Subject: crystal structure,special positions

From: [email-masked]
Date: Thu, 20 Aug 1998 17:05:30 +0000

Hi ccl'ers,
I am relatively new in the world of crystallography.  I have recently 
solved a structure of calix(4)arene in the hexagonal space group 
p63/m, with an Rfactor down to 5.83%.  The problem is that as yet I 
have not identified the solvent, initially I thought that it was 
acetonitrile, as I had three peaks, however the bond lengths vary are 
shorter than even a CN triple bond.  The atoms lie on special 
positions, but I am confused as to how to tackle this.
Any help would be much appreciated.
I have attached an output file from a shelxl refinement.

TITL AL HYDROXY-CALIX-4-ARENE COMPLEX 27.7.98
CELL 0.71073  14.4788 14.4673 18.8024 89.8904 90.0331 119.9812
ZERR  6 .0013 .0041 .0121 0.361 0.02 0.0105
LATT 1
SYMM -Y, X-Y, Z
SYMM Y-X, -X, Z
SYMM -X, -Y, 0.5+Z
SYMM Y, Y-X, 0.5+Z
SYMM X-Y, X, 0.5+Z
SFAC C H O N
UNIT 168 144 24 0
L.S. 6
WGHT    0.078400    0.769600
EXTI    0.006795
FVAR       0.74488
O01     3  -0.00286   0.26856   0.15779  11.00000   0.05881   0.08170 =
        0.11258  -0.02072  -0.00765   0.03695
AFIX 143
H01     2   0.01965   0.32827   0.17463  11.00000  -1.50000
AFIX   0
C11     1  -0.07980   0.24927   0.10816  11.00000   0.05241   0.07996 =
        0.07552  -0.01632   0.01274   0.03315
C21     1  -0.09135   0.33352   0.08292  11.00000   0.05882   0.08038 =
        0.06184  -0.00233   0.01863   0.03284
C31     1  -0.16422   0.31155   0.02869  11.00000   0.07949   0.11218 =
        0.06112  -0.00448   0.00995   0.04587
AFIX  43
H31     2  -0.17313   0.36645   0.01058  11.00000  -1.20000
AFIX   0
C41     1  -0.22368   0.21068   0.00097  11.00000   0.09397   0.13605 =
        0.06702  -0.03410  -0.00713   0.04999
AFIX  43
H41     2  -0.27104   0.19797  -0.03614  11.00000  -1.20000
AFIX   0
C51     1  -0.21255   0.12884   0.02856  11.00000   0.08298   0.10804 =
        0.09646  -0.04985   0.00213   0.03862
AFIX  43
H51     2  -0.25378   0.06043   0.01024  11.00000  -1.20000
AFIX   0
C61     1  -0.14183   0.14565   0.08266  11.00000   0.06717   0.08412 =
        0.09980  -0.03518   0.01101   0.03945
C10     1  -0.13471   0.05266   0.11509  11.00000   0.07654   0.08115 =
        0.16269  -0.05289  -0.00016   0.04552
AFIX  23
H10A    2  -0.16442  -0.00643   0.08184  11.00000  -1.20000
H10B    2  -0.06026   0.07426   0.12220  11.00000  -1.20000
AFIX   0
O02     3  -0.03105   0.11806   0.25000  10.50000   0.05038   0.07552 =
        0.17967   0.00000   0.00000   0.03866
AFIX 143
H02     2  -0.01472   0.16060   0.21702  10.50000  -1.50000
AFIX   0
C12     1  -0.14028   0.04975   0.25000  10.50000   0.05136   0.05157 =
        0.16323   0.00000   0.00000   0.03611
C22     1  -0.19264   0.01518   0.18508  11.00000   0.06211   0.05206 =
        0.16098  -0.01797  -0.00067   0.03740
C32     1  -0.30215  -0.05649   0.18699  11.00000   0.07067   0.05457 =
        0.17493  -0.02320  -0.01040   0.03302
AFIX  43
H32     2  -0.33926  -0.08115   0.14444  11.00000  -1.20000
AFIX   0
C42     1  -0.35639  -0.09144   0.25000  10.50000   0.06350   0.05209 =
        0.20408   0.00000   0.00000   0.02510
AFIX  43
H42     2  -0.42954  -0.13858   0.25003  10.50000  -1.20000
AFIX   0
C20     1  -0.02780   0.44392   0.38553  11.00000   0.06170   0.06964 =
        0.06784  -0.01210  -0.01769   0.02654
AFIX  23
H20A    2   0.04529   0.46032   0.37888  11.00000  -1.20000
H20B    2  -0.02712   0.49522   0.41898  11.00000  -1.20000
AFIX   0
O04     3   0.05577   0.42890   0.25000  10.50000   0.04268   0.06751 =
        0.09729   0.00000   0.00000   0.02462
AFIX 143
H04     2   0.05342   0.39534   0.28580  10.50000  -1.50000
AFIX   0
C14     1  -0.03006   0.44687   0.25000  10.50000   0.03651   0.03895 =
        0.07141   0.00000   0.00000   0.01320
C24     1  -0.07096   0.45666   0.31491  11.00000   0.04805   0.04320 =
        0.06297  -0.00545  -0.00617   0.01681
C34     1  -0.15390   0.47827   0.31312  11.00000   0.06052   0.05100 =
        0.06705  -0.00777   0.00109   0.02710
AFIX  43
H34     2  -0.18233   0.48555   0.35567  11.00000  -1.20000
AFIX   0
C44     1  -0.19514   0.48920   0.25000  10.50000   0.05796   0.05473 =
        0.08090   0.00000   0.00000   0.03435
AFIX  43
H44     2  -0.25073   0.50394   0.24996  10.50000  -1.20000
AFIX   0
N1      1   0.33333   0.66667   0.25000  10.16667   0.20274   0.20274 =
        0.01890   0.00000   0.00000   0.10137
N2      1   0.33333   0.66667   0.30440  10.33333   0.16585   0.16585 =
        0.16177   0.00000   0.00000   0.08293
C4      1   0.40062   0.72871   0.34977  11.00000   0.44802   0.44705 =
        0.46619  -0.23905  -0.16872   0.23859
FMAP 2
PLAN -20
HKLF 4
END  
     
