++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
+ SHELXTL XLMP CRYSTAL STRUCTURE REFINEMENT - MULTI-CPU VERSION +
+ Copyright(c) Bruker AXS Inc. 1993-2018 Version 2018/3 +
+ neal054 started at 12:14:29 on 19-Oct-2021 +
++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
Command line parameters: neal054 -a50000 -b3000 -c624 -g0 -m0 -t12
-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 12 threads on 12 processors
TITL neal054 in P2(1)
CELL 1.54178 6.2572 11.763 13.0387 90 96.6572 90
ZERR 2 0.0005 0.0009 0.001 0 0.0027 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H N O I
UNIT 34 46 4 8 2
V = 953.22 F(000) = 448.0 Mu = 13.39 mm-1 Cell Wt = 892.55 Rho = 1.555
L.S. 20
PLAN 30
SIZE 0.028 0.099 0.172
TEMP -173.15
CONF
BOND $H
LIST 6
MORE -1
fmap 2
ACTA
WGHT 0.0522 1.0934
FVAR 0.17752
REM
REM
REM
I1 5 1.07140 0.20810 -0.02957 11.00000 0.05034 0.04733 0.03001 =
-0.01120 -0.00010 0.00966
O1 4 -0.00416 0.58955 0.43818 11.00000 0.02615 0.02643 0.05111 =
-0.00360 0.00350 -0.00321
O2 4 0.44225 0.59324 0.60549 11.00000 0.03306 0.01865 0.02023 =
-0.00324 0.00448 0.00713
O3 4 0.59559 0.42702 0.56160 11.00000 0.02790 0.01522 0.02685 =
-0.00040 0.00758 0.00440
O4 4 0.48098 0.55008 0.16942 11.00000 0.03379 0.04194 0.02025 =
-0.00204 0.00215 0.00231
N1 3 0.07941 0.77008 0.48851 11.00000 0.02037 0.01767 0.03777 =
-0.00070 0.00597 -0.00088
H1 2 0.14899 0.81540 0.48779 11.00000 0.01464
N2 3 0.44968 0.55230 0.44097 11.00000 0.02303 0.01584 0.02195 =
-0.00319 0.00440 0.00191
C1 1 -0.12451 0.79573 0.52624 11.00000 0.02689 0.02825 0.06497 =
0.00209 0.01218 0.00223
AFIX 137
H1a 2 -0.11625 0.87057 0.55948 11.00000 -1.50000
H1b 2 -0.15577 0.73783 0.57645 11.00000 -1.50000
H1c 2 -0.23917 0.79611 0.46827 11.00000 -1.50000
AFIX 0
C2 1 0.12200 0.66948 0.44870 11.00000 0.01709 0.01613 0.03226 =
0.00477 -0.00122 -0.00300
C3 1 0.34649 0.66167 0.41317 11.00000 0.01960 0.01763 0.02414 =
0.00029 -0.00052 0.00061
H3 2 0.43139 0.72823 0.44095 11.00000 0.01146
C4 1 0.33876 0.66310 0.29555 11.00000 0.03518 0.02150 0.02660 =
0.00410 -0.00082 -0.00091
H4a 2 0.34138 0.73362 0.26999 11.00000 0.01525
H4b 2 0.22022 0.62254 0.27716 11.00000 0.02311
C5 1 0.52327 0.58834 0.27346 11.00000 0.02890 0.03126 0.01779 =
0.00122 0.00318 -0.00641
H5 2 0.65483 0.63729 0.27984 11.00000 0.03689
C6 1 0.52440 0.49430 0.35348 11.00000 0.02662 0.02058 0.02072 =
-0.00242 0.00810 -0.00450
H6a 2 0.40892 0.43485 0.32569 11.00000 0.02876
H6b 2 0.67065 0.46713 0.36813 11.00000 0.05313
C7 1 0.50351 0.51670 0.53849 11.00000 0.01839 0.01608 0.02508 =
-0.00534 0.00445 -0.00284
C8 1 0.45224 0.56486 0.71663 11.00000 0.04359 0.03136 0.01870 =
-0.00372 0.00794 0.00350
C9 1 0.68328 0.54612 0.76294 11.00000 0.04935 0.04202 0.02508 =
0.00113 -0.00509 -0.00114
AFIX 137
H9a 2 0.73742 0.47535 0.73583 11.00000 -1.50000
H9b 2 0.68953 0.54095 0.83824 11.00000 -1.50000
H9c 2 0.77215 0.60994 0.74465 11.00000 -1.50000
AFIX 0
C10 1 0.30825 0.46215 0.72957 11.00000 0.04725 0.04308 0.03533 =
0.00789 0.02378 0.00274
AFIX 137
H10a 2 0.16909 0.47297 0.68786 11.00000 -1.50000
H10b 2 0.28602 0.45428 0.80241 11.00000 -1.50000
H10c 2 0.37728 0.39333 0.70675 11.00000 -1.50000
AFIX 0
C11 1 0.35688 0.67038 0.75908 11.00000 0.08078 0.04280 0.03443 =
-0.01016 0.02068 0.01592
AFIX 137
H11a 2 0.44306 0.73673 0.74440 11.00000 -1.50000
H11b 2 0.35678 0.66253 0.83390 11.00000 -1.50000
H11c 2 0.20891 0.68038 0.72649 11.00000 -1.50000
AFIX 0
C12 1 0.54818 0.42475 0.03891 11.00000 0.03959 0.04415 0.02119 =
0.00230 0.00045 -0.00312
H12 2 0.39563 0.43592 0.01953 11.00000 0.07262
C13 1 0.67628 0.34973 -0.00640 11.00000 0.04318 0.04930 0.01689 =
-0.00532 0.00047 -0.00156
