+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
+ SHELXL - CRYSTAL STRUCTURE REFINEMENT - MULTI-CPU VERSION +
+ Copyright(C) George M. Sheldrick 1993-2017 Version 2017/1 +
+ xray072 started at 11:14:50 on 01-Jun-2021 +
+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
Command line parameters: xray072 -a50000 -b3000 -c624 -g0 -m0 -t4
-a sets the approximate maximum number of atoms including hydrogens.
-b sets the maximum number of full-matrix parameters (not used by CGLS).
For example -b9000 allows refinement of 1000 anisotropic atoms or 3000
with BLOC 1. For a 32-bit version, -b times the square root of the
number of threads should not exceed about 65500. -c sets the reflection
buffer size. This depends on the CPU cache size but will rarely
need changing.
-g sets the number of reflection groups used for calculating R_complete,
This must be greater than 1 but not greater than the total number of
reflections for refinement. -m sets the current reflection group number.
This may not be less than 1 nor greater than the number set by -g. These
command line flags override other ways of defining free-R reflections.
The -m value is also used as a seed for the WIGL pseudo-random shifts.
-t sets the number of threads, otherwise it is set to the apparent
number of CPUs. For optimal performance on hyperthreading systems,
-t should be set to a little more than half the number of CPUs;
e.g. -t4 or -t5 for an Intel i7 processor.
Running 4 threads on 4 processors
TITL xray072_a.res in P2(1)/m
REM Old TITL
REM SHELXT solution in P2(1)/m
REM R1 0.232, Rweak 0.011, Alpha 0.022, Orientation as input
REM Formula found by SHELXT: C9 I
CELL 1.54178 8.0879 7.0547 8.2312 90 103.02 90
ZERR 2 0.0006 0.0005 0.0006 0 0.002 0
LATT 1
SYMM -X,0.5+Y,-Z
SFAC C H I
UNIT 18 22 2
V = 457.58 F(000) = 236.0 Mu = 26.89 mm-1 Cell Wt = 492.15 Rho = 1.786
L.S. 20
PLAN 20
SIZE 0.103 0.186 0.241
TEMP -73.15
CONF
BOND $H
list 4
MORE -1
fmap 2
acta
OMIT 1 0 0
OMIT 1 0 1
OMIT -1 0 2
OMIT 1 1 3
OMIT 0 3 2
OMIT 2 0 2
OMIT 2 1 0
OMIT -2 0 2
OMIT 3 0 0
WGHT 0.1078 0.5447
FVAR 0.59204
REM
REM
REM
PART 1
I1 3 0.35353 0.25000 0.14389 10.50000 0.05055 0.03961 0.04504 =
0.00000 -0.02340 -0.00000
C1 1 0.52942 0.25000 0.51231 10.50000 0.02383 0.02343 0.03456 =
0.00000 0.00652 -0.00000
C2 1 0.66876 0.25000 0.64600 10.50000 0.02756 0.02702 0.02706 =
0.00000 0.00904 -0.00000
AFIX 43
H2 2 0.65084 0.25000 0.75616 10.50000 -1.20000
AFIX 0
C3 1 0.83539 0.25000 0.62315 10.50000 0.01354 0.03699 0.02337 =
0.00000 -0.00927 -0.00000
C4 1 0.85909 0.25000 0.46175 10.50000 0.02135 0.02983 0.03269 =
0.00000 0.00802 -0.00000
AFIX 43
H4 2 0.97166 0.25000 0.44536 10.50000 -1.20000
AFIX 0
C5 1 0.72588 0.25000 0.32410 10.50000 0.03972 0.02602 0.02840 =
0.00000 0.01210 0.00000
C6 1 0.56003 0.25000 0.34925 10.50000 0.02865 0.02459 0.02657 =
0.00000 -0.00335 -0.00000
C7 1 0.35455 0.25000 0.54479 10.50000 0.02675 0.03635 0.06138 =
0.00000 0.01479 -0.00000
AFIX 33
H7a 2 0.27051 0.25000 0.43843 10.50000 -1.50000
H7c 2 0.33935 0.13658 0.60861 10.50000 -1.50000
H7b 2 0.33935 0.36342 0.60861 10.50000 -1.50000
AFIX 0
C8 1 0.98023 0.25000 0.77192 10.50000 0.02692 0.07240 0.04218 =
0.00000 -0.00987 -0.00000
AFIX 33
H8a 2 0.93645 0.25000 0.87366 10.50000 -1.50000
H8b 2 1.04970 0.13658 0.76991 10.50000 -1.50000
H8c 2 1.04970 0.36342 0.76991 10.50000 -1.50000
AFIX 0
C9 1 0.76148 0.25000 0.15172 10.50000 0.06759 0.05246 0.03567 =
0.00000 0.02529 -0.00000
AFIX 33
