My GIA for 17 years
Professor Shao-Fan Lin
March 25, 2004
It is my great honor to be presented with the Distinguished Grantee Award. I must say that this honor should not belong to me only but to my group. Actually it is my group who has done those work for past 17 years. I am only a member of the group. I would never forget the valuable help of my friends in ICDD, Jerry Johnson, Ron Jenkins, Fangling Needham, Ting Huang, Shelley Wolkov and so on.
▉ SUBMIT REFERENCE PATTERNS
1. How I joined the ICDD GIA?
1980s The World Bank provided a loan to China to help Chinese Universities. 1986 Professor Jerry Johnson as the specialist came to Nankai University to help us in developing the application of computer in powder Diffraction. I was the host professor to welcome Dr. Johnson. Before leaving he pointed out that the specialty of organic chemistry is very strong in Nankai University and it has high quality single crystal and powder diffractometers, so, he suggested to me to join the ICDD GIA program. Since 1987 I began to apply the GIA and to submit reference patterns.
2. From 1987 to now I have my GIA program every year. Following list is the history of my GIA program.
year / The number of submitted patterns / year / The number of submitted patterns1987 / 14 / 1996 / 46
1988 / 20 / 1997 / 50
1989 / 30 / 1998 / 40
1990 / 30 / 1999 / 50
1991 / 40 / 2000 / 50
1992 / 40 / 2001 / 60
1993 / 40 / 2002 / 60
1994 / 40 / 2003 / 60
1995 / 40
Total / 710
3. How do we prepare the powder pattern?
In Nankai University, more than one thousand new organic compounds are synthesized every year in the study works of professors. They are pharmaceuticals, pesticides, organo-metallic compounds and their intermediate compounds. A part of them are solid state and a few of them can be made to their single crystals. Only the compounds, which can be made to their single crystals, are used to get their single and powder data.
The steps used to prepare our patterns and data:
a. First we used these single crystals to do experiments with single crystal diffractometers to get their cell parameters, space group, three-dimensional structures, and three-dimensional coordinates of atoms.
(Use ENRAF-NONIUS CAD4 and Bruker-AXS-CCD before 1999 and after 2000 respectively)
b. Calculate the theoretical powder pattern of the phase according to its cell parameters, space group, and three-dimensional coordinate.(Program POWDER-12 was used)
c. Do experiments using powder diffractometers and get their powder diffraction patterns (D/Max-3A and D/Max-RC were used before 1997 and after 1998 repectively)
d. Compare the theoretical powder pattern and the experimental powder diffraction pattern to see whether they are well matched or not. If yes, then this data will be adopted and submitted to ICDD, otherwise it will be discarded. Usually we can get about 70-75 high quality powder patterns from 100 single crystal compounds. Because some compounds are not so stable, they change their crystal structures or even react with air and/or moisture.
Therefore, we can submit the cell parameters, space group, three-dimensional coordinates, the digitized data, peaks of the powder pattern, and the structure formula of every compound.
4. What is the data form to be submitted?
For convenience to the treatment of editors, the input form of program PDFEAPC was submitted. However only electronic files were submitted and no paper was needed. Five files should be submitted for every reference data. They are:
a. Lin-2003-01-dat: This is the powder pattern data. The data format is the same as what appears in the PDF database. It is readable by AIDS-83 program.