H13 2 0.62166 0.31263 -0.05751 11.00000 0.02343
C14 1 0.88432 0.32906 0.03821 11.00000 0.04311 0.03080 0.02474 =
-0.00346 0.01069 0.00353
C15 1 0.96416 0.38279 0.12965 11.00000 0.02951 0.03200 0.02398 =
0.00094 0.00237 -0.00475
H15 2 1.08980 0.36569 0.16093 11.00000 0.02493
C16 1 0.83246 0.45663 0.17644 11.00000 0.03567 0.03376 0.02207 =
-0.00103 0.00714 -0.00808
H16 2 0.87693 0.49653 0.23491 11.00000 0.02863
C17 1 0.62577 0.47845 0.13209 11.00000 0.03201 0.03666 0.02097 =
0.00340 0.00673 -0.00860
HKLF 4
Covalent radii and connectivity table for neal054 in P2(1)
C 0.770
H 0.320
N 0.700
O 0.660
I 1.330
I1 - C14
O1 - C2
O2 - C7 C8
O3 - C7
O4 - C17 C5
N1 - C2 C1
N2 - C7 C6 C3
C1 - N1
C2 - O1 N1 C3
C3 - N2 C4 C2
C4 - C5 C3
C5 - O4 C4 C6
C6 - N2 C5
C7 - O3 O2 N2
C8 - O2 C11 C9 C10
C9 - C8
C10 - C8
C11 - C8
C12 - C13 C17
C13 - C12 C14
C14 - C13 C15 I1
C15 - C16 C14
C16 - C17 C15
C17 - O4 C16 C12
Floating origin restraints generated
h k l Fo^2 Sigma Why rejected (first 50 of each listed)
0 -1 0 0.27 0.04 systematically absent but >3sig(I)
0 -3 0 0.34 0.10 systematically absent but >3sig(I)
0 -3 0 0.28 0.07 systematically absent but >3sig(I)
0 -3 0 0.28 0.09 systematically absent but >3sig(I)
0 -3 0 0.31 0.07 systematically absent but >3sig(I)
0 -3 0 0.35 0.08 systematically absent but >3sig(I)
0 -3 0 0.22 0.05 systematically absent but >3sig(I)
0 -3 0 0.32 0.06 systematically absent but >3sig(I)
0 -3 0 0.38 0.12 systematically absent but >3sig(I)
46 Systematically absent reflections rejected
18124 Reflections read, of which 46 rejected
-7 =< h =< 7, -13 =< k =< 13, -15 =< l =< 15, Max. 2-theta = 127.62
9 Systematic absence violations (I>3sig(I)) before merging
0 Inconsistent equivalents
3118 Unique reflections, of which 0 suppressed
R(int) = 0.0562 R(sigma) = 0.0339 Friedel opposites not merged
Maximum memory for data reduction = 2805 / 31237
Reflection statistics for all twin components combined (TWST 0 set)
Number of data for d > 0.859A (CIF: max) and d > 0.859A (CIF: full)
(ignoring systematic absences):
Unique reflections found (point group) 3118 3117
Unique reflections possible (point group) 3144 3142
Unique reflections found (Laue group) 1652 1651
Unique reflections possible (Laue group) 1659 1658
Unique Friedel pairs found 1466 1466
Unique Friedel pairs possible 1485 1484
Default effective X-H and X-D distances for T = -173.2C
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 = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 1 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17752 0.00048 -0.009 OSF
Mean shift/esd = 0.002 Maximum = -0.024 for x I1
Max. shift = 0.000 A for H12 Max. dU = 0.000 for H6B
Least-squares cycle 2 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 2 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 -0.001 OSF
Mean shift/esd = 0.001 Maximum = -0.008 for x I1
Max. shift = 0.000 A for H12 Max. dU = 0.000 for H5
Least-squares cycle 3 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 3 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.001 for x H6B
Max. shift = 0.000 A for H12 Max. dU = 0.000 for H6B
Least-squares cycle 4 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 4 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 5 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 5 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 6 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 6 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 7 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 7 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 8 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 8 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 