H9a 2 0.65397 0.25000 0.06807 10.50000 -1.50000
H9b 2 0.82679 0.36342 0.13761 10.50000 -1.50000
H9c 2 0.82679 0.13658 0.13761 10.50000 -1.50000
AFIX 0
HKLF 4
Covalent radii and connectivity table for xray072_a.res in P2(1)/m
C 0.770
H 0.320
I 1.330
I1^a - C6^a
C1^a - C2^a C6^a C7^a
C2^a - C1^a C3^a
C3^a - C4^a C2^a C8^a
C4^a - C5^a C3^a
C5^a - C4^a C6^a C9^a
C6^a - C5^a C1^a I1^a
C7^a - C1^a
C8^a - C3^a
C9^a - C5^a
Operators for generating equivalent atoms:
$1 x, -y+1/2, z
h k l Fo^2 Sigma Why rejected (first 50 of each listed)
0 1 0 2.20 0.20 systematically absent but >3sig(I)
0 3 0 4.50 0.40 systematically absent but >3sig(I)
0 5 0 1.80 0.30 systematically absent but >3sig(I)
0 5 0 1.40 0.30 systematically absent but >3sig(I)
0 7 0 1.70 0.30 systematically absent but >3sig(I)
0 7 0 1.20 0.30 systematically absent but >3sig(I)
6 Systematically absent reflections rejected
4983 Reflections read, of which 27 rejected
-9 =< h =< 9, -8 =< k =< 8, -8 =< l =< 10, Max. 2-theta = 144.13
6 Systematic absence violations (I>3sig(I)) before merging
0 Inconsistent equivalents
953 Unique reflections, of which 0 suppressed
R(int) = 0.0599 R(sigma) = 0.0502 Friedel opposites merged
Maximum memory for data reduction = 1518 / 9362
Number of data for d > 0.810A (CIF: max) and d > 0.833A (CIF: full)
(ignoring systematic absences):
Unique reflections found (point group) 953 882
Unique reflections possible (point group) 978 900
Unique reflections found (Laue group) 953 882
Unique reflections possible (Laue group) 978 900
Special position constraints for I1^a
y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000
Input constraints retained (at least in part) for sof
Special position constraints for C1^a
y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000
Input constraints retained (at least in part) for sof
Special position constraints for C2^a
y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000
Input constraints retained (at least in part) for sof
Special position constraints for C3^a
y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000
Input constraints retained (at least in part) for sof
Special position constraints for C4^a
y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000
Input constraints retained (at least in part) for sof
Special position constraints for C5^a
y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000
Input constraints retained (at least in part) for sof
Special position constraints for C6^a
y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000
Input constraints retained (at least in part) for sof
Special position constraints for C7^a
y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000
Input constraints retained (at least in part) for sof
Special position constraints for C8^a
y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000
Input constraints retained (at least in part) for sof
Special position constraints for C9^a
y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000
Input constraints retained (at least in part) for sof
Default effective X-H and X-D distances for T = -73.2C
AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16
d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95
Note that these distances are chosen to give the best fit to the X-ray data
and so avoid the introduction of systematic error. The true internuclear
distances are longer and do not vary with temperature! The apparent
variation with temperature is caused by libration.
