#------------------------------------------------------------------------------
#$Date: 2018-01-13 08:36:24 +0200 (Sat, 13 Jan 2018) $
#$Revision: 205190 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/86/1548682.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_1548682
loop_
_publ_author_name
'El-Hiti, Gamal A.'
'Abdel-Wahab, Bakr F.'
'Alotaibi, Mohammad Hayal'
'Hegazy, Amany S.'
'Kariuki, Benson M.'
_publ_section_title
;
(E)-3-(4-Fluorophenyl)-1-[1-(4-fluorophenyl)-5-methyl-1H-1,2,3-triazol-4-yl]prop-2-en-1-one
;
_journal_coeditor_code HB4197
_journal_issue 1
_journal_name_full IUCrData
_journal_page_first x171841
_journal_paper_doi 10.1107/S2414314617018417
_journal_volume 3
_journal_year 2018
_chemical_formula_iupac 'C18 H13 F2 N3 O'
_chemical_formula_moiety 'C18 H13 F2 N3 O'
_chemical_formula_sum 'C18 H13 F2 N3 O'
_chemical_formula_weight 325.31
_chemical_name_systematic
(E)-3-(4-Fluorophenyl)-1-[1-(4-fluorophenyl)-5-methyl-1H-1,2,3-triazol-4-yl]prop-2-en-1-one
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_audit_creation_method SHELXL-2013
_cell_angle_alpha 68.075(4)
_cell_angle_beta 84.220(4)
_cell_angle_gamma 74.627(4)
_cell_formula_units_Z 4
_cell_length_a 8.1891(4)
_cell_length_b 14.1804(6)
_cell_length_c 14.5050(6)
_cell_measurement_reflns_used 6895
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 27.6760
_cell_measurement_theta_min 4.2010
_cell_volume 1506.65(13)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) and CHEMDRAW Ultra (Cambridge Soft,
2001)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0294
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 26379
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.829
_diffrn_reflns_theta_min 2.989
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.109
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.503
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.434
_exptl_crystal_description plate
_exptl_crystal_F_000 672
_exptl_crystal_size_max 0.325
_exptl_crystal_size_mid 0.208
_exptl_crystal_size_min 0.096
_refine_diff_density_max 0.143
_refine_diff_density_min -0.206
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.050
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 435
_refine_ls_number_reflns 7530
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.050
_refine_ls_R_factor_all 0.0863
_refine_ls_R_factor_gt 0.0526
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+0.4741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1202
_refine_ls_wR_factor_ref 0.1409
_reflns_number_gt 4890
_reflns_number_total 7530
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb4197sup1.cif
_cod_data_source_block I
_cod_database_code 1548682
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.966
_shelx_estimated_absorpt_t_max 0.990
_shelx_hkl_file
;
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-10 -9 -7 384.480 67.8534 4
-10 -9 -8 35.6763 24.7449 4
-10 -9 -9-17.2960 19.4802 4
10 10 -3-37.9909 23.5638 7
10 10 -2 17.5743 18.9326 7
10 10 -1 339.663 63.1960 7
10 10 -1 253.418 69.9743 1
-10 -10 0 63.1612 28.1176 4
10 10 0 66.9304 31.9284 7