9 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 9 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 10 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 10 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 11 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 11 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 12 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 12 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 13 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 13 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 14 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 14 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 15 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 15 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 16 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 16 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 17 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 17 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 18 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 18 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 19 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 19 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Least-squares cycle 20 Maximum vector length = 623 Memory required = 56 / 3496 / 395246
wR2 = 0.087275 before cycle 20 for 3118 data and 265 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
N value esd shift/esd parameter
1 0.17751 0.00048 0.000 OSF
Mean shift/esd = 0.000 Maximum = 0.000 for x H6B
Max. shift = 0.000 A for H6B Max. dU = 0.000 for H6B
Largest correlation matrix elements
0.600 U33 I1 / OSF 0.585 U22 I1 / OSF
0.591 U11 I1 / OSF 0.546 U11 H1 / U12 N1
Idealized hydrogen atom generation before cycle 21
Name x y z AFIX d(X-H) shift Bonded to Conformation determined by
H1A -0.1163 0.8706 0.5595 137 0.980 0.000 C1 N1 H1A
H1B -0.1558 0.7378 0.5764 137 0.980 0.000 C1 N1 H1A
H1C -0.2392 0.7961 0.4683 137 0.980 0.000 C1 N1 H1A
H9A 0.7374 0.4753 0.7358 137 0.980 0.000 C9 C8 H9A
H9B 0.6895 0.5409 0.8382 137 0.980 0.000 C9 C8 H9A
H9C 0.7722 0.6099 0.7447 137 0.980 0.000 C9 C8 H9A
H10A 0.1691 0.4730 0.6879 137 0.980 0.000 C10 C8 H10A
H10B 0.2860 0.4543 0.8024 137 0.980 0.000 C10 C8 H10A
H10C 0.3773 0.3933 0.7067 137 0.980 0.000 C10 C8 H10A
H11A 0.4431 0.7367 0.7444 137 0.980 0.000 C11 C8 H11A
H11B 0.3568 0.6625 0.8339 137 0.980 0.000 C11 C8 H11A
H11C 0.2089 0.6804 0.7265 137 0.980 0.000 C11 C8 H11A
neal054 in P2(1)
ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq
I1 1.07140 0.20810 -0.02957 1.00000 0.05034 0.04733 0.03001 -0.01120 -0.00010 0.00966 0.04293
0.00072 0.00007 0.00004 0.00003 0.00000 0.00029 0.00029 0.00026 0.00023 0.00017 0.00026 0.00019
O1 -0.00416 0.58955 0.43818 1.00000 0.02615 0.02643 0.05112 -0.00360 0.00350 -0.00321 0.03464
0.00946 0.00078 0.00042 0.00043 0.00000 0.00237 0.00247 0.00318 0.00228 0.00230 0.00202 0.00112
O2 0.44225 0.59325 0.60549 1.00000 0.03307 0.01865 0.02023 -0.00324 0.00448 0.00713 0.02387
0.00825 0.00071 0.00036 0.00034 0.00000 0.00240 0.00207 0.00223 0.00172 0.00181 0.00180 0.00093
O3 0.59559 0.42702 0.56160 1.00000 0.02790 0.01521 0.02685 -0.00040 0.00758 0.00440 0.02298
0.00839 0.00072 0.00036 0.00034 0.00000 0.00230 0.00214 0.00244 0.00173 0.00182 0.00177 0.00093
O4 0.48098 0.55008 0.16942 1.00000 0.03379 0.04193 0.02025 -0.00204 0.00215 0.00231 0.03207
0.00889 0.00080 0.00043 0.00037 0.00000 0.00253 0.00288 0.00236 0.00200 0.00192 0.00210 0.00109
N1 0.07941 0.77008 0.48851 1.00000 0.02037 0.01768 0.03776 -0.00070 0.00597 -0.00088 0.02507
0.01314 0.00096 0.00061 0.00052 0.00000 0.00317 0.00347 0.00353 0.00265 0.00256 0.00240 0.00135