WGHT      0.0743      0.8687 
Q1    1  -0.6166 -0.2866  0.2500  10.50000  0.05    0.26
Q2    1  -0.0195  0.1900  0.1914  11.00000  0.05    0.25
Q3    1  -0.6039 -0.3039  0.3725  11.00000  0.05    0.20
Q4    1  -0.4980 -0.2480  0.2500  10.50000  0.05    0.18
Q5    1  -0.3333  0.3333  0.2500  10.16667  0.05    0.17
Q6    1  -0.0400  0.0622  0.1605  11.00000  0.05    0.17
Q7    1  -0.5625 -0.3125  0.3047  11.00000  0.05    0.16
Q8    1  -0.0400  0.0786  0.2934  11.00000  0.05    0.16
Q9    1  -0.4602 -0.5100  0.3466  11.00000  0.05    0.15
Q10   1  -0.2400  0.3461  0.2500  10.50000  0.05    0.15
Q11   1  -0.5355 -0.1955  0.3917  11.00000  0.05    0.14
Q12   1  -0.6400 -0.2274  0.3175  11.00000  0.05    0.14
Q13   1  -0.4520 -0.4220  0.3207  11.00000  0.05    0.14
Q14   1  -0.2600  0.2430 -0.0509  11.00000  0.05    0.14
Q15   1  -0.4619 -0.3619  0.2996  11.00000  0.05    0.14
Q16   1  -0.2300  0.0665  0.2500  10.50000  0.05    0.14
Q17   1  -0.1965  0.3400  0.1119  11.00000  0.05    0.13
Q18   1   0.0300  0.0113  0.5268  11.00000  0.05    0.13
Q19   1   0.0129  0.3929  0.1989  11.00000  0.05    0.13
Q20   1  -0.2700  0.4458  0.2975  11.00000  0.05    0.12