Syn thesis and Crysta l Structure of Neodym ium Com plex w ith Glyc ine [Nd (Gly) (H2O ) 7 ]Cl3

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1 V o l. 15 N o Chem ical R esearch in Ch inese U niversities Syn thesis and Crysta l Structure of Neodym ium Com plex w ith Glyc ine [Nd (Gly) (H2O ) 7 ]Cl3 L I Jun2ran 3 3, ZHOU L i2p ing and J IN T ian2zhu (S tate K ey L aboratory of R are E arth M aterials Chem istry and A pp lication, P ek ing U niversity, B eij ing , P. R. Ch ina) YU Ka i2bei (Cheng d u Centre f or A naly sis and M easu rem ent, A cad em ic S inica, Cheng d u , P. R. Ch ina) (R eceived M ay 13, 1999) T he title comp lex [N d (Gly) (H 2O ) 7 ]C l3 w as synthesized and its crystal structure w as deter2 m ined by X2ray diffraction to obtain a final R value of and a w R value of T he crystal is of m onoclinic system w ith a space groug Pm. Every tw o neodym ium ions in the crystal are connected w ith a carboxyl group to fo rm a po lym eric chain mo lecule. A nd each neodym ium ion is further coo rdinated w ith seven oxygen atom s from w ater mo lecules. T he counter ion (C l - ) is non2coo rdinated to fill up the space betw een the po lym eric chainṡ So the N d 3+ cation is nine2coo r2 dinated and the coo rdination po lyhedron is a trigono tetradecahedron. In addition, there exists the m irro r symm etry in the comp lex. Ke yw o rds N eodym ium comp lex, Glycine, C rystal structure In troduction A pp lication of the rare earth compounds have been found in m edicine and agricu ltu re. So there m ay be rare earth compounds in pep tide and p ro tein comp lexes. It is impo rtan t to understand mo re clearly the bonding of the lan than ide ion s in the coo rdination compounds w ith am ino acids. Som e rare earth coo rdination compounds w ith glycine w ere syn thesized and the crystal structu re w ere determ ined [1_ 5 ]. But there is no crystallograph ic study on the com p lex com po sed of N dc l3 and g lycine. To fu rther invest iga te the in teract ion betw een N dc l3 and glycine, w e studied the syn thesis and crystal structu re of the title comp lex. Exper im en tal 1 Prepara tion of the Title Com plex N dc l3 and glycine w ere m ixed in an 1 1 mo lar ratio in w ater at ph 3. A purp lish red single crystal w as ob tained by the slow evapo ration of the aqueou s so lu tion at room tempera2 3 Suppo rted by the State Key L abo rato ry of R are Earth M aterial Chem istry and A pp lication, the C lim bing P rogram, and the N ational Key P ro ject fo r Foundam ental R esearch. 3 3 To w hom co rrespondence should be addressed.

2 N o. 4 L I Jun2ran, ZHOU L i2p ing, J IN T ian2zhu et al. 307 tu re. 2 IR Spectra and Therma l Ana lysis of the Com plex T he IR spectra of the comp lex and glycine w ere ob tained from KB r pellets at room tem 2 peratu re u sing a N ico let M agna2ir 750 spectropho tom eter. T he resu lts of the therm al analy2 sis w ere ob tained u sing a DU PON T 1090B therm al analyzer. 3 X-ray Ana lysis T he purp lish red crystal of the title comp lex w as w rapped w ith the glue fo r structu re de2 term ination. T he reflection s w ere co llected on a Siem en s P4 diffractom eter. T he in ten sities w ere co rrected fo r ab so rp tion by a sem i2emp irical m ethod from p si2scan ṡ T he neodyn ium ion coo rdinates w ere determ ined by direct m ethod and all the non2hydrogen atom s w ere de2 term ined by difference Fou rier syn theses. T he refinem en t w as m ade by fu ll2m atrix least2 squares on F 2. Results and D iscuss ion 1 The Com position of the Com plex T he compo sition of the comp lex w as deduced from the elem en tal analyses. Found (% ) : N d 3112, C 5179, H 3199, N 3134, w h ich are con sisten t w ith the calcu lated resu lts (% ) : N d 3119, C 5131, H 4121, N 3110 from the fo rm u la [N d (Gly) (H 2O ) 7 ]C l3 ob tained by diffrac2 tion analysiṡ 2 IR Spectra and Therma l Ana lysis Compared w ith the IR spectrum of glycine, the Μas (carboxyl) band of the comp lex w as flooded by the s (H 2O ) band (a strong and w ide band at cm - 1, w h ich indicates that there are m any w ater mo lecu les in the comp lex [2 ] ), the Μs (carboxyl) band of the comp lex at cm - 1 w as no t sh ifted to h igher w ave num bers although the carboxyl group of glycine w as coo rdinated to the neodym ium ion. T he resu lt is uncommon fo r the coo rdination com 2 pounds of carboxylic acids [2_ 5 ]. T he therm al dissociation data are listed in T ab le 1. T able 1 T he therm al dissociation data of the comp lex tg 75. 8_ _ _ 514 L o ss of w eigh t 3 (% ) (7. 97) (19. 92) (16. 60) Fo rm ula of p roduct N dc l3 (Gly) (H 2O ) 5 N dc l3 (Gly) N dc l3 3 Calculated value from the fo rm ula [N dc l3 (Gly) (H 2O ) 7 ] in parentheseṡ T he resu lts in T ab le 1 show that the p rocesses of lo sing the w ater mo lecu les in the com 2 p lex are divided in to tw o step ṡ T h is can be exp lained by the fact that the five ones of the seven coo rdination bonds betw een N d 3+ and seven H 2O mo lecu les are stronger than the o ther tw o. In addition, the temperatu re of lo sing glycine is h igher than that of lo sing w ater, w h ich show s that the coo rdination bond betw een N d 3+ and the carboxyl oxygen atom is stronger than that betw een N d 3+ and the oxygen atom in w ater mo lecu le. 3 The Crysta l Structure T he crystal data, details of data co llection and refinem en t are listed in T ab le 2. T he se2

