X-ray Diffraction Studies of Co(II), Sm(III) and Nd(III) Complexes with Gliclazide (N-(hexahydrocyclopenta[c] pyrrol-2(1H)-carbamoyl)-4-methylbenzenesulfonamide, An Oral Antidiabetic Drug

Introduction

Polyfunctionally rings compounds and synthesis of their metal complex which have various biological activities and include hetero atom, have been formed in organic synthesis and coordination chemistry.^1-6 Many trasition and inner trasition metal complexes have been synthesized for analytical and commercial applications many of medicinal use.^7-9,24-28 literature survey reveals that the transition and inner transition metal complexes generally crystallized with tetrahedral, octahedral geometry. ^10-12

Experimental 

All the chemicals used for the preparation of complexes are of Hi-media AR grade E-merk. Metal complexes are synthesized by adding metal salt solution in appropriate solvent to the solution of the ligand. The mixture was refluxed for 3-4 hours. Then the precipitate of metal complxes was obtained. It is filtered, washed and dried in vacuum desiccators.

All selected metals forms 1:2 complexes with gliclazide were confirmed by Jobs  method as modified by Turner and Anderson.^13-14

Table 1: Physico-chemical and Analytical data of Gliclazide Complexes.

Results and Discussion

The X-ray diffraction of Co(II),Sm(III) and Nd (III) complexes with Gliclazide were obtained and summarized in following tables. All reflections has been indexed for h, k, l values using reported literature^15-23and full proof suit XRD software v.2.0 by using foolproof suite XRD software the d-values of metal complexes were obtained.

X-ray diffraction study of Gliclazide complexes

The X-ray diffraction pattern of Co(II), Sm(III) and Nd(III) complexes has been determined 2θ range from 6.1963 to 79.97884°,Diffractograms (Fig-1,2,3,) and data has been summarized in the following table..

Gliclazide (GLZ-Co)

Figure 1: X-ray difractogram of GLZ-Co Complex Click here to View figure

 

Table 1: Cell data and crystal parameter of GLZ-Co complex

a(Å) = 21.6990                                                                      Volume(abcsinb)Å= 13880.931

b(Å) = 23.1881                                                                Dcal=4.02100 g/cm³

c(Å) = 27.5891                                                                                                                         Dobs= 4.03241 g/cm³

Standard deviation = 0.024%                                  Crystal system       =    Monoclinic

α=90°, β=89.4°, γ =90°                                            Porosity(%)           =    2.837

Density  = 0.05329g/cm³                                          Particle size           =    15.794microns

Space group = Pm

2θ	I/I0	D(Obs)	D(Cal)	h	k	l
10.5540	69.89	8.38237	8.46731	1	0	3
16.3437	60.23	5.42369	5.42470	4	0	0
19.0109	99.40	4.66834	4.64949	2	3	4
19.8736	82.38	4.46760	4.46387	3	4	1
20.4293	53.81	4.34731	4.34770	1	4	4
22.0439	100.00	4.03241	4.02100	5	2	1
31.8513	52.99	2.80964	2.80664	7	1	4
39.3397	29.09	2.29037	2.28905	1	4	11
45.6199	37.40	1.98697	1.98754	9	3	7

 

Figure 2: X-ray difractogram of GLZ-Sm Complex   Click here to View figure

Table 2: Cell data and crystal parameters for [ (GLZ)₂Sm2H₂O] complex

a(Å) = 21.7621                                                Volume (abcsinβ)Å     = 14065.269

b(Å) = 23.4271                                            Dcal                        = 13.86574 g/cm³

c(Å) = 27.5913                                             Dobs                       = 14.17908 g/cm³

Standard deviation = 0.0034%                    Crystal system    = Monoclinic(Octahedral)

α =90°, β=89.2°, γ =90°                               Porosity(%)                        = 3.0055 %

Density                             = 0.059094g/cm³

Space group                        = Pm                              Particle size          =23.5720 microns