H1 0.14901 0.81541 0.48780 1.00000 0.01466
0.15186 0.01270 0.00737 0.00572 0.00000 0.02019
N2 0.44968 0.55230 0.44097 1.00000 0.02303 0.01584 0.02195 -0.00319 0.00440 0.00191 0.02013
0.00937 0.00083 0.00042 0.00041 0.00000 0.00260 0.00254 0.00275 0.00195 0.00209 0.00202 0.00108
C1 -0.12451 0.79573 0.52624 1.00000 0.02689 0.02826 0.06497 0.00209 0.01219 0.00222 0.03950
0.01588 0.00125 0.00068 0.00071 0.00000 0.00348 0.00361 0.00569 0.00334 0.00346 0.00305 0.00185
H1A -0.11626 0.87058 0.55948 1.00000 0.05925
0.00000 0.00000
H1B -0.15577 0.73783 0.57645 1.00000 0.05925
0.00000 0.00000
H1C -0.23918 0.79611 0.46827 1.00000 0.05925
0.00000 0.00000
C2 0.12200 0.66949 0.44870 1.00000 0.01709 0.01613 0.03226 0.00477 -0.00122 -0.00300 0.02215
0.01174 0.00107 0.00052 0.00058 0.00000 0.00274 0.00312 0.00340 0.00250 0.00270 0.00230 0.00134
C3 0.34650 0.66167 0.41317 1.00000 0.01960 0.01763 0.02414 0.00029 -0.00051 0.00061 0.02070
0.01150 0.00098 0.00052 0.00050 0.00000 0.00294 0.00274 0.00341 0.00238 0.00251 0.00241 0.00127
H3 0.43140 0.72822 0.44095 1.00000 0.01148
0.12298 0.00939 0.00605 0.00457 0.00000 0.01459
C4 0.33876 0.66310 0.29555 1.00000 0.03517 0.02150 0.02660 0.00410 -0.00082 -0.00091 0.02810
0.01495 0.00130 0.00067 0.00058 0.00000 0.00376 0.00323 0.00388 0.00277 0.00300 0.00282 0.00148
H4A 0.34138 0.73364 0.26999 1.00000 0.01525
0.12711 0.01070 0.00709 0.00531 0.00000 0.01679
H4B 0.22020 0.62254 0.27715 1.00000 0.02311
0.15232 0.01278 0.00663 0.00582 0.00000 0.01780
C5 0.52327 0.58834 0.27345 1.00000 0.02890 0.03125 0.01779 0.00122 0.00318 -0.00641 0.02594
0.01200 0.00106 0.00058 0.00049 0.00000 0.00338 0.00338 0.00317 0.00263 0.00252 0.00283 0.00134
H5 0.65483 0.63730 0.27983 1.00000 0.03693
0.15965 0.01370 0.00737 0.00665 0.00000 0.02134
C6 0.52440 0.49430 0.35348 1.00000 0.02662 0.02058 0.02071 -0.00242 0.00810 -0.00450 0.02222
0.01178 0.00110 0.00052 0.00050 0.00000 0.00335 0.00316 0.00319 0.00243 0.00267 0.00255 0.00131
H6A 0.40892 0.43484 0.32568 1.00000 0.02876
0.15063 0.01248 0.00689 0.00618 0.00000 0.01934
H6B 0.67069 0.46713 0.36814 1.00000 0.05318
0.18869 0.01710 0.00839 0.00803 0.00000 0.02752
C7 0.50351 0.51670 0.53849 1.00000 0.01839 0.01608 0.02508 -0.00533 0.00445 -0.00284 0.01970
0.01080 0.00099 0.00050 0.00048 0.00000 0.00282 0.00309 0.00336 0.00245 0.00231 0.00243 0.00126
C8 0.45224 0.56486 0.71663 1.00000 0.04359 0.03136 0.01870 -0.00372 0.00794 0.00350 0.03088
0.01305 0.00121 0.00059 0.00051 0.00000 0.00396 0.00361 0.00327 0.00263 0.00287 0.00297 0.00151
C9 0.68328 0.54612 0.76294 1.00000 0.04934 0.04203 0.02508 0.00113 -0.00509 -0.00113 0.03955
0.01434 0.00137 0.00071 0.00059 0.00000 0.00456 0.00439 0.00368 0.00313 0.00323 0.00352 0.00176
H9A 0.73742 0.47535 0.73583 1.00000 0.05933
0.00000 0.00000
H9B 0.68953 0.54095 0.83824 1.00000 0.05933
0.00000 0.00000
H9C 0.77215 0.60994 0.74466 1.00000 0.05933
0.00000 0.00000
C10 0.30825 0.46215 0.72957 1.00000 0.04725 0.04308 0.03533 0.00789 0.02378 0.00274 0.04040
0.01707 0.00140 0.00071 0.00065 0.00000 0.00440 0.00446 0.00425 0.00341 0.00363 0.00362 0.00185
H10A 0.16909 0.47297 0.68786 1.00000 0.06060
0.00000 0.00000
H10B 0.28602 0.45428 0.80241 1.00000 0.06060
0.00000 0.00000
H10C 0.37729 0.39333 0.70675 1.00000 0.06060
0.00000 0.00000
C11 0.35688 0.67038 0.75908 1.00000 0.08078 0.04280 0.03443 -0.01016 0.02068 0.01592 0.05157
0.01825 0.00174 0.00070 0.00066 0.00000 0.00625 0.00476 0.00441 0.00319 0.00429 0.00399 0.00230
H11A 0.44306 0.73673 0.74441 1.00000 0.07736
0.00000 0.00000
H11B 0.35677 0.66253 0.83390 1.00000 0.07736
0.00000 0.00000
H11C 0.20892 0.68038 0.72649 1.00000 0.07736
0.00000 0.00000
