-
2004/12/16
-
1
single crystal
twin
1.1 0.96
0.1x0.1x0.1 0.3x0.3x0.3 mm
12 mm
-
2
K
Mo K0.71073 K1 K2
K
X-ray beam
-
3
X-ray diffractionscattering
(h)
2
X
Z
2=0
diffuse scattering
X
X
(Braggs law)
2
(Z)
X
H
C
10
23456789
10
O
1211
131415161718
Cl
Figure 20.
ddsin
A
B
-
4
2dsin
0.71073
2dsin
n=1
n=1,2,3,..
h k l
n=1,2,3,,,
2
sin/
2
2
2dsin = n (n=1,2,3,...) (Bragg's Equation) ()
2
a
b
0
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M M M M M M M M
M M M M M M M M
M
M
M
M
M
M
M
M
M
M
-
5
++++
( 0 1 ) ( 1 1 ) ( 1 2 ) ( 1 3 )
n=1
h k l
x
y
0
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M M M M M M M M
M M M M M M M M
M
M
M
M
M
M
M
M
M
M
a
b
x=a y=b (x=a/1, y=b/1) ( 1 1 )
d
x
y
0
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M M M M M M M M
M M M M M M M M
M
M
M
M
M
M
M
M
M
M
a
b
x=a y=b/2 (x=a/1, y=b/2) ( 1 2 )
y=b/2
d
x
y
0
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M M M M M M M M
M M M M M M M M
M
M
M
M
M
M
M
M
M
M
a
b
y=b ( 01 )
d
x
y
0
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M
M M M M M M M M
M M M M M M M M
M
M
M
M
M
M
M
M
M
M
a
b
x=a y=b/3 (x=a/1, y=b/3) ( 1 3 )
y=b/3
d
-
6
h k l -1
h k l
Structure Factor
Fo observed
Fc I=|Fo|2
h k l Fo Fc
Fo F(h k l)
0 a
c
b
x1a
z1cy1c
(x1, y1, z1)
0 a
b
c
-
7
fjh k l
h k l
TjB11,B22,B33,B12,B23,B13
parameters per
atomXYZBeq; 9 parameters per atom: XYZB11B22B33B12B23B13
XYZUeq, XYZU11U22U33U12U23U13
exponential j h
k l F(h k l)
h k l
XYZU11U22U33U12U23U13
F(h k l) = fjTjexp{2i(hxj+kyj+lzj)}j (1)
B11 B12 B13B12 B22 B23B13 B23 B33
Tj = exp{-(h2B11+k
2B22+l2B33+2klB23+2lhB31+2hkB12))} (2)
()
R1 = (3) (|Fo|-Fc|)
(|Fo|) x 100 (%)
-
8
Reliability Factor, 1
10
(X, Y, Z) (X, Y, Z) F(h k l)
h k l o
-1
(x, y, z) =h k l
(4)V1 F(h k l)exp{-2i(hx+ky+lz)}
O2
O1
Pt
O3
O4
O1*O3*
Pt* O2*O4*
h k l Fo (Fo)XYZU11U22U33U23U13U12
atom X Y Z U11Pt 0.016424 0.994173 0.363648 0.0397O1 0.076123
0.887084 0.344977 0.05416O2 -0.05577 0.895159 0.334312 0.05374O3
0.15537 0.763549 0.543312 0.04975O4 0.172814 0.543615 0.773102
0.09682
U22 U33 U23 U13 U120.03118 0.03894 -0.0034 0.01041
0.001270.04998 0.06374 -0.0056 0.01443 0.010550.04131 0.05051
-0.00948 0.01848 -0.01050.04376 0.04983 -0.00887 0.01744
-0.00990.09404 0.14115 -0.00538 0.04084 0.02225
h k l Fo (Fo)-1 -1 4 810.76 12-1 1 4 820.73 12.4-1 -1 3 135.96
4.05-1 1 3 133.64 4.06-1 -1 2 26.11 1.46-1 1 2 27.41 1.53-1 1 1