3 308 Chem ical R esearch in Ch inese U niversities V o l. 15 lected bond length s and angles are given in T ab le 3. T he crystal structre of the title com 2 p lex, the coo rdination po lyhedron around the cen tral ion and the cell of the crystal are illu s2 trated in F ig. 1, F ig. 2 and F ig. 3, respectively. Emp irical fo rm ula C rystal size C rystal system Space group T able 2 T he crystal data and details of data co llection and refinem ent C 2H 19NO 9C l3n d mm mm mm Reflection co llected M onoclinic Pm agnm (10) bgnm (2) cgnm (10) Βg( ) (10) V gnm (2) Z 4 M D c (g cm - 3 ) Ηrange ( ) 3_ 66 Independent reflections O bserved reflections 2 861[Fo> 4. 0Ρ(F o) ] W eigh ting schem e N um ber of 167 param eters refined F inal R F inal w R Goodness of fit on F w - 1 = Ρ 2 (F 2 o) + ( P ) P P = [m ax (F 2 o, o) + 2F 2 c ]g3 Θm ax, Θm ing(e nm - 3 ) 1 552, T able 3 T he selected bond length s (nm ) and angles ( ) of the comp lex 3 N d1 O (11) N d1 O (9) N d1 O (8) O 1 N d1 O 2a (4) O 1 N d1 O 3c (3) O 1 N d1 O 4c (3) O 1 N d1 O (2) O 2a N d1 O (2) O 2a N d1 O (2) O 2a N d1 O (4) O 2a N d1 O 6c (3) O 3 N d1 O (3) O 3 N d1 O (4) O 3 N d1 O 6c (3) O 3c N d1 O 4c (3) N d1 O (13) N d1 O 6c (9) N d1 O 2a (12) O 3c N d1 O (3) O 4 N d1 O 4c (4) O 4 N d1 O (3) O 4c N d1 O (2) O 4c N d1 O 6c (3) O 5 N d1 O 6c (3) O 1 N d1 O (3) O 1 N d1 O (3) O 1 N d1 O (4) O 1 N d1 O 6c (2) O 2a N d1 O 3c (2) O 2a N d1 O 4c (2) N d1 O 3c (9) N d1 O 4c (8) N d1 O (9) O 2a N d1 O (3) O 3 N d1 O 3c (5) O 3 N d1 O 4c (3) O 3 N d1 O (3) O 3c N d1 O (3) O 3c N d1 O (4) O 3c N d1 O 6c (3) O 4 N d1 O (2) O 4 N d1 O 6c (2) O 4c N d1 O (2) O 5 N d1 O (3) O 6 N d1 O 6c (4) 3 Symm etry operation: a. x + 1, y, z; b. x, - y + 1, z; c. x - 1, y, z; d. x, - y, z. T able 4 T he non2hydrogen atom ic coo rdinates ( 10 4 nm ) and equivalent iso trop ic disp lacem ent param eters ( 10 5 nm 2 ) of the comp lex A tom x y z U eq N d1-591 (1) (1) 13 (1) N d2 536 (1) (1) 12 (1) C l (8) (2) (4) 39 (1) C l (9) (2) (5) 41 (1) C l (9) (3) (7) 49 (1) O (21) (12) 26 (3) O (19) (13) 17 (2) O (14) (7) (13) 29 (2) O (13) (6) (10) 22 (2) O (25) (15) 22 (2) O (16) (5) (10) 21 (2) O (14) (12) 17 (2) A tom x y z U eq O (20) (14) 24 (3) O (16) (6) (11) 26 (2) O (18) (6) (13) 33 (2) O (19) (7) (12) 30 (2) O (25) (14) 28 (3) N (32) (23) 41 (4) N (22) (15) 25 (3) C (21) (15) 9 (2) C (30) (20) 27 (4) C (34) (23) 25 (3) C (25) (20) 19 (3) In the comp lex, each N d 3+ ion is coo rdinated w ith tw o carboxyl oxygen atom s from dif2