C12 0.54817 0.42475 0.03891 1.00000 0.03959 0.04415 0.02119 0.00229 0.00045 -0.00312 0.03522
0.01398 0.00132 0.00069 0.00058 0.00000 0.00410 0.00404 0.00351 0.00307 0.00295 0.00330 0.00161
H12 0.39557 0.43591 0.01954 1.00000 0.07260
0.22757 0.01881 0.01175 0.00907 0.00000 0.03696
C13 0.67627 0.34973 -0.00640 1.00000 0.04318 0.04931 0.01689 -0.00532 0.00047 -0.00156 0.03669
0.01492 0.00127 0.00074 0.00056 0.00000 0.00428 0.00455 0.00351 0.00317 0.00311 0.00347 0.00168
H13 0.62165 0.31264 -0.05751 1.00000 0.02342
0.15056 0.01201 0.00674 0.00656 0.00000 0.01820
C14 0.88432 0.32906 0.03821 1.00000 0.04311 0.03080 0.02475 -0.00345 0.01069 0.00353 0.03236
0.01352 0.00123 0.00064 0.00052 0.00000 0.00398 0.00374 0.00380 0.00272 0.00308 0.00306 0.00158
C15 0.96416 0.38279 0.12965 1.00000 0.02951 0.03200 0.02397 0.00094 0.00237 -0.00474 0.02855
0.01267 0.00118 0.00060 0.00054 0.00000 0.00356 0.00358 0.00340 0.00268 0.00283 0.00288 0.00140
H15 1.08980 0.36569 0.16094 1.00000 0.02494
0.14206 0.01290 0.00653 0.00590 0.00000 0.01871
C16 0.83246 0.45663 0.17644 1.00000 0.03566 0.03377 0.02207 -0.00103 0.00714 -0.00807 0.03020
0.01353 0.00120 0.00062 0.00055 0.00000 0.00373 0.00375 0.00350 0.00283 0.00285 0.00296 0.00148
H16 0.87693 0.49654 0.23493 1.00000 0.02864
0.15451 0.01238 0.00692 0.00654 0.00000 0.01962
C17 0.62577 0.47845 0.13209 1.00000 0.03201 0.03666 0.02097 0.00340 0.00673 -0.00860 0.02959
0.01288 0.00111 0.00062 0.00052 0.00000 0.00349 0.00358 0.00324 0.00275 0.00279 0.00294 0.00143
Final Structure Factor Calculation for neal054 in P2(1)
Total number of l.s. parameters = 265 Maximum vector length = 623 Memory required = 56 / 3231 / 29281
wR2 = 0.087275 before cycle 21 for 3118 data and 0 / 265 parameters
GooF = S = 1.077; Restrained GooF = 1.077 for 1 restraints
Weight = 1 / [ sigma^2(Fo^2) + ( 0.0522 * P )^2 + 1.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3
wR2 = 0.087275, GooF = S = 1.07693, Restrained GooF = 1.07674 for all data
R1 = 0.032459 for 3072 Fo > 4sig(Fo) and 0.032995 for all 3118 data
Flack x = -0.024(9) by classical fit to all intensities
-0.024(6) from 1408 selected quotients (Parsons' method)
Occupancy sum of asymmetric unit = 24.00 for non-hydrogen and 23.00 for H and D atoms
Principal mean square atomic displacements U
0.0637 0.0407 0.0244 I1
0.0518 0.0292 0.0229 O1
0.0361 0.0223 0.0133 O2
0.0319 0.0236 0.0134 O3
0.0429 0.0333 0.0201 O4
0.0379 0.0199 0.0174 N1
0.0242 0.0226 0.0136 N2
0.0657 0.0288 0.0240 C1
0.0355 0.0176 0.0133 C2
0.0261 0.0188 0.0173 C3
0.0381 0.0270 0.0192 C4
0.0367 0.0238 0.0173 C5
0.0314 0.0185 0.0168 C6
0.0281 0.0178 0.0132 C7
0.0446 0.0320 0.0160 C8
0.0540 0.0419 0.0228 C9
0.0615 0.0417 0.0179 C10
0.0874 0.0491 0.0182 C11
0.0465 0.0383 0.0208 C12
0.0502 0.0439 0.0159 C13
0.0451 0.0324 0.0196 C14
0.0359 0.0259 0.0239 C15
0.0431 0.0272 0.0203 C16
0.0434 0.0285 0.0169 C17
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 0.043 0.067 0.087 0.105 0.126 0.150 0.177 0.222 0.290 1.000
Number in group 317. 307. 319. 314. 304. 316. 306. 314. 310. 311.
GooF 1.051 1.105 1.057 1.095 1.099 0.942 0.954 1.213 1.001 1.215
K 1.071 1.020 1.011 1.018 1.012 1.008 1.010 0.985 0.986 1.041
Resolution(A) 0.86 0.89 0.93 0.97 1.02 1.08 1.17 1.28 1.47 1.86 inf
Number in group 324. 303. 316. 305. 311. 310. 314. 314. 310. 311.
GooF 1.162 1.003 1.056 0.999 0.815 0.847 0.854 0.937 1.162 1.668
K 1.014 1.020 1.026 1.017 1.007 0.993 0.975 0.981 0.995 1.059
R1 0.062 0.043 0.041 0.034 0.028 0.024 0.024 0.023 0.028 0.039
Recommended weighting scheme: WGHT 0.0522 1.0939
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)
4 -6 7 537.07 850.45 5.63 0.181 0.98
1 3 3 85.14 40.70 4.70 0.039 2.55