2.46 0.411 1 -1 2.3 0.41-1 1 0 797.74 8.97 -15 -13 10 5.69 2.88
-
9
Fo
Fo Fo2(Fo2)
PtO4
1
asymmetric unit(
)
a,b,c,,,
hkl Fo Fo
(Fo) Fo Fo2
(Fo2)
cm-1
Fo
Fo
Fo
-
10
Heavy Atom Method
PtO3N2C6H12 (fw=355)
PtO3N2C6H12V=491 3 d=2.4 g/cm3
Z=2 PtO3N2C6H12
Z=2.4X6.02X1023X491X10-24/355=1.998
(1)x, y, z (2) x, -y, -z
P1- (No.2)
Fo Fourier Synthesis
difference Fourier
synthesis
Fc
Direct Method
1 e/A3
1.0
QTAM (Quantum Theory of Atoms in Molecules)
Oak Ridge
-
11
Johnson
Oak Ridge Thermal Ellipsoid Plot program
Fo Fc scaling factor
Flack Parameter
[]
Shelx97 KenX
Molecular Structure teXsan
Crystan G, SHELXTL
Sheldrick Shelx97
Shelx97
SHELXTL Sheldrick
Shelxl97 Shelxl97
Shelx97
(GUI)
KenX Shelx97 Shelxs97 Shelxl97
s Structure Solution Solution
s l least-squares
refeinment l Shelxh.exe
Shelx97 Sheldrick
KenX HP
Email
-
12
C:
solve.ins solve.hkl( HP )[cntrl]+[C]
[cntrl]+[V]
solve.hkl [cntrl]+[C][cntrl]+[V]
solve.hkl
[F2]test1.hkl
solve.hkl
5005
H3NPtIII
N
H3N N
H3NPtIII
O
H3N O
Cl
Cl(NO3
-)2
Pt Cl O N C H
2+
[Pt(III)2(NH3)4(C4H6NO)2Cl2](NO3)2
1) TITL [Pt2(NH3)4(C4H6NO)2Cl2](NO3)2 in P1- (No.2)2) CELL
0.71073 10.1143 11.9883 8.7891 100.822 95.955 79.6073) ZERR ?
0.0017 0.0025 0.0016 0.015 0.015 0.0144) LATT 15) SFAC C H N O CL
PT6) UNIT ? ? ? ? ? ?7) PATT8) HKLF 49) END
TITLP1
1)
2)CELLa, b, c,, ,
3)ZERR?a, b, c,, ,
LATT 1No.2 -x,-y,-zLATT
4)
SFACScattering FACtor
5)
UNITUNIT_CELLSFAC
6)
PATTPatterson()PATTTREF
7)
Fo2
-
13
5004 h, k, l, Fo2, s(Fo2)
solve.ins
Shelxs.exe
Pt(III)2solve.ins
[File][]
WSXS97.EXE
solve
c:
solve.ORT
Shelxs97
solve.ins
[NO][OK]
solve.res
-
14
[][]
test1.ins .hkl .ins
test1.hkl
[] test1.ins Shelxl97
test1
test1.ins
solve.ins
WSXS97.EXE
(Solution) WSXL97.EXE (Least-Squares)
L.S. 4 BOND FMAP 2 PLAN 20
FoFc
test1.lst
Difference Fourier Synthesis, D
Q1...Q20test1.insQ
PT1 6 0.14312 0.18785 0.35814 11.00000 0.04 ............CL6 5
0.16200 0.12323 0.22763 11.00000 0.04 ......
SFACSFAC
X Y Z sof Ueq
(site occupancy factor)*
*
-
15
jobname test1
Overwrite .INS?[]
test1.ins
Fo>4S(Fo)0.1312
13.12
e/3
[] [] [OK]
text1.ins
KenX KenX
*.ins []
[File][Open_*.ins/*.res/backups]test1.ins
[MovePks]
-
16
[Name][Name]
[Apply]
Mouse_Down_Move
[Rotate][Name]
[Name][Apply]
[Rotate][Delete]
[Apply]
[Delete]
[File][Save_*.ins]
test1.ins
[Ellipse]
[Params][XYZUij+Others]
Normal, aBitLarge, *Large, **tooLarge, ###nonPos!
###nonPos!