4 N o. 4 L I Jun2ran, ZHOU L i2p ing, J IN T ian2zhu et al. 309 feren t g lycine m o lecu les and seven oxygen atom s of w ater. T he n ine coo rdinating oxygen a tom s fo rm a t rigono tet radecahed ron. Every tw o N d 3+ ion s are connected by a carboxyl group from the glycine serving as the carboxyl b ridge, fo rm ing a one2dim en sional chain com 2 p lex of infin ite length. T he C l - an ion is non2 coo rdinated to the N d 3+ ion. T he long chain of {[N d (Gly) (H 2O ) 7 ] 3+ }n has a m irro r symm e2 try. T he C, N and O atom s in the glycine mo lecu le, an oxygen atom of w ater and the N d 3+ ion are in the mo irro r. T he o ther six oxygen atom s of w ater are distribu ted ou tside of the m irro ṙ T he cell has also the m irro r symm etry (F ig. 3). T here are tw o types of structu re un its in the cell. T he d ifference betw een their st ruc2 tu res (bond length s and angles) is sm all. Comparing the bond length s betw een F ig. 1 T he structure of [N d (Gly) (H 2O ) 7 ]C l3. N d 3+ and carboxylic oxygen atom s, the bond length of N d1 O 2a [ ( 12) nm ] is longer than that of N d1 O 1[ (11) nm ]. T he difference ( nm ) is larger. So the chain of the po lym eric mo lecu les can be easily b roken in to sm aller mo lecu les w hen they are heated o r disso lved in w ater [6 ]. F ig. 2 T he coo rdination po lyhedron of the N d 3+ ion in [N d (Gly) (H 2O ) 7 ]C l3. F ig. 3 T he cell pack ing of [N d (Gly) (H 2O ) 7 ]C l3.

5 310 Chem ical R esearch in Ch inese U niversities V o l. 15 F rom the bond length of N d O (H 2O ), w e found that the length s of N d1 O 6 and N d1 O 6c bonds are m uch longer than tho se of the o ther five N d O (H 2O ) bonds, and the bond length s of all N d O (H 2O ) are longer than that of N d1 O 2a (COO ). T hese differ2 ences among the bond length s cau se the resu lts of the therm al analysis above m en tioned. T here are hydrogen bonds no t on ly among the w ater mo lecu les bu t also betw een the w a2 ter mo lecu les and the am ino2group of glycine mo lecu les in the crystal structu re. Zhao J ian jun et a l. [5 ] syn thesized the comp lex [E r2 (Gly) 2 (H 2O ) 12 ] (C lo 4) 6 4H 2O. T he mo lar ratio betw een the rare earth ion and glycine in the comp lex is the sam e as that in the ti2 tle comp lex, how ever, the comp lex in literstu re [ 5 ] is a b inuclear comp lex, it has no t the m irro r symm etry, the coo rdination num ber of the E r 3+ is 8 and its coo rdination po lyhedron is a disto rted square an tip rism. Re fe re nce s [ 1 ] L egendziew icz J., H uskow ska E., W askow ska A. et al., Ino rg. Ch im. A cta, 92, 151 (1984) [ 2 ] J IN T ian2zhu, YAN G Chang2qing, YAN G Q ing2chuan et al., Chem. J. Ch inese U niversities (Ch inese), 10 (2), 118 (1989) [ 3 ] J IN T ian2zhu, SUN X iao2dong, XU Guang2xian, J. Ch inese R are Earth Society (Ch inese), 8 (3), 194 (1990) [ 4 ] CH EN Ju2xiang, RAN X in2quan, GUO Zh i2zhen et al., Chem. J. Ch inese U niversities (Ch inese), 13 (9), (1992) [ 5 ] ZHAO J ian2jun, J IN T ian2zhu, Chem. J. Ch inese U niversities (Ch inese), 17 (4), 519 (1996) [ 6 ] L I Jun2ran, ZHOU L i2p ing, J IN T ian2zhu, J. Ch inese R are Earth Society (Ch inese), 15 (2), 97 (1997)

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