Least-squares cycle 1 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 1 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59196 0.00358 -0.022 OSF
Mean shift/esd = 0.007 Maximum = -0.041 for U11 I1^a
Max. shift = 0.000 A for C3^a Max. dU = 0.000 for C8^a
Least-squares cycle 2 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 2 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 -0.010 OSF
Mean shift/esd = 0.003 Maximum = -0.013 for U11 I1^a
Max. shift = 0.000 A for C8^a Max. dU = 0.000 for C8^a
Least-squares cycle 3 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 3 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.001 for x C8^a
Max. shift = 0.000 A for H8B^a Max. dU = 0.000 for C3^a
Least-squares cycle 4 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 4 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C8^a Max. dU = 0.000 for C1^a
Least-squares cycle 5 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 5 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C8^a Max. dU = 0.000 for C7^a
Least-squares cycle 6 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 6 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C7^a Max. dU = 0.000 for C7^a
Least-squares cycle 7 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 7 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C7^a Max. dU = 0.000 for C8^a
Least-squares cycle 8 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 8 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C7^a Max. dU = 0.000 for C8^a
Least-squares cycle 9 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 9 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C7^a Max. dU = 0.000 for C8^a
Least-squares cycle 10 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 10 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C5^a Max. dU = 0.000 for C7^a
Least-squares cycle 11 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 11 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C4^a Max. dU = 0.000 for C7^a
Least-squares cycle 12 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 12 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C7^a Max. dU = 0.000 for C7^a
Least-squares cycle 13 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 13 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C7^a Max. dU = 0.000 for C7^a
Least-squares cycle 14 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 14 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C7^a Max. dU = 0.000 for C7^a
Least-squares cycle 15 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 15 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C4^a Max. dU = 0.000 for C7^a
Least-squares cycle 16 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 16 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C7^a Max. dU = 0.000 for C7^a
Least-squares cycle 17 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 17 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C4^a Max. dU = 0.000 for C7^a
Least-squares cycle 18 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 18 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C8^a Max. dU = 0.000 for C7^a
Least-squares cycle 19 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 19 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for C7^a Max. dU = 0.000 for C7^a
Least-squares cycle 20 Maximum vector length = 623 Memory required = 31 / 1738 / 104808
wR2 = 0.1481 before cycle 20 for 953 data and 61 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.59193 0.00358 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x I1^a
Max. shift = 0.000 A for H8B^a Max. dU = 0.000 for C7^a
Largest correlation matrix elements
0.682 U33 I1^a / OSF 0.590 U13 C4^a / U11 C4^a 0.509 U13 C5^a / U33 C5^a
0.672 U13 C9^a / U11 C9^a 0.559 U13 C5^a / U11 C5^a 0.508 z C5^a / x C5^a
0.670 U11 I1^a / OSF 0.547 U13 C7^a / U33 C7^a 0.505 U13 C2^a / U33 C2^a
0.649 U22 I1^a / OSF 0.542 U13 C4^a / U33 C4^a 0.502 U13 C2^a / U11 C2^a
0.618 z C9^a / x C9^a 0.533 U13 C7^a / U11 C7^a
0.612 U13 C9^a / U33 C9^a 0.514 z C7^a / x C7^a
Idealized hydrogen atom generation before cycle 21
Name x y z AFIX d(X-H) shift Bonded to Conformation determined by
H2 0.6508 0.2500 0.7562 43 0.950 0.000 C2^a C1^a C3^a
H4 0.9717 0.2500 0.4454 43 0.950 0.000 C4^a C5^a C3^a