5 -3 7 573.95 843.73 4.39 0.180 0.95
1 1 0 152.23 241.24 4.35 0.096 5.50
0 0 4 14334.49 11053.15 4.21 0.651 3.24
3 -4 7 1865.62 2490.99 4.05 0.309 1.19
0 0 1 902.14 1195.88 4.04 0.214 12.95
1 -3 5 134.58 221.72 3.99 0.092 1.98
0 0 5 4009.10 3150.11 3.97 0.347 2.59
-3 0 1 13.15 1.79 3.93 0.008 2.08
0 -2 7 918.63 709.12 3.76 0.165 1.76
2 -6 8 680.50 905.12 3.72 0.186 1.12
1 1 2 1088.67 794.12 3.71 0.174 3.99
1 -1 2 1243.14 894.26 3.66 0.185 3.99
4 -5 7 261.84 368.08 3.59 0.119 1.02
3 -6 7 721.85 948.48 3.57 0.191 1.09
-4 -11 2 128.08 78.13 3.56 0.055 0.88
-2 -2 4 1078.73 834.92 3.54 0.179 2.21
1 -7 8 835.72 1094.97 3.51 0.205 1.13
4 -3 7 226.31 319.18 3.50 0.111 1.08
2 3 5 102.54 62.66 3.40 0.049 1.70
3 -8 7 439.31 583.04 3.39 0.149 0.98
1 0 1 15562.75 12600.54 3.35 0.695 5.37
3 6 0 73.56 120.76 3.28 0.068 1.42
-2 -2 5 208.10 146.64 3.23 0.075 1.99
6 -3 6 343.05 480.07 3.23 0.136 0.87
7 -2 1 210.08 313.69 3.12 0.110 0.87
0 0 7 4991.46 4151.94 3.10 0.399 1.85
2 -3 5 40.89 72.78 3.10 0.053 1.70
2 -7 8 140.68 199.22 3.10 0.087 1.06
-2 2 2 112.79 163.54 3.10 0.079 2.63
-1 -2 2 12506.07 10217.33 3.08 0.626 3.70
1 0 4 11870.92 9914.39 3.08 0.616 2.74
-2 2 4 1035.71 832.37 3.07 0.179 2.21
-2 -13 1 371.56 260.44 3.07 0.100 0.87
0 4 2 2340.27 2857.95 3.07 0.331 2.68
3 11 1 285.32 194.17 3.06 0.086 0.94
-3 2 9 1006.64 1258.28 3.05 0.220 1.22
1 2 2 18412.44 15093.81 3.04 0.760 3.44
1 -3 3 43.02 71.80 3.02 0.052 2.55
2 -4 0 68.65 103.85 2.99 0.063 2.14
-7 0 5 62.36 33.87 2.98 0.036 0.87
-2 -2 2 431.16 328.00 2.96 0.112 2.63
-7 0 2 78.56 46.69 2.96 0.042 0.89
0 2 7 580.45 456.20 2.95 0.132 1.76
2 2 4 12067.28 10091.73 2.95 0.622 2.00
2 0 0 14511.12 12055.03 2.94 0.680 3.11
5 9 3 63.92 20.91 2.87 0.028 0.87
1 1 4 1349.70 1109.01 2.87 0.206 2.67
-2 6 2 33.13 59.45 2.86 0.048 1.63
Bond lengths and angles
I1 - Distance Angles
C14 2.1014 (0.0070)
I1
O1 - Distance Angles
C2 1.2252 (0.0082)
O1
O2 - Distance Angles
C7 1.3411 (0.0074)
C8 1.4814 (0.0080) 120.21 (0.48)
O2 C7
O3 - Distance Angles
C7 1.2228 (0.0078)
O3
O4 - Distance Angles
C17 1.3674 (0.0088)
C5 1.4246 (0.0081) 118.42 (0.54)
O4 C17
N1 - Distance Angles
C2 1.3314 (0.0086)
C1 1.4515 (0.0092) 122.71 (0.71)
H1 0.6892 (0.0853) 121.81 (6.58) 115.17 (6.52)
N1 C2 C1
N2 - Distance Angles
C7 1.3439 (0.0086)
C6 1.4523 (0.0079) 121.90 (0.51)
C3 1.4659 (0.0080) 124.22 (0.50) 113.00 (0.50)
N2 C7 C6
C1 - Distance Angles
N1 1.4515 (0.0092)
H1A 0.9800 109.47
H1B 0.9800 109.47 109.47
H1C 0.9800 109.47 109.47 109.47
C1 N1 H1A H1B
C2 - Distance Angles
O1 1.2252 (0.0082)
N1 1.3314 (0.0086) 124.77 (0.69)
C3 1.5321 (0.0092) 121.43 (0.62) 113.78 (0.56)
C2 O1 N1
C3 - Distance Angles
N2 1.4659 (0.0080)
C4 1.5289 (0.0098) 102.68 (0.51)
C2 1.5321 (0.0092) 111.77 (0.50) 112.28 (0.57)
H3 0.9908 (0.0705) 113.63 (3.45) 108.13 (3.46) 108.28 (3.39)
C3 N2 C4 C2
C4 - Distance Angles
C5 1.5055 (0.0102)
C3 1.5289 (0.0098) 104.46 (0.56)
H4A 0.8950 (0.0823) 115.00 (4.34) 112.58 (4.34)
H4B 0.8912 (0.0832) 105.58 (4.71) 101.11 (4.84) 116.53 (6.73)
C4 C5 C3 H4A
C5 - Distance Angles
O4 1.4246 (0.0081)
C4 1.5055 (0.0102) 107.75 (0.57)
C6 1.5202 (0.0089) 114.16 (0.54) 103.67 (0.53)
H5 1.0001 (0.0876) 108.74 (4.99) 106.85 (4.82) 115.06 (4.95)
C5 O4 C4 C6
C6 - Distance Angles
N2 1.4523 (0.0079)
C5 1.5202 (0.0089) 102.77 (0.50)
H6A 1.0402 (0.0825) 108.40 (4.32) 107.60 (4.40)
H6B 0.9674 (0.1061) 112.55 (6.22) 107.75 (5.96) 116.73 (7.24)
C6 N2 C5 H6A
C7 - Distance Angles
O3 1.2228 (0.0078)
O2 1.3411 (0.0074) 125.50 (0.58)
N2 1.3439 (0.0086) 124.14 (0.54) 110.35 (0.51)
C7 O3 O2
C8 - Distance Angles
O2 1.4814 (0.0080)
C11 1.5098 (0.0099) 101.52 (0.56)
C9 1.5168 (0.0112) 110.63 (0.57) 111.87 (0.68)