1 1 0 2 0 2 0 0 70 0 0 0 1 0
16.03434 7.19207 13.29965 110.864 X S T P L03A01M1
.00153 .00075 .00164 .010 L03A01M2
P21/c 14 4 1.525 L03A01M3
O L03A01M5
(4-Chloroanilinium) (3-chloro-4-nitrobenzoate) P 1 L03A01M6
C6 H7 Cl N * C7 H3 Cl N O4 X L03A01M7
00GRNT 2003 Lin, S.-F., Nankai Univ., Tianjin, P.R.China. 1 L03A01M9
0PCOMC 2002 Meng Jiben, Chemistry Department of Nankai PRC2 L03A01M9
University, Tianjin, 300071, China. PR 3 L03A01M9
0PCOMC 2003 Wang H.,State Key Lab.of Nankai Univ.,Tianjin,UCC4 L03A01M9
300071, China. Structure Report No.011103B UC 5 L03A01M9
0PCOMC 2003 Hao Jianmin, Electronic Materials Research PDC6 L03A01M9
Institute, Tianjin, 300192, China. PD 7 L03A01M9
L03A01MA
colorless CL 1 L03A01MB
138-139 MP 2 L03A01MB
CuKa1 1.54059 M Graph 2 D Si I L03A01MF
D P 0.76 0.07 I G L03A01MG
5.890 36 1 0 0 11.800 13 2 0 0 13.320 2 -1 0 2 1 L03A01MI
13.620 9 1 1 0 14.210 7 0 1 1 14.370 4 -1 1 1 2 L03A01MI
14.940 2 -2 0 2 16.810 14 -2 1 1 17.070 10 2 1 0 3 L03A01MI
17.760 2 3 0 0 18.220 5 -1 1 2 18.400 2 -3 0 2 4 L03A01MI
18.860 2 0 1 2 19.390 2 -2 1 2 20.060 2 2 1 1 5 L03A01MI
21.570 4 2 0 2 21.660 4 -3 1 0 22.190 5 -3 1 2 6 L03A01MI
22.890 4 -4 0 2 23.610 17 -1 1 3 23.760 100 4 0 0 7 L03A01MI
24.750 9 0 2 0M 24.750 9 3 1 1M 24.930 6 2 1 2 8 L03A01MI
25.450 2 -4 1 1M 25.450 2 -1 2 0M 25.880 3 -1 2 1 9 L03A01MI
27.040 72 1 2 1 27.310 25 -2 2 1 28.050 7 -5 0 2 10 L03A01MI
28.650 4 0 2 2 28.980 4 -2 2 2 29.820 21 5 0 0 11 L03A01MI
30.700 4 -5 1 1 30.980 2 -3 2 2 32.080 4 -1 2 3 12 L03A01MI
32.430 2 -5 1 3 32.910 2 3 2 1 33.540 4 -6 0 2 13 L03A01MI
33.800 3 1 1 4 35.980 48 -2 1 5 36.970 4 -6 1 3 14 L03A01MI
37.170 4 2 1 4 37.970 2 1 3 0 38.200 2 0 3 1 15 L03A01MI
39.130 2 1 3 1 40.320 1 0 3 2 40.750 2 -3 0 6 16 L03A01MI
40.940 2 2 3 1 42.250 9 -2 2 5 43.060 1 -6 1 5M 17 L03A01MI
43.060 1 -6 2 3M 43.060 1 -2 3 3M 43.780 2 -7 1 4 18 L03A01MI
45.220 2 -5 1 6 45.840 1 4 1 4M 45.840 1 -6 0 6M 19 L03A01MI
46.040 1 -4 3 3 47.080 2 -8 1 2 47.380 2 -3 3 4 20 L03A01MI
47.510 2 -7 2 3 47.860 1 0 3 4 48.650 3 -5 3 3 21 L03A01MI
49.530 1 7 2 0 49.940 3 -4 1 7 51.510 2 -6 3 1 22 L03A01MI
52.240 1 -9 0 4 53.640 1 -8 2 4 53.890 1 -9 1 4M 23 L03A01MI
53.890 1 -6 3 4M 55.240 2 -8 2 0M 55.240 2 -2 4 3M 24 L03A01MI
55.720 2 1 1 7M 55.720 2 -7 2 6M 55.960 2 -2 0 8 25 L03A01MI
56.370 1 -4 4 2M 56.370 1 7 1 3M 56.680 1 9 1 0 26 L03A01MI
57.260 1 4 2 5 57.420 1 -7 3 4 57.960 1 -10 0 4 27 L03A01MI
58.330 1 -2 4 4 58.620 1 -5 3 6M 58.620 1 -9 2 4M 28 L03A01MI
58.960 1 2 1 7M 58.960 1 -5 4 1M 58.960 1 -10 1 3M 29 L03A01MI
58.960 1 -5 4 2M 58.960 1 2 4 3M 59.440 1 -10 1 2M 30 L03A01MI
59.440 1 0 0 8M 60.040 1 -5 4 3 60.490 1 -9 2 5 31 L03A01MI
60.640 1 -6 3 6 61.340 1 -9 2 0 62.020 2 -5 4 4 32 L03A01MI
62.500 1 -3 4 5 62.900 1 -8 3 0 64.040 1 -8 1 8 33 L03A01MI
64.640 1 -6 4 4 34 L03A01MI
L03A01MK
b. Lin-2003-01-pd3: This is the original pattern with the digitized data. The data format is requested by ICDD.