H7A 0.2705 0.2500 0.4384 33 0.980 0.000 C7^a C1^a C2^a
H7C 0.3393 0.1366 0.6086 33 0.980 0.000 C7^a C1^a C2^a
H7B 0.3393 0.3634 0.6086 33 0.980 0.000 C7^a C1^a C2^a
H8A 0.9365 0.2500 0.8737 33 0.980 0.000 C8^a C3^a C4^a
H8B 1.0497 0.1366 0.7699 33 0.980 0.000 C8^a C3^a C4^a
H8C 1.0497 0.3634 0.7699 33 0.980 0.000 C8^a C3^a C4^a
H9A 0.6540 0.2500 0.0681 33 0.980 0.000 C9^a C5^a C4^a
H9B 0.8268 0.3634 0.1376 33 0.980 0.000 C9^a C5^a C4^a
H9C 0.8268 0.1366 0.1376 33 0.980 0.000 C9^a C5^a C4^a
xray072_a.res in P2(1)/m
ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq
I1^a 0.35353 0.25000 0.14389 0.50000 0.05053 0.03960 0.04503 0.00000 -0.02340 0.00000 0.05046
0.00061 0.00006 0.00000 0.00005 0.00000 0.00046 0.00044 0.00046 0.00000 0.00029 0.00000 0.00034
C1^a 0.52942 0.25000 0.51230 0.50000 0.02381 0.02340 0.03458 0.00000 0.00651 0.00000 0.02727
0.01133 0.00076 0.00000 0.00085 0.00000 0.00278 0.00272 0.00328 0.00000 0.00242 0.00000 0.00125
C2^a 0.66877 0.25000 0.64600 0.50000 0.02753 0.02700 0.02705 0.00000 0.00902 0.00000 0.02674
0.01043 0.00074 0.00000 0.00074 0.00000 0.00263 0.00281 0.00257 0.00000 0.00220 0.00000 0.00113
H2^a 0.65084 0.25000 0.75617 0.50000 0.03209
0.00000 0.00000
C3^a 0.83538 0.25000 0.62316 0.50000 0.01351 0.03704 0.02338 0.00000 -0.00926 0.00000 0.02677
0.01003 0.00069 0.00000 0.00077 0.00000 0.00233 0.00367 0.00254 0.00000 0.00198 0.00000 0.00128
C4^a 0.85909 0.25000 0.46176 0.50000 0.02130 0.02985 0.03267 0.00000 0.00799 0.00000 0.02764
0.00991 0.00067 0.00000 0.00075 0.00000 0.00255 0.00289 0.00312 0.00000 0.00243 0.00000 0.00123
H4^a 0.97166 0.25000 0.44537 0.50000 0.03317
0.00000 0.00000
C5^a 0.72587 0.25000 0.32409 0.50000 0.03972 0.02599 0.02835 0.00000 0.01207 0.00000 0.03066
0.01246 0.00090 0.00000 0.00086 0.00000 0.00353 0.00306 0.00310 0.00000 0.00269 0.00000 0.00140
C6^a 0.56003 0.25000 0.34925 0.50000 0.02866 0.02453 0.02661 0.00000 -0.00335 0.00000 0.02812
0.01096 0.00081 0.00000 0.00083 0.00000 0.00314 0.00292 0.00295 0.00000 0.00233 0.00000 0.00126
C7^a 0.35455 0.25000 0.54478 0.50000 0.02670 0.03634 0.06138 0.00000 0.01477 0.00000 0.04071
0.01358 0.00083 0.00000 0.00107 0.00000 0.00308 0.00347 0.00446 0.00000 0.00312 0.00000 0.00162
H7A^a 0.27051 0.25000 0.43842 0.50000 0.06107
0.00000 0.00000
H7C^a 0.33935 0.13658 0.60860 0.50000 0.06107
0.00000 0.00000
H7B^a 0.33935 0.36342 0.60860 0.50000 0.06107
0.00000 0.00000
C8^a 0.98024 0.25000 0.77192 0.50000 0.02687 0.07236 0.04220 0.00000 -0.00988 0.00000 0.04994
0.01203 0.00090 0.00000 0.00099 0.00000 0.00313 0.00556 0.00392 0.00000 0.00295 0.00000 0.00186
H8A^a 0.93647 0.25000 0.87367 0.50000 0.07491
0.00000 0.00000
H8B^a 1.04971 0.13658 0.76990 0.50000 0.07491
0.00000 0.00000
H8C^a 1.04971 0.36342 0.76991 0.50000 0.07491
0.00000 0.00000
C9^a 0.76147 0.25000 0.15171 0.50000 0.06759 0.05244 0.03564 0.00000 0.02527 0.00000 0.04973
0.01760 0.00132 0.00000 0.00107 0.00000 0.00503 0.00472 0.00400 0.00000 0.00393 0.00000 0.00211
H9A^a 0.65396 0.25000 0.06806 0.50000 0.07460
0.00000 0.00000
H9B^a 0.82678 0.36342 0.13760 0.50000 0.07460
0.00000 0.00000
H9C^a 0.82678 0.13658 0.13760 0.50000 0.07460
0.00000 0.00000
Final Structure Factor Calculation for xray072_a.res in P2(1)/m
Total number of l.s. parameters = 61 Maximum vector length = 623 Memory required = 31 / 1677 / 26790
wR2 = 0.1481 before cycle 21 for 953 data and 0 / 61 parameters
GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.1078 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
wR2 = 0.1481, GooF = S = 1.123, Restrained GooF = 1.123 for all data
R1 = 0.0544 for 953 Fo > 4sig(Fo) and 0.0544 for all 953 data
Occupancy sum of asymmetric unit = 5.00 for non-hydrogen and 5.50 for H and D atoms
Principal mean square atomic displacements U
0.0920 0.0396 0.0198 I1^a
0.0347 0.0237 0.0234 C1^a
0.0296 0.0270 0.0236 C2^a
0.0370 0.0366 0.0066 C3^a
0.0327 0.0298 0.0204 C4^a
0.0404 0.0260 0.0255 C5^a
0.0400 0.0245 0.0198 C6^a
0.0614 0.0363 0.0244 C7^a
0.0724 0.0589 0.0185 C8^a
0.0702 0.0524 0.0266 C9^a
0 atoms may be split and 0 atoms NPD
Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group
Fc/Fc(max) 0.000 0.019 0.034 0.052 0.070 0.087 0.110 0.139 0.174 0.228 1.000
Number in group 105. 89. 95. 97. 92. 96. 93. 97. 93. 96.