C10 1.5282 (0.0110) 109.12 (0.59) 110.27 (0.65) 112.83 (0.66)
C8 O2 C11 C9
C9 - Distance Angles
C8 1.5168 (0.0112)
H9A 0.9800 109.47
H9B 0.9800 109.47 109.47
H9C 0.9800 109.47 109.47 109.47
C9 C8 H9A H9B
C10 - Distance Angles
C8 1.5282 (0.0110)
H10A 0.9800 109.47
H10B 0.9800 109.47 109.47
H10C 0.9800 109.47 109.47 109.47
C10 C8 H10A H10B
C11 - Distance Angles
C8 1.5098 (0.0098)
H11A 0.9800 109.47
H11B 0.9800 109.47 109.47
H11C 0.9800 109.47 109.47 109.47
C11 C8 H11A H11B
C12 - Distance Angles
C13 1.3712 (0.0118)
C17 1.4051 (0.0107) 120.08 (0.74)
H12 0.9679 (0.1185) 125.67 (7.43) 113.34 (7.22)
C12 C13 C17
C13 - Distance Angles
C12 1.3712 (0.0118)
C14 1.3843 (0.0110) 120.01 (0.73)
H13 0.8358 (0.0831) 118.30 (5.31) 121.40 (5.26)
C13 C12 C14
C14 - Distance Angles
C13 1.3843 (0.0110)
C15 1.3901 (0.0101) 120.49 (0.67)
I1 2.1014 (0.0070) 119.00 (0.54) 120.41 (0.55)
C14 C13 C15
C15 - Distance Angles
C16 1.3865 (0.0107)
C14 1.3901 (0.0101) 119.30 (0.71)
H15 0.8663 (0.0806) 119.43 (5.07) 120.97 (5.12)
C15 C16 C14
C16 - Distance Angles
C17 1.3782 (0.0108)
C15 1.3865 (0.0107) 120.59 (0.69)
H16 0.9112 (0.0851) 115.84 (4.92) 123.47 (4.94)
C16 C17 C15
C17 - Distance Angles
O4 1.3674 (0.0088)
C16 1.3782 (0.0108) 126.42 (0.65)
C12 1.4051 (0.0107) 114.08 (0.65) 119.50 (0.69)
C17 O4 C16
Selected torsion angles
1.13 ( 1.14) C1 - N1 - C2 - O1
179.61 ( 0.67) C1 - N1 - C2 - C3
175.55 ( 0.59) C7 - N2 - C3 - C4
6.14 ( 0.67) C6 - N2 - C3 - C4
-63.90 ( 0.78) C7 - N2 - C3 - C2
126.69 ( 0.57) C6 - N2 - C3 - C2
-42.99 ( 0.89) O1 - C2 - C3 - N2
138.48 ( 0.60) N1 - C2 - C3 - N2
71.80 ( 0.82) O1 - C2 - C3 - C4
-106.74 ( 0.70) N1 - C2 - C3 - C4
-26.47 ( 0.67) N2 - C3 - C4 - C5
-146.67 ( 0.56) C2 - C3 - C4 - C5
-178.74 ( 0.55) C17 - O4 - C5 - C4
-64.19 ( 0.75) C17 - O4 - C5 - C6
158.21 ( 0.55) C3 - C4 - C5 - O4
36.87 ( 0.69) C3 - C4 - C5 - C6
-153.37 ( 0.57) C7 - N2 - C6 - C5
16.32 ( 0.66) C3 - N2 - C6 - C5
-149.25 ( 0.52) O4 - C5 - C6 - N2
-32.31 ( 0.66) C4 - C5 - C6 - N2
-9.97 ( 0.92) C8 - O2 - C7 - O3
170.13 ( 0.55) C8 - O2 - C7 - N2
-9.12 ( 0.93) C6 - N2 - C7 - O3
-177.62 ( 0.57) C3 - N2 - C7 - O3
170.78 ( 0.53) C6 - N2 - C7 - O2
2.28 ( 0.80) C3 - N2 - C7 - O2
-176.51 ( 0.62) C7 - O2 - C8 - C11
64.61 ( 0.76) C7 - O2 - C8 - C9
-60.10 ( 0.75) C7 - O2 - C8 - C10
-1.71 ( 1.18) C17 - C12 - C13 - C14
0.83 ( 1.18) C12 - C13 - C14 - C15
177.26 ( 0.60) C12 - C13 - C14 - I1
0.62 ( 1.08) C13 - C14 - C15 - C16
-175.76 ( 0.51) I1 - C14 - C15 - C16
-1.19 ( 1.04) C14 - C15 - C16 - C17
-14.59 ( 0.95) C5 - O4 - C17 - C16
165.88 ( 0.60) C5 - O4 - C17 - C12
-179.20 ( 0.62) C15 - C16 - C17 - O4
0.31 ( 1.04) C15 - C16 - C17 - C12
-179.29 ( 0.68) C13 - C12 - C17 - O4
1.15 ( 1.09) C13 - C12 - C17 - C16
FMAP and GRID set by program
FMAP 2 1 16
GRID -3.846 -2 -2 3.846 2 2
R1 = 0.028636 for 1652 unique reflections after merging for Fourier
Electron density synthesis with coefficients Fo-Fc
Highest peak 0.87 at 0.2006 0.2408 0.9582 [ 0.93 A from I1 ]
Deepest hole -0.47 at 0.1221 0.2053 0.1077 [ 1.78 A from I1 ]
Fourier peaks appended to .res file
x y z sof U Peak Distances to nearest atoms (including eq.)
Q1 1 1.2006 0.2408 -0.0418 1.00000 0.05 0.87 0.93 I1 2.56 C14 2.68 H12 2.80 H13^a
Q2 1 0.9761 0.1452 -0.0070 1.00000 0.05 0.84 1.02 I1 2.33 C14 2.98 H13^a 3.05 C13
Q3 1 0.9929 0.2801 -0.0161 1.00000 0.05 0.73 1.00 I1 1.19 C14 2.16 C13 2.28 C15
Q4 1 1.1399 0.1475 -0.0534 1.00000 0.05 0.58 0.91 I1 2.74 C17 2.78 C16^a 2.95 H16
Q5 1 1.1093 0.2064 0.0370 1.00000 0.05 0.40 0.87 I1 2.02 C14 2.49 H15 2.62 C15
Q6 1 0.5142 0.3896 0.5774 1.00000 0.05 0.36 0.72 O3 1.58 C7 1.95 H3 1.98 H10C
Q7 1 0.5758 0.4636 0.5590 1.00000 0.05 0.33 0.45 O3 0.80 C7 1.87 O2 1.95 N2