2 θ	I/I0	D(Obs)	D(Cal)	h	k	l
6.2336	100	14.17908	13.86574	1	1	1
16.2587	34.89	5.45184	5.43999	4	0	0
28.1979	21.43	3.16480	3.16244	-6	1	4
29.3552	34.62	3.04261	3.04027	2	3	8
41.0622	19.06	2.19818	2.19539	-4	6	9
50.4845	14.68	1.80782	1.80644	8	3	11
58.0457	8.22	1.58780	1.58759	10	1	12

From the cell data and crystal lattice one can conclude that Co(II),Sm(III) and Nd(III) complex is having monoclinic crystal

Figure 3: X-ray difractogram of GLZ-Nd Complex   Click here to View figure

 

Table 3: Cell data and crystal parameter of GLZ-Nd Complex

a(Å) = 21.762                                                                           Volume (abcsin b)Å= 14065.307

b(Å) = 23.4271                                                                                 Dcal = 13.86574 g/cm³

c(Å) = 27.274                                                                           Dobs =14.26441 g/cm³

Standard deviation = 0.0026%                                                     Crystal system             =      monoclinic

α=90°, β=89.2, γ =90°                                                                     Porosity(%)                   =      3.0055

Density = 0.0586592g/cm³                                                            Particle size                   =      15.484microns

Space group = Pm

2θ	I/I0	D(Obs)	D(Cal)	h	k	l
6.1963	100	14.26441	13.86574	1	1	1
16.0639	16.52	5.55751	5.51772	0	0	5
18.2478	2.92	4.86181	4.85591	-3	1	4
27.9094	10.13	3.19686	3.19271	-3	5	5
28.9225	15.47	2.76823	3.08474	-6	3	3
32.3407	2.16	2.42315	2.76573	7	3	3
37.1028	0.92	2.22463	2.42107	4	2	10
40.5523	8.43	2.09735	2.22284	3	10	1
43.1325	1.82	1.82716	2.09549	6	7	7
49.9132	6.76	1.76742	1.82558	-8	1	11
51.7224	0.86	1.61184	1.76595	12	3	0
57.1485	2.36	1.54030	1.61049	-6	13	1
60.0677	0.80	1.42229	1.53910	3	9	14

Conclusion

X-ray diffraction studies also confirms the complexes and formation of new bonds. The number of peaks in Gliclazide are 22 while that of (GLC)₂ Nd   (GLC)₂Co and (GLC)₂Sm. are 24,9 and 8 respectively  . Thus indicating that complexes formed are a well kit one moreover the X-ray pattern of neither Gliclazide all the reflections present are new ones and the patterns are fairly strong. On comparing the pattern obtained with available literature. It is evident that its pattern is not in good agreement with available information and thus confirms the formation of totally new complexes The X-ray pattern have been indexed by using computer software(FPSUIT 2.0V) and applying interactive trial and error method keeping in mind the characterstics of the various symmetry system,till a good fit was obtained between the observed and the calculated Sin²θ value.The unit cell parameters were calculated from the indexed data, from cell data and crystal lattice parameters of system. (GLC)₂Co.2H₂O and (GLC)₂Sm.2H₂O and (GLZ)₂Nd2H₂O complexes attributed to Monoclinic crystal system .

Table 4

Molecular Formula	complexes	Molr Weight (gm/mole)	Crystal/ System
(C15H20N3O3 S)2Co2H2O	Co(II)	739.75	Monoclinic
(C15H20N3O3 S)2Nd2H2O	Nd(III)	825.06	Monoclinic
(C15H20N3O3 S)2Sm2H2O	Sm(III)	831.18	Monoclinic

 

Scheme 1 Click here to View scheme

 

Where, M = Co(II),Sm(III) and Nd(III)

Proposed structure of (GLZ)₂Co2H₂O , (GLZ)₂Sm2H₂O and (GLZ)₂Nd2H₂O  complexes

Acknowledgement 

The author is thankful to the principal of Saifia Science College, Bhopal and Principal, of Cresent College of Technology , Bhopal for providing all necessary facilities and Punjab University for providing XRD spectra.

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