GooF 1.345 1.143 0.924 0.934 1.014 1.113 1.004 0.973 1.305 1.337
K 1.243 1.003 0.980 1.025 1.016 1.049 1.027 1.028 1.001 0.941
Resolution(A) 0.81 0.84 0.88 0.91 0.97 1.02 1.11 1.21 1.38 1.72 inf
Number in group 98. 93. 97. 93. 97. 95. 94. 96. 94. 96.
GooF 0.871 1.036 0.904 0.937 0.833 0.943 0.908 1.279 1.423 1.738
K 0.969 0.973 1.014 1.022 0.987 1.024 1.012 1.057 0.974 0.929
R1 0.053 0.063 0.056 0.046 0.044 0.047 0.038 0.054 0.057 0.068
Recommended weighting scheme: WGHT 0.1077 0.5440
Most Disagreeable Reflections (* if suppressed or used for Rfree).
Error/esd is calculated as sqrt(wD^2/) where w is given by the weight
formula, D = Fo^2-Fc^2 and <> refers to the average over all reflections.
h k l Fo^2 Fc^2 Error/esd Fc/Fc(max) Resolution(A)
1 3 1 33.71 4.79 6.50 0.013 2.13
2 0 0 481.51 940.91 4.70 0.180 3.94
1 5 1 19.91 6.37 4.30 0.015 1.36
0 2 2 385.45 228.71 4.15 0.089 2.65
3 0 1 746.55 440.57 3.72 0.123 2.34
-1 0 1 523.38 899.64 3.64 0.176 6.39
5 4 4 83.09 151.55 3.56 0.072 0.95
3 1 3 39.46 19.94 3.54 0.026 1.65
0 4 2 156.42 95.52 3.45 0.057 1.61
9 1 1 138.80 233.63 3.30 0.090 0.84
1 2 2 1626.22 2527.85 3.01 0.295 2.40
-3 4 2 8.52 19.00 2.86 0.026 1.43
-2 2 1 2760.18 4035.62 2.79 0.373 2.62
4 1 2 2068.33 2956.74 2.69 0.319 1.59
1 4 2 1660.89 1190.80 2.68 0.202 1.55
-6 0 2 379.63 270.00 2.66 0.096 1.34
4 0 3 706.17 1009.86 2.65 0.186 1.44
0 0 5 181.66 128.34 2.59 0.066 1.60
4 2 0 1398.48 2053.04 2.59 0.266 1.72
4 3 4 4.42 1.05 2.59 0.006 1.12
5 1 1 1078.71 786.16 2.57 0.164 1.45
-3 3 2 1975.95 2859.51 2.55 0.314 1.70
7 0 2 15.13 7.09 2.54 0.016 1.03
1 2 0 2362.08 3379.43 2.48 0.341 3.22
8 1 1 7.00 2.59 2.48 0.009 0.94
2 0 4 20.33 11.65 2.41 0.020 1.64
2 1 1 3418.54 4834.72 2.40 0.408 2.96
1 4 0 2350.09 1635.49 2.39 0.237 1.72
1 0 2 2622.06 3690.88 2.37 0.356 3.29
-5 0 7 27.64 17.06 2.29 0.024 1.05
-1 4 4 124.53 90.31 2.28 0.056 1.34
-9 2 1 91.36 129.20 2.27 0.067 0.87
6 2 3 1408.22 1069.76 2.27 0.192 1.04
-5 0 4 12.81 6.76 2.27 0.015 1.40
0 4 8 101.31 143.30 2.24 0.070 0.87
7 1 2 1600.85 1223.17 2.24 0.205 1.01
6 0 1 318.29 238.28 2.23 0.091 1.25
3 4 7 370.48 502.92 2.23 0.132 0.85
-1 1 6 7.07 3.14 2.17 0.010 1.34
-6 1 4 16.36 9.56 2.16 0.018 1.21
4 1 1 802.63 612.75 2.15 0.145 1.76
0 3 4 465.19 355.30 2.14 0.111 1.53
-3 2 1 2761.71 4109.85 2.13 0.376 2.13