-10 -10 -1 16.3222 16.9923 4
10 10 1-1.39489 14.8862 7
10 10 1 17.1945 24.0066 1
-10 -10 -2 405.249 64.8885 4
10 10 2 360.878 72.8044 1
10 10 2 400.004 75.4588 7
10 10 3 18.3124 19.8880 1
-10 -10 -3 8.32677 12.3821 4
-10 -10 -4 29.9858 21.9832 4
-10 -10 -5 497.606 71.5666 4
-10 -10 -6 106.478 39.2810 4
-10 -10 -7 10.8131 16.8836 4
-10 -10 -8 40.5770 25.2356 4
-10 -10 -9 18.3106 18.5738 4
10 11 -1 131.652 42.7394 7
10 11 0 25.0452 27.5011 1
10 11 0 7.71119 15.7121 7
10 11 1 56.6083 34.4744 1
10 11 1 22.1080 26.1906 7
10 11 2 264.404 61.4500 7
10 11 2 163.698 52.9101 1
10 11 3-7.43313 18.4318 7
10 11 3 3.62106 17.0750 1
-10 -11 -4-10.1044 19.0081 4
-10 -11 -5 4.56270 13.3139 4
-10 -11 -6-4.02849 12.7908 4
-10 -11 -7-36.4237 22.3638 4
-10 -11 -8-17.6773 17.4244 4
-10 -11 -9-3.31625 16.5697 4
10 12 0 68.9074 35.4925 7
10 12 1-14.0473 18.5463 7
10 12 1 63.2401 37.0990 1
10 12 2-39.2303 30.3362 1
10 12 2 28.5317 24.4822 7
10 12 3-40.8124 29.1218 1
10 12 3 6.96706 20.3757 7
10 13 2 9.47633 16.5557 7
11 1 0 17.7756 19.7998 1
11 2 -1 50.9691 30.6615 1
11 2 0-4.30229 17.9077 1
11 2 1-29.6066 22.9934 1
11 3 -1 0.17347 14.4056 1
11 3 0-19.6451 21.5660 1
11 3 1 50.1323 29.7493 1
11 4 -1 71.6367 36.0771 1
11 4 0 68.9267 36.0635 1
11 4 1-41.8026 26.7300 1
11 5 -1 4.48289 22.7889 1
11 5 0 10.2115 19.6846 1
11 5 1 5.11130 20.0539 1
11 6 0 69.2348 35.6843 1
11 6 1 20.1198 22.4180 1
11 7 0 20.8025 27.5686 1
11 7 1-15.0735 20.6225 1
-11 -8 0-10.8293 17.1182 4
11 8 0 73.7710 37.4925 1
-11 -8 -1-20.5141 20.0218 4
11 8 1-64.5435 34.7422 1
-11 -8 -2 17.8347 21.5254 4
-11 -8 -3 21.6628 22.1450 4
-11 -9 -1 20.1051 20.5450 4
-11 -9 -2-0.15049 11.6832 4
-11 -9 -3-53.3813 29.0767 4
-11 -9 -4 34.8035 26.2032 4
0 0 0 0.00 0.00 0
TITL bmk1627b in P-1
REM P-1 (#2 in standard setting)
CELL 0.71073 8.189105 14.180433 14.505012 68.0754 84.2205 74.6265
ZERR 2.00 0.000404 0.000643 0.000615 0.0041 0.0038 0.0041
LATT 1
SFAC C H N O S
UNIT 64.00 24.00 4.00 4.00 2.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 41864
_shelx_res_file
;
TITL bmk1627b in P-1
CELL 0.71073 8.1891 14.1804 14.5050 68.075 84.220 74.627
ZERR 4.00 0.0004 0.0006 0.0006 0.004 0.004 0.004
LATT 1
SFAC C H N O F
UNIT 72 52 12 4 8
MERG 2
FMAP 2
PLAN 5
SIZE 0.096 0.208 0.325
ACTA
bond $h
mpla f1 c1 c2 c3 c4 c5 c6
mpla n1 n2 n3 c7 c8 c9
mpla o1 c10 c11 c12 c13 c14 c15 c16 c17 c18 f2
mpla f3 c19 c20 c21 c22 c23 c24
mpla c25 c26 c27 n4 n5 n6
mpla o2 c28 c29 c30 c31 c32 c33 c34 c35 c36 f4
eqiv $1 x+1, y-1, z
eqiv $2 x, y+1, z+1
eqiv $3 x-1, y+1, z
eqiv $4 x, y-1, z-1
htab c24 f1_$1
htab c35 f2_$2
htab c2 f3_$3
htab c17 f4_$4
L.S. 4
TEMP 23.00
WGHT 0.047700 0.474100
FVAR 2.81790
C1 1 0.207538 0.012663 0.033788 11.00000 0.07047 0.06203 =
0.06147 -0.03768 0.00525 -0.01689
C2 1 0.238376 0.059939 -0.064805 11.00000 0.09475 0.04733 =
0.06665 -0.02752 0.00708 -0.02393
AFIX 43
H2 2 0.228100 0.131896 -0.092605 11.00000 -1.20000
AFIX 0
C3 1 0.285360 -0.001710 -0.122579 11.00000 0.08175 0.04586 =
0.04728 -0.01673 0.00580 -0.02246
AFIX 43
H3 2 0.306699 0.028578 -0.190078 11.00000 -1.20000
AFIX 0
C4 1 0.300280 -0.108144 -0.079443 11.00000 0.05024 0.04286 =