Q8 1 0.6032 0.3840 0.5456 1.00000 0.05 0.32 0.55 O3 1.68 C7 1.84 H1 1.86 H3
Q9 1 0.4027 0.5158 0.4535 1.00000 0.05 0.32 0.56 N2 1.21 C7 1.61 C6 1.82 C3
Q10 1 0.0331 0.6578 0.4443 1.00000 0.05 0.31 0.57 C2 0.84 O1 1.46 N1 2.05 H1
Q11 1 -0.0025 0.6058 0.4937 1.00000 0.05 0.30 0.75 O1 1.27 C2 2.00 N1 2.18 H1B
Q12 1 0.3536 0.5136 0.7216 1.00000 0.05 0.29 0.68 C10 0.87 C8 1.28 H10A 1.37 H10B
Q13 1 0.4587 0.6722 0.2838 1.00000 0.05 0.28 0.79 C4 1.03 H4A 1.08 C5 1.30 H5
Q14 1 -0.0330 0.7805 0.5056 1.00000 0.05 0.27 0.68 C1 0.77 N1 1.26 H1 1.34 H1C
Q15 1 0.4290 0.5824 0.6437 1.00000 0.05 0.26 0.53 O2 0.97 C8 1.69 C7 1.92 C11
Q16 1 0.2269 0.6553 0.4359 1.00000 0.05 0.25 0.72 C2 0.84 C3 1.54 H3 1.64 O1
Q17 1 0.4518 0.6373 0.7356 1.00000 0.05 0.24 0.80 C11 0.89 C8 1.18 H11A 1.50 H11B
Q18 1 0.9910 0.2065 0.0992 1.00000 0.05 0.23 1.74 C14 1.81 I1 2.10 H15 2.12 C15
Q19 1 0.4228 0.6885 0.2268 1.00000 0.05 0.22 0.96 H4A 1.13 C4 1.44 C5 1.65 H5
Q20 1 0.4825 0.6412 0.1798 1.00000 0.05 0.22 1.08 O4 1.37 C5 1.59 H5 1.86 C4
Q21 1 0.1646 0.4590 0.7195 1.00000 0.05 0.21 0.45 H10A 0.89 C10 1.25 H10B 1.56 H10C
Q22 1 0.9024 0.4058 0.1643 1.00000 0.05 0.21 0.68 C15 0.77 C16^a 1.27 H15 1.43 H16
Q23 1 0.4799 0.3546 0.4232 1.00000 0.05 0.21 1.60 H6A 1.91 C6 1.97 H6B 2.05 O3
Q24 1 0.6141 0.6962 0.1753 1.00000 0.05 0.21 1.52 H5 1.91 O4 1.93 C5 2.26 H4A
Q25 1 0.8010 0.3288 -0.0177 1.00000 0.05 0.21 0.85 C14 0.85 C13 1.20 H13^a 2.14 C12
Q26 1 0.5868 0.4203 0.0221 1.00000 0.05 0.21 0.35 C12 1.09 C13 1.21 H12 1.58 C17
Q27 1 1.0178 0.3745 0.0139 1.00000 0.05 0.20 1.07 C14 1.59 C15 1.92 H15 2.08 I1
Q28 1 0.4307 0.6341 0.6043 1.00000 0.05 0.20 0.49 O2 1.67 C8 1.72 C7 2.16 C11
Q29 1 0.5651 0.4428 0.0973 1.00000 0.05 0.20 0.70 C17 0.79 C12 1.38 H12 1.69 O4
Q30 1 0.3205 0.4559 0.7548 1.00000 0.05 0.20 0.34 C10 0.68 H10B 1.05 H10C 1.23 H10A
Shortest distances between peaks (including symmetry equivalents)
6 8 0.73 13 19 0.77 15 28 0.80 12 30 0.84 10 11 0.93 19 20 0.94 7 8 0.97
6 7 0.99 21 30 1.03 26 29 1.04 20 24 1.05 5 18 1.16 1 4 1.16 3 27 1.18
2 5 1.20 10 16 1.23 2 4 1.25 3 5 1.28 1 5 1.30 3 25 1.33 12 21 1.34
15 17 1.35 4 5 1.40 12 15 1.42 13 20 1.43 19 24 1.44 1 3 1.45 25 27 1.47
2 18 1.55 12 17 1.58 2 3 1.59 17 28 1.70 10 14 1.72 8 23 1.72 3 18 1.74
7 9 1.76 11 16 1.79 13 24 1.83 25 26 1.84 1 2 1.89 3 4 1.90 9 16 1.97
9 23 2.01 6 23 2.04 7 15 2.06 5 27 2.07 11 14 2.07 1 27 2.12 12 28 2.18
22 27 2.20 7 23 2.21 22 29 2.23 15 30 2.24 6 9 2.25 8 9 2.25 1 24 2.26
18 27 2.28 7 28 2.31 17 30 2.31 18 25 2.32 4 18 2.39 9 28 2.40 4 24 2.41
1 18 2.41 2 25 2.42 16 28 2.42 14 16 2.45 5 25 2.45 15 21 2.49 6 15 2.51
22 25 2.55 22 26 2.55 18 22 2.58 9 15 2.59 25 29 2.60 13 16 2.60 20 29 2.65
6 12 2.67 23 28 2.69 2 27 2.72 7 12 2.73 17 21 2.75 1 25 2.76 26 27 2.76
6 30 2.84 9 10 2.84 9 11 2.85 3 22 2.89 8 16 2.89 9 13 2.93 8 15 2.93
11 28 2.94 4 27 2.94 6 28 2.95 15 16 2.98
Time profile in seconds
-----------------------
0.07: 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.
0.07: Read intensity data, sort/merge etc.
0.00: Set up constraints
0.01: OSF, H-atoms from difference map
0.34: Set up l.s. refinement
0.00: Generate idealized H-atoms
0.56: Structure factors and derivatives
0.23: Sum l.s. matrices
0.00: Generate and apply antibumping restraints
0.01: Apply other restraints
0.20: Solve l.s. equations
0.00: Generate HTAB table
0.10: Other dependent quantities, CIF, tables
0.00: Analysis of variance
0.02: 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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+ neal054 finished at 12:14:31 Total elapsed time: 1.63 secs +
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