-5 6 5 295.82 393.06 2.08 0.116 0.87
-5 1 2 27.47 18.01 2.08 0.025 1.55
-3 2 2 26.15 39.08 2.05 0.037 2.02
-1 2 2 2208.83 2911.91 2.05 0.316 2.63
-6 5 1 13.38 7.65 2.05 0.016 0.97
5 2 2 1449.35 1127.11 2.02 0.197 1.27
6 1 1 455.07 354.50 2.00 0.110 1.23
Bond lengths and angles
I1^a - Distance Angles
C6^a 2.0916 (0.0069)
I1^a
C1^a - Distance Angles
C2^a 1.3866 (0.0095)
C6^a 1.4185 (0.0090) 117.84 (0.51)
C7^a 1.4974 (0.0070) 119.33 (0.58) 122.83 (0.64)
C1^a C2^a C6^a
C2^a - Distance Angles
C1^a 1.3866 (0.0095)
C3^a 1.4019 (0.0068) 121.84 (0.51)
H2^a 0.9500 119.08 119.08
C2^a C1^a C3^a
C3^a - Distance Angles
C4^a 1.3844 (0.0081)
C2^a 1.4019 (0.0068) 118.28 (0.54)
C8^a 1.4918 (0.0097) 122.32 (0.50) 119.39 (0.54)
C3^a C4^a C2^a
C4^a - Distance Angles
C5^a 1.3765 (0.0101)
C3^a 1.3844 (0.0081) 122.55 (0.48)
H4^a 0.9500 118.73 118.73
C4^a C5^a C3^a
C5^a - Distance Angles
C4^a 1.3765 (0.0101)
C6^a 1.4025 (0.0098) 118.41 (0.57)
C9^a 1.5101 (0.0082) 119.60 (0.64) 122.00 (0.74)
C5^a C4^a C6^a
C6^a - Distance Angles
C5^a 1.4025 (0.0098)
C1^a 1.4185 (0.0090) 121.08 (0.66)
I1^a 2.0916 (0.0069) 119.79 (0.50) 119.13 (0.46)
C6^a C5^a C1^a
C7^a - Distance Angles
C1^a 1.4974 (0.0070)
H7A^a 0.9800 109.47
H7C^a 0.9800 109.47 109.47
H7B^a 0.9800 109.47 109.47 109.47
C7^a C1^a H7A^a H7C^a
C8^a - Distance Angles
C3^a 1.4918 (0.0097)
H8A^a 0.9800 109.47
H8B^a 0.9800 109.47 109.47
H8C^a 0.9800 109.47 109.47 109.47
C8^a C3^a H8A^a H8B^a
C9^a - Distance Angles
C5^a 1.5101 (0.0082)
H9A^a 0.9800 109.47
H9B^a 0.9800 109.47 109.47
H9C^a 0.9800 109.47 109.47 109.47
C9^a C5^a H9A^a H9B^a
Selected torsion angles
0.00 ( 0.00) C6^a - C1^a - C2^a - C3^a
180.00 ( 0.00) C7^a - C1^a - C2^a - C3^a
0.00 ( 0.00) C1^a - C2^a - C3^a - C4^a
180.00 ( 0.00) C1^a - C2^a - C3^a - C8^a
0.00 ( 0.00) C2^a - C3^a - C4^a - C5^a
180.00 ( 0.00) C8^a - C3^a - C4^a - C5^a
0.00 ( 0.00) C3^a - C4^a - C5^a - C6^a
180.00 ( 0.00) C3^a - C4^a - C5^a - C9^a
0.00 ( 0.00) C4^a - C5^a - C6^a - C1^a
180.00 ( 0.00) C9^a - C5^a - C6^a - C1^a
180.00 ( 0.00) C4^a - C5^a - C6^a - I1^a
0.00 ( 0.00) C9^a - C5^a - C6^a - I1^a
0.00 ( 0.00) C2^a - C1^a - C6^a - C5^a
180.00 ( 0.00) C7^a - C1^a - C6^a - C5^a
180.00 ( 0.00) C2^a - C1^a - C6^a - I1^a
0.00 ( 0.00) C7^a - C1^a - C6^a - I1^a
FMAP and GRID set by program
FMAP 2 2 11
GRID -3.125 -2 -2 3.125 2 2