0.04697 -0.02025 0.00685 -0.01599
C5 1 0.266490 -0.153565 0.020064 11.00000 0.07670 0.04672 =
0.05125 -0.01769 0.01576 -0.01780
AFIX 43
H5 2 0.275563 -0.225376 0.048412 11.00000 -1.20000
AFIX 0
C6 1 0.219148 -0.092205 0.077548 11.00000 0.08067 0.06266 =
0.04941 -0.02323 0.01298 -0.01678
AFIX 43
H6 2 0.195615 -0.121803 0.144832 11.00000 -1.20000
AFIX 0
C7 1 0.574350 -0.108546 -0.249354 11.00000 0.06263 0.05364 =
0.05843 -0.02136 0.01370 -0.03154
AFIX 137
H7A 2 0.519858 -0.045720 -0.301696 11.00000 -1.50000
H7B 2 0.674437 -0.144103 -0.274832 11.00000 -1.50000
H7C 2 0.604857 -0.090741 -0.196846 11.00000 -1.50000
AFIX 0
C8 1 0.456409 -0.178405 -0.210123 11.00000 0.04463 0.03778 =
0.03962 -0.01195 0.00575 -0.01504
C9 1 0.440639 -0.262153 -0.231688 11.00000 0.04859 0.03833 =
0.04414 -0.01352 0.00613 -0.01654
C10 1 0.532930 -0.307264 -0.303443 11.00000 0.05084 0.04146 =
0.04594 -0.01541 0.00557 -0.01473
C11 1 0.512679 -0.410660 -0.293526 11.00000 0.05480 0.04484 =
0.05026 -0.02010 0.00805 -0.01861
AFIX 43
H11 2 0.444630 -0.442837 -0.242580 11.00000 -1.20000
AFIX 0
C12 1 0.587200 -0.459858 -0.354037 11.00000 0.05341 0.04271 =
0.04408 -0.01542 0.00236 -0.01361
AFIX 43
H12 2 0.651260 -0.424710 -0.405646 11.00000 -1.20000
AFIX 0
C13 1 0.579146 -0.563629 -0.348074 11.00000 0.04936 0.04338 =
0.04336 -0.01672 0.00100 -0.01117
C14 1 0.497033 -0.627600 -0.271102 11.00000 0.06943 0.05120 =
0.05196 -0.02220 0.01223 -0.02050
AFIX 43
H14 2 0.443794 -0.603713 -0.221417 11.00000 -1.20000
AFIX 0
C15 1 0.493044 -0.725586 -0.267045 11.00000 0.07543 0.05215 =
0.06559 -0.01912 0.01324 -0.02787
AFIX 43
H15 2 0.438646 -0.768174 -0.215185 11.00000 -1.20000
AFIX 0
C16 1 0.571497 -0.758541 -0.341585 11.00000 0.07022 0.04308 =
0.07621 -0.02599 -0.00315 -0.01498
C17 1 0.653053 -0.699113 -0.418659 11.00000 0.07766 0.05325 =
0.06763 -0.03386 0.00980 -0.01406
AFIX 43
H17 2 0.704940 -0.723635 -0.468213 11.00000 -1.20000
AFIX 0
C18 1 0.656613 -0.601396 -0.421233 11.00000 0.06543 0.04901 =
0.05094 -0.02049 0.00988 -0.01542
AFIX 43
H18 2 0.712275 -0.559887 -0.473254 11.00000 -1.20000
AFIX 0
C19 1 1.242476 -0.661735 0.015461 11.00000 0.05418 0.05445 =
0.05095 -0.02599 0.00634 -0.01299
C20 1 1.328336 -0.590300 0.010264 11.00000 0.05565 0.08350 =
0.05823 -0.03377 0.02104 -0.03346
AFIX 43
H20 2 1.422881 -0.583400 -0.030609 11.00000 -1.20000
AFIX 0
C21 1 1.273554 -0.528118 0.066366 11.00000 0.06491 0.07166 =
0.05619 -0.02929 0.01547 -0.04100
AFIX 43
H21 2 1.331684 -0.479159 0.064122 11.00000 -1.20000
AFIX 0
C22 1 1.132339 -0.538583 0.125880 11.00000 0.04912 0.04050 =
0.03676 -0.01272 0.00135 -0.01677
C23 1 1.045086 -0.610352 0.128619 11.00000 0.04945 0.04641 =
0.04967 -0.01969 0.00987 -0.01933
AFIX 43
H23 2 0.948503 -0.616376 0.167801 11.00000 -1.20000
AFIX 0
C24 1 1.101559 -0.673312 0.072976 11.00000 0.05932 0.05079 =
0.06077 -0.02724 0.01057 -0.02478
AFIX 43
H24 2 1.044609 -0.722635 0.074695 11.00000 -1.20000
AFIX 0
C25 1 0.966326 -0.581666 0.340806 11.00000 0.07240 0.03987 =
0.04937 -0.01258 0.01562 -0.02083
AFIX 137
H25A 2 0.854889 -0.584660 0.328971 11.00000 -1.50000