Delete Uij
L.S. 4 L.S. 7
KenX KenX [ReOpn]
[SavIns]
KenX [Commands][Edit
Shelxl-97 Commands]test1.ins
[All Aniso][ACTA][CONF]
[All Aniso] ANIS
U11,U22,U33,U23,U13,U12
[ACTA]test1.cif
CifConv.exe
File Open test1.cif File
SaveAsFile test1.sup MS Word
a,b Symbol
-
17
[Renumber]
[Apply]
[cntrl] + X
[Sort Labels][OK]
[Close][SavIns]
Shelxl97
R
[HFIX]HFIX Coding
Rules
Shelxl97
OK
C N sp2
CH sp3 CH2 riding
model [Name][Delete]
[Apply]NH3 m=13/n=7
[HFIX][Apply]HFIX
[cntrl] + E HFIX
[SavIns]Shelxl97
Shelxl97 KenX
C28 HFIX
43 1.2 C28
Shelxl97 -1.2
C28 Ueq 1.2
-1.5
KenX [SavIns]
KenX
L.S. 7 x 3 sets
KenX [SavIns]
Mean
Shift/esd 0.0000 Maximum Shift/esd 0.0000
-
18
Shift/esd
Shift/esd
ORTEOP32.exe
[File][Open File]test1.ins
ORTEP
[Labels][Set Mouse Labels][OK]
[Cancel]
[Cancel]
EPS Encapsulated Postscript File[File]
[Write Postscript File][Colour][Monochrome]
ORTEP001.EPS, ORTEP002.EPS
Print mswinprint2
[OK]
value
V
0
1
2
3
4
5
6
7
8
9
10
11
12
13
14
ValueShiftShift/esd
Shift/esdvalue
esd
-
19
PLATON
Cl-Pt-Pt-Cl
PWT.EXE
PLATON PLATON for Windows Taskbar [File][Select
Data File]test1.ins
Platon Graphical Menu
Platon Graphics Contour-Fo
Fo Fourier
Contour ORTEP
Cl1, Pt1, Pt2
Working
Contour_Menu Ch_Cntr_Lev
Up Down
-
20
[Cntrl]+[PrintScreen][][][
][][Cntrl]+[V] BMP
[][
][]
[File][]
Word Word
KenX Stereo
[ReExp]
P1- No. 2
2P1-
KenX [ShowCell],
[LabAxes][ShowPks][Packing]
KenX [File][Save Graphics]Black and White
[OK]
[Stereo] Scl
Save Graphics
ACTA test1.cifCifConV.exeKenX
Word
-
21
Table 1. Crystallographic Data of
[Pt(III)2(NH3)4(C4H6NO)2Cl2](NO3)2
_________________________________________________________________
formula ?
fw ?
crystal system ?
space group ?
a, ?
b, ?
c, ?
, deg ?
, deg ?
, deg ?
V, 3 ?
Z ?
dcalc, g/cm3 ?
(Mo K), mm-1 ?
radiation, ?
data/restraints/params ?/?/?
R1 ?
max/min diff. peaks ?/?
Table 2. Atomic Coordinates and Equivalent Isotropic Thermal
Parameters
for [Pt(III)2(NH3)4(C4H6NO)2Cl2](NO3)2
__________________________________________________________________
atom X Y Z Ueq
__________________________________________________________________
Pt1 0.18538(4) ? ? ?
Pt2 ? ? ? 0.02952(13)
?
?
?
-
22
Table 3. Selected Interatomic Distances () and Angles (deg)
[Pt(III)2(NH3)4(C4H6NO)2Cl2](NO3)2
______________________________________________________________________
Pt1-N10 2.158(10) Pt1-N9 ?
Pt1-N5 ? Pt1-N6 ?
Pt1-Cl3 ? Pt1-Pt2 ?
Pt2-O12 ? Pt2-N3 ?
Pt2-N4 ? Pt2-O11 ?
Pt2-Cl4 ? N10-Pt1-N9 ?
N10-Pt1-N5 ? N9-Pt1-N5 ?
N10-Pt1-N6 ? N9-Pt1-N6 ?
N5-Pt1-N6 ? N10-Pt1-Cl3 ?
N9-Pt1-Cl3 ? N5-Pt1-Cl3 ?
N6-Pt1-Cl3 ? O12-Pt2-N3 ?
O12-Pt2-N4 ? N3-Pt2-N4 ?
O12-Pt2-O11 ? N3-Pt2-O11 ?
N4-Pt2-O11 ? O12-Pt2-Cl4 ?
N3-Pt2-Cl4 ? N4-Pt2-Cl4 ?
O11-Pt2-Cl4 ? O12-Pt2-Pt1 ?
CIF [International Union of Crystallography (IUCr);
http://www.iucr.org/ http://www.iucr.ac.uk/]
Acta Crystallographica X Check CIF CIF IUCr ()
http://journals.iucr.org/services/cif/checking/checkform.html
CIF CIF CIF Alert Alert CIF
-
23
Alert CIF
time consuming Alert A CIF Alert A CIF Alert A ()
IUCr X
812-8581 6-10-1
Fax: 092-642-2596 E-mail: [email protected]