R1 = 0.0543 for 953 unique reflections after merging for Fourier
Electron density synthesis with coefficients Fo-Fc
Highest peak 2.22 at 0.5242 0.2500 0.1439 [ 1.34 A from H9A ]
Deepest hole -1.75 at 0.4324 0.2500 0.1081 [ 0.76 A from I1 ]
Mean = 0.00, Rms deviation from mean = 0.23, Highest memory used = 1725 / 11878
Fourier peaks appended to .res file
x y z sof U Peak Distances to nearest atoms (including eq.)
Q1 1 0.5242 0.2500 0.1439 0.50000 0.05 2.22 1.34 H9A 1.38 I1 1.65 C6 1.91 C9
Q2 1 0.1877 0.2500 0.1602 0.50000 0.05 1.58 1.38 I1 2.24 H7A 2.74 H8A 2.99 H9B
Q3 1 0.7818 0.2500 0.5853 0.50000 0.05 0.82 0.47 C3 1.14 C2 1.31 C4 1.94 H2
Q4 1 0.3191 0.0062 0.0787 1.00000 0.05 0.81 1.80 I1 2.15 H9C 2.15 H9B 2.21 H9A
Q5 1 0.3984 0.0102 0.2033 1.00000 0.05 0.77 1.78 I1 1.92 H2 2.30 C6 2.35 C2
Q6 1 0.9299 0.2500 0.1934 0.50000 0.05 0.73 1.17 H9B 1.17 H9C 1.17 H9B 1.17 H9C
Q7 1 0.4009 0.2500 0.0177 0.50000 0.05 0.67 1.19 I1 1.99 H9A 2.74 C6 2.88 C9
Q8 1 0.8778 0.2500 0.6856 0.50000 0.05 0.62 0.55 C3 0.96 C8^a 1.51 H8A 1.62 H8B
Q9 1 0.2836 0.1325 0.4839 1.00000 0.05 0.50 0.91 H7A 1.02 H7C 1.02 H7B^a 1.07 C7
Q10 1 1.0395 0.2500 0.4644 0.50000 0.05 0.49 0.54 H4 1.45 C4 1.93 H7A 2.32 C3
Q11 1 0.2978 0.2500 0.2835 0.50000 0.05 0.48 1.33 I1 1.34 H7A 2.07 C6 2.10 C7
Q12 1 0.4295 0.0624 0.2948 1.00000 0.05 0.46 1.69 C6 1.82 I1 2.23 C1 2.31 H2
Q13 1 0.3919 0.2500 0.7004 0.50000 0.05 0.43 1.12 H7C 1.12 H7B^a 1.12 H7C 1.12 H7B^a
Q14 1 0.3207 0.2500 0.8094 0.50000 0.05 0.40 1.87 H7C 1.87 H7B^a 1.87 H7C 1.87 H7B^a
Q15 1 0.4014 -0.0077 0.6039 1.00000 0.05 0.40 1.14 H7C 1.14 H7B^a 1.76 C6 1.90 C7
Q16 1 0.8178 0.0399 0.3576 1.00000 0.05 0.40 1.65 C5 1.71 C4 1.84 H7C 1.84 H7B^a
Q17 1 0.3737 0.2500 0.4989 0.50000 0.05 0.39 0.44 C7 0.87 H7A 1.24 C1 1.28 H7C
Q18 1 0.4225 0.2500 0.3293 0.50000 0.05 0.39 1.09 C6 1.50 I1 1.56 C1 1.68 H7A
Q19 1 1.0588 0.2500 1.0448 0.50000 0.05 0.38 1.53 H8A 2.19 C8^a 2.32 H9B 2.32 H9C
Q20 1 1.1045 0.1689 0.9578 1.00000 0.05 0.37 1.49 H8A 1.53 H8B 1.53 H8C 1.73 C8^a
Shortest distances between peaks (including symmetry equivalents)
5 12 0.82 11 18 0.99 3 8 1.00 19 20 1.05 4 5 1.08 9 17 1.09 20 20 1.14
13 14 1.17 2 11 1.19 2 19 1.24 1 7 1.27 12 18 1.36 12 15 1.48 17 18 1.53
9 15 1.56 13 17 1.63 9 9 1.66 11 12 1.69 7 14 1.69 11 17 1.74 2 20 1.75
