical ions bridgings 2 Mn (III) atomic buildings double-core manganese node, d (Mn (3)-Mn (3)i)=2 4,4'-Bipyridine molecules distinguish 2 Mn (III) nodes of bridging, form
Another one-dimensional condensation zone infinitely extended along [100] direction；Its bond distance and bond angle be d (Mn-O)=2.116 (2)-∠ (N-Mn-N)=178.29 (9) °,
2 4- fluobenzoic acid radical ions bridgings 2 Mn (III) atomic buildings double-core manganese node, d (Mn (3)-Mn (3)i)=2 4,4'-Bipyridine molecules distinguish 2 Mn (III) nodes of bridging, form
Another one-dimensional condensation zone infinitely extended along [100] direction；Its bond distance and bond angle are
∠ (N-Mn-N)=178.29 (9) °,
Bivalent manganese is with the band A of manganic composition and with B with 2：1 ratio simultaneously mutually staggers by AABAAB form, passes through coordination
Water, the crystallization water, coordination and noncoordinating 2- fluobenzoic acids root oxygen atom (fluorine atom) between strong hydrogen bonding act on to be formed it is three-dimensional super
Molecular network structure,∠ (O-H ... O)=111-172 °, d (O-H ... F)=∠ (O-H ... F)=112-138 °.
The unique distinction of this crystal structure, first,+divalent, the manganese ion of 2 kinds of different valence states of+trivalent, constitute 2 kinds of differences
Double-core manganese, and then formed 2 kinds of different one-dimensional polymeric chains.Second, 2 kinds of different polymeric chains are by 2：The 1 orderly staggered row of ratio
Row, while also form the ordered arrangement of electroneutral polymeric chain and+1 valency cation chain.Third, the 4- fluorobenzene first that -1 valency is noncoordinating
Acid radical anion is present in the space of complex micropore simultaneously with crystalline water molecules, is that this complex is handed over as anion
Conversion materials, ionic catalyst provide necessary condition.
2. main bond distance of tableWith bond angle [°]
Symmetry transformations used to generate equivalent atoms:#1-x+2,-y+1,-
z；#2x-1,y,z；#3x+1,y,z.
Claims (10)
1. a kind of one-dimensional Dual-band type coordination polymer of different price double-core manganese (II, III), has following structural formula：
{[Mn(II)2(4,4’ -bpy)2(L)4]2[Mn(III)2(4,4’ -bpy)2(L)4(H2O)2].(L)2·8H2O}；
Described 4,4 '-bpy are 4,4'-Bipyridine, and HL is 4- fluobenzoic acids.
2. the one-dimensional Dual-band type coordination polymer of different price double-core manganese (II, III) according to claim 1, it is characterised in that：
The compound is made up of two kinds of one-dimensional bands, the 4- fluobenzoic acids root not being coordinated and crystalline water molecules, bivalent manganese and Manganic ion
Two kinds of different one-dimensional banding coordination polymerization chains are respectively constituted.
3. the one-dimensional Dual-band type coordination polymer of different price double-core manganese (II, III) according to claim 2, it is characterised in that：
In the one-dimensional band that the compound bivalent manganese is formed, each Mn (II) atoms and 4 oxygen atoms from 3 4- fluobenzoic acid roots and
From 24,4 '-bpy 2 nitrogen-atoms are coordinated, and constitute the hexa-coordinate MnN slightly to distort2O4Octahedral coordination environment；
2 4- fluobenzoic acid radical ion bridging Mn (1) (II), Mn (2) (II) atomic building double-core manganese node, d (Mn
(1)–Mn(2))= 4.085(2)Å；2 4,4'-Bipyridine molecules distinguish 2 Mn (II) nodes of bridging, form along [100] side
To the one-dimensional condensation zone infinitely extended；Its bond distance and bond angle are d (Mn-O)=2.070 (2) -2.404 (2), d (Mn-N)=
2.276 (3) -2.283 (2), ∠ (N-Mn-N)=174.31 (11) and 179.07 (11) °.
4. the one-dimensional Dual-band type coordination polymer of different price double-core manganese (II, III) according to claim 2, it is characterised in that：
The compound manganic form one-dimensional band in, each Mn (III) atoms except with 3 oxygen from 3 4- fluobenzoic acid roots
Atom and from 24,4 '-bpy 2 nitrogen-atoms coordination is outer, is also coordinated with 1 water of coordination molecule oxygen, constitutes and slightly distort
Hexa-coordinate MnN2O4Octahedral coordination environment；
2 4- fluobenzoic acid radical ions bridgings 2 Mn (III) atomic buildings double-core manganese node, d (Mn (3)-Mn (3)i)=
4.922 (2) [i=- x+2 ,-y+1 ,-z]；2 4,4'-Bipyridine molecules distinguish 2 Mn (III) nodes of bridging, form another
A kind of one-dimensional condensation zone infinitely extended along [100] direction；Its bond distance and bond angle are d (Mn-O)=2.115 (2) -2.193 (3)
, d (Mn-N)=2.290 (3) -2.298 (3), ∠ (N-Mn-N)=178.37 (11) °, d (Mn (3)-Mn (3)ii)=
11.645(2)Å, ( ii = x-1, y, z )。
5. the one-dimensional Dual-band type coordination polymer of different price double-core manganese (II, III) according to claim 2,3,4, its feature
It is：The compound bivalent manganese is with the band A of manganic composition and with B with 2：1 ratio simultaneously mutually staggers by AABAAB form,
Pass through the strong hydrogen bonding and the weak hydrogen of C-H ... O between the oxygen atom of water of coordination, the crystallization water, coordination and noncoordinating 2- fluobenzoic acids root
Key acts on forming two-dimentional supermolecule plane, between layers by the C21 and carboxyl O1 of 2- fluobenzoic acid rootsivAtom (iv=x, 1/
2-y, -1/2+z) between the weak hydrogen bond actions of C-H ... O constitute Three-dimensional Supramolecular Network structure；d(C–H…O = 3.123
(3)-3.379 (3), ∠ (C-H ... O)=120-166 °.
6. the preparation right of the one-dimensional Dual-band type coordination polymer of different price double-core manganese (II, III) according to claim 1 will
Ask, it is characterised in that the preparation method comprises the following steps：
1）Freshly prepared MnCO3, 2- fluobenzoic acids, 4,4'-Bipyridine, with CH3OH/H2O(v:v = 1:2) mixed solvent mixes
Stir a few hours, then the khaki suspension of gained is enclosed in the stainless steel cauldron of inner liner polytetrafluoroethylene, compactedness 60-
85%, reactor is finally placed in 120-160 DEG C of temperature programmed control of baking oven inside holding one week；
2）Room temperature is naturally cooled to, is filtered to remove khaki insoluble matter；
3）Gained pale yellow filtrate is placed in natural evaporation at room temperature, obtains being applied to the yellow crystals of monocrystalline test after one month；
4）With distillation water washing after spontaneously dry.
7. the experimental procedure 1 according to right 6）, it is characterised in that：Organic solvent used is methanol or ethanol.
8. according to the experimental procedure 1 described in right 6,7）, it is characterised in that：The ratio of organic solvent and distilled water is 1：2.0-2.5.
9. the experimental procedure 1 according to right 6）, it is characterised in that：React the stainless steel cauldron in inner liner polytetrafluoroethylene
Middle progress.
10. the experimental procedure 1 according to right 6）, it is characterised in that：Reaction temperature control range is 120-160 DEG C, reaction
About one week time.
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