&SAMPLE IDENT= Chloroaniliniumchlorobenz
&ICDD-DX=1.00
&DATE=2003-06-10
&FILE IDENT=Lin-03-A-01.PD3
&SOURCE IDENT=Lin-03-A-01.LIS
&CROSS REFERENCE=2003.REF
&GRANT NO=90-06SFL
&PDFNO=XX-YYYY
&DIV SLIT=0.5
&WAVELENGTH=1.54059
&COUNT TIME=5.000
&STEP SIZE=0.0100
&XUNITS=DEG (2T)
&YUNITS=COUNTS
&YFACTOR=1.0
&FIRSTX= 5.000
&LASTX=65.000
&MAXY= 47089
&NPOINTS=6000
&XYDATA=(X++(Y..Y))
5.000 1040 1037 1036 1047 1064 1087 1097 1109
5.080 1126 1141 1177 1187 1199 1206 1208 1181
5.160 1169 1155 1148 1143 1135 1141 1148 1148
5.240 1148 1155 1165 1173 1182 1193 1225 1248
5.320 1269 1286 1301 1330 1341 1356 1392 1400
------
------
11.000 423 422 420 429 433 438 446 450
11.080 457 466 484 484 484 484 484 483
------
------
20.360 523 513 503 503 503 499 495 495
20.440 495 495 495 499 501 497 495 490
20.520 484 496 501 508 512 511 509 505
------
------
64.760 555 559 561 565 573 569 567 568
64.840 570 571 573 564 552 535 529 524
64.920 512 505 492 489 481 478 471 0
&END
c. Lin-2003-01-xyz: This is the three-dimensional coordinate of the atoms for the compound.
Atoms x y z Ueq Occupancy
------
Cl1 0.07845(6) 0.37184(13) -0.04436(8) 0.0522(3) 1.0
Cl2 0.40463(8) 0.4614(2) 0.36361(11) 0.1051(5) 1.0
O1 0.07621(14) 0.7837(3) -0.16377(18) 0.0461(6) 1.0
O2 0.09194(17) 0.8778(4) 0.0011(2) 0.0669(8) 1.0
O3 0.49354(19) 0.3706(5) 0.1326(3) 0.1193(15) 1.0
O4 0.40736(19) 0.1394(5) 0.1227(3) 0.0837(10) 1.0
N1 0.4208(2) 0.3048(6) 0.1128(3) 0.0676(10) 1.0
N2 0.07870(18) -0.0056(4) 0.1908(2) 0.0403(7) 1.0
C1 0.2813(2) 0.7300(5) 0.0260(3) 0.0518(10) 1.0
C2 0.3553(2) 0.6162(6) 0.0668(3) 0.0550(10) 1.0
C3 0.3422(2) 0.4290(5) 0.0716(3) 0.0468(9) 1.0
C4 0.2582(2) 0.3503(5) 0.0390(2) 0.0422(8) 1.0
C5 0.18545(19) 0.4669(5) -0.0028(2) 0.0347(8) 1.0
C6 0.1948(2) 0.6571(4) -0.0113(2) 0.0357(8) 1.0
C7 0.1143(2) 0.7824(4) -0.0609(3) 0.0388(8) 1.0
C8 0.1508(2) 0.2967(5) 0.2475(3) 0.0436(9) 1.0
C9 0.2272(3) 0.4044(5) 0.2883(3) 0.0572(10) 1.0
C10 0.3097(3) 0.3230(6) 0.3156(3) 0.0590(11) 1.0
C11 0.3178(2) 0.1352(6) 0.3028(3) 0.0571(10) 1.0
C12 0.2415(2) 0.0283(5) 0.2617(3) 0.0453(9) 1.0
C13 0.1590(2) 0.1095(5) 0.2349(2) 0.0343(7) 1.0
------
d. Lin-2003-01-Str: This is the structure formula of the compound.