6 19 1.78 4 12 1.84 9 11 1.87 15 16 1.88 1 18 1.89 4 7 1.95 5 18 1.97
9 13 1.98 13 15 1.99 5 15 2.00 15 17 2.00 5 11 2.05 9 18 2.05 1 12 2.08
9 16 2.08 2 18 2.09 1 5 2.09 9 10 2.11 4 20 2.13 2 6 2.16 2 4 2.20
6 10 2.21 9 12 2.21 15 18 2.21 12 17 2.26 5 7 2.28 2 7 2.29 6 16 2.32
10 16 2.34 1 4 2.37 1 11 2.37 2 5 2.37 7 20 2.41 2 12 2.41 14 20 2.42
11 19 2.43 4 11 2.44 3 16 2.46 8 10 2.47 3 10 2.50 5 13 2.50 7 11 2.51
7 18 2.53 3 15 2.55 14 16 2.58 15 15 2.59 7 13 2.60 7 12 2.60 8 20 2.62
10 16 2.63 12 13 2.63 13 16 2.63 12 12 2.65 12 15 2.65 1 15 2.65 10 17 2.65
14 15 2.66 4 18 2.67 4 19 2.68 14 17 2.68 6 20 2.70 2 9 2.73 1 2 2.75
9 14 2.76 15 17 2.76 3 9 2.78 4 14 2.81 5 9 2.81 7 19 2.83 10 11 2.83
11 20 2.84 2 17 2.85 1 14 2.87 6 11 2.90 9 15 2.91 4 20 2.91 9 15 2.94
15 18 2.94 5 14 2.94 11 15 2.95 9 12 2.95 16 16 2.96 16 17 2.97 5 20 2.97
8 19 2.99
Time profile in seconds
-----------------------
0.21: Read and process instructions
0.00: Fit rigid groups
0.00: Interpret restraints etc.
0.00: Generate connectivity array
0.00: Analyse DFIX and DANG restraints
0.00: Analyse SAME, SADI and NCSY restraints
0.00: Generate CHIV restraints
0.00: Check if bonds in residues restrained
0.00: Generate DELU and RIGU restraints
0.00: Generate SIMU restraints
0.00: Generate ISOR restraints
0.00: Analyse electron density
0.00: Analyse other restraints etc.
0.04: Read intensity data, sort/merge etc.
0.00: Set up constraints
0.08: OSF, H-atoms from difference map
1.48: Set up l.s. refinement
0.00: Generate idealized H-atoms
2.54: Structure factors, sum l.s. matrics
0.27: final structure factors
0.00: Generate and apply antibumping restraints
0.00: Apply other restraints
0.03: Solve l.s. equations
0.00: Generate HTAB table
0.14: Other dependent quantities, CIF, tables
0.00: Analysis of variance
0.16: Merge reflections for Fourier and .fcf
0.00: Fourier summations
0.00: Peaksearch
0.00: Analyse peaklist
** WARNING: These times are only approximate for multiple threads.
To get better estimates run with -t1 **
Please cite: G.M. Sheldrick (2015) "Crystal structure refinement with
SHELXL", Acta Cryst., C71, 3-8 (Open Access) if SHELXL proves useful.
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+ xray072 finished at 11:14:55 Total elapsed time: 4.94 secs +
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