e. Lin-2003-01-Ref: This is the digitized data of standard material (we use the NIST-SRM-1976 supplied by ICDD)
&SAMPLE IDENT= NIST-SRM-1976
&ICDD-DX=1.00
&DATE=2003-05-10
&FILE IDENT=2003.REF
&SOURCE IDENT=2003-05-NIST-SRM-1976
&GRANT NO=90-06SFL
&GENERATOR TYPE=CP
&ANODE=Cu
&GEN KV=40
&GEN MA=100
&DIFFRACTOMETER=BBR
&DIV SLIT=1.0
&REC SLIT=0.15
&DETECTOR=Scint
&MONOCHROMETER=PG(DB)
&WAVELENGTH=1.54059
&COUNT TIME=2.0-4.0
&STEP SIZE=0.004
&XUNITS=DEG (2T)
&YUNITS=COUNTS/SECOND
&YFACTOR=1.0
&FIRSTX=25.000
&LASTX=137.500
&MAXY= 13968
&NPOINTS=5874
&XYDATA=(X++(Y..Y))
25.000 140 132 137 143 137 141 137 149
25.032 146 146 150 155 152 155 161 158
------
25.608 4539 4456 4364 4241 4080 3922 3660 3481
25.640 3263 3025 2876 2665 2500 2334 2227 2110
25.672 2008 1925 1780 1686 1605 1492 1332 1199
------
35.256 6380 6340 6360 6271 6152 6094 5776 5625
35.288 5302 4979 4531 4112 3653 3228 2698 2377
35.320 1980 1671 1397 1118 949 777 679 603
------
52.448 481 520 532 552 600 653 683 732
52.480 784 837 881 949 1036 1085 1139 1269
52.512 1355 1444 1545 1671 1817 1898 2042 2209
52.544 2352 2488 2646 2809 3004 3136 3342 3466
52.576 3623 3713 3836 3844 3860 3852 3729 3600
52.608 3452 3350 3053 2862 2646 2370 2191 1958
------
95.232 315 326 354 385 423 462 509 541
95.264 576 638 68 746 816 863 896 97373
95.296 1012 1077 1126 1156 1199 1212 1238 1251
95.328 1247 1256 1234 1208 1143 1110 1056 1024
95.360 957 911 848 767 719 647 628 558
------
137.440 46 51 44 54 44 50 45 47
137.472 49 49 52 48 45 48 49 49
&END
Beside the reference patterns, I have done some other works concerning PDF database. They are:
▉ INPUT THE STRUCTURE FORMULA FOR ORGANIC PHASES
Before 1990, the organic phases of PDF Database did not have the structure message, but the structure formula is very important for organic phase. Since 1991 we input the structure formulae for every organic phase. We finished this work in 1994. The total input number was about 15,000. After that we continue to input the new structures every year.
▉ COMPARE THE MERCK DATABASE WITH ICDD PDF
This work is to see how many solid compounds in the Merck database are absent in ICDD PDF. This work was done from 1997 to 2001. About five or six members joined this task group. The leader is Dr. Rendle. I completed 10,713 compounds (the total is 12,839)
▉ ABSTRACT THE CRYSTAL MESSAGE FROM THE ARTICLES ON METAL-ALLOY FIELD
This work was done in cooperation with Professor Jerry Johnson, Dr. Sury, Professor Antipov and me from 2000-2003. We completed 5,000 phases. Professor Antipov has done 7,000 phases.
Thanks to the Chairman to give me the chance to introduce my work. I would do my best to serve to ICDD continually.