H25B 2 0.972956 -0.584591 0.407560 11.00000 -1.50000
H25C 2 1.048346 -0.640046 0.331820 11.00000 -1.50000
AFIX 0
C26 1 1.001574 -0.482206 0.269758 11.00000 0.04700 0.03802 =
0.03841 -0.01119 0.00238 -0.01431
C27 1 0.980200 -0.386550 0.279266 11.00000 0.06017 0.03785 =
0.04238 -0.01214 0.00130 -0.01851
C28 1 0.907759 -0.351163 0.360981 11.00000 0.05789 0.03988 =
0.04601 -0.01514 0.00125 -0.01369
C29 1 0.916926 -0.244847 0.349648 11.00000 0.06808 0.04423 =
0.04841 -0.01674 0.00483 -0.02026
AFIX 43
H29 2 0.977390 -0.209200 0.296171 11.00000 -1.20000
AFIX 0
C30 1 0.843501 -0.197919 0.411704 11.00000 0.05872 0.04405 =
0.04589 -0.01587 0.00198 -0.01456
AFIX 43
H30 2 0.782567 -0.234774 0.464093 11.00000 -1.20000
AFIX 0
C31 1 0.848562 -0.093451 0.406163 11.00000 0.05580 0.04089 =
0.04440 -0.01629 -0.00165 -0.01110
C32 1 0.949451 -0.033986 0.337946 11.00000 0.06419 0.05467 =
0.05615 -0.02707 0.00951 -0.02026
AFIX 43
H32 2 1.017071 -0.061114 0.293769 11.00000 -1.20000
AFIX 0
C33 1 0.950474 0.063908 0.335011 11.00000 0.06964 0.05360 =
0.06554 -0.02106 0.00489 -0.02756
AFIX 43
H33 2 1.017933 0.103051 0.289470 11.00000 -1.20000
AFIX 0
C34 1 0.850096 0.102421 0.400545 11.00000 0.07227 0.04050 =
0.06271 -0.02049 -0.01307 -0.01263
C35 1 0.748857 0.048119 0.468110 11.00000 0.07892 0.04959 =
0.05868 -0.02750 0.00240 -0.01013
AFIX 43
H35 2 0.681197 0.076542 0.511431 11.00000 -1.20000
AFIX 0
C36 1 0.749161 -0.050196 0.470697 11.00000 0.07062 0.04745 =
0.04878 -0.01836 0.00773 -0.01627
AFIX 43
H36 2 0.681135 -0.088373 0.516783 11.00000 -1.20000
AFIX 0
N1 3 0.341729 -0.174220 -0.136925 11.00000 0.05293 0.03994 =
0.04810 -0.01850 0.01144 -0.02063
N2 3 0.257413 -0.251528 -0.115156 11.00000 0.06775 0.05580 =
0.06833 -0.03326 0.02761 -0.03580
N3 3 0.318584 -0.304412 -0.172046 11.00000 0.06356 0.04953 =
0.06452 -0.03006 0.02323 -0.02965
N4 3 1.074876 -0.469190 0.179514 11.00000 0.06197 0.03885 =
0.03975 -0.01316 0.00606 -0.02379
N5 3 1.099133 -0.369739 0.135504 11.00000 0.10726 0.04627 =
0.04424 -0.01609 0.01652 -0.04092
N6 3 1.041896 -0.320991 0.196097 11.00000 0.09966 0.04440 =
0.04511 -0.01623 0.01078 -0.03399
O1 4 0.623849 -0.260829 -0.366257 11.00000 0.08357 0.05598 =
0.06482 -0.02730 0.03379 -0.03316
O2 4 0.844473 -0.407169 0.433451 11.00000 0.08793 0.04888 =
0.05481 -0.01934 0.02095 -0.02495
F1 5 0.159196 0.072844 0.090646 11.00000 0.12264 0.08474 =
0.08517 -0.06055 0.01810 -0.02740
F2 5 0.568252 -0.855794 -0.336842 11.00000 0.11974 0.05381 =
0.12442 -0.04580 0.01546 -0.03317
F3 5 1.298473 -0.722822 -0.040056 11.00000 0.08783 0.08803 =
0.09154 -0.06229 0.03277 -0.03084
F4 5 0.851503 0.198913 0.397812 11.00000 0.11290 0.04986 =
0.09812 -0.03448 -0.00753 -0.02644
HKLF 4
REM bmk1627b in P-1
REM R1 = 0.0526 for 4890 Fo > 4sig(Fo) and 0.0863 for all 7530 data
REM 435 parameters refined using 0 restraints
END
WGHT 0.0477 0.4741
REM Highest difference peak 0.143, deepest hole -0.206, 1-sigma level 0.041
Q1 1 0.9835 -0.4325 0.2844 11.00000 0.05 0.14
Q2 1 0.1444 -0.2491 -0.0828 11.00000 0.05 0.14
Q3 1 0.9697 -0.3821 0.3200 11.00000 0.05 0.14
Q4 1 0.2978 -0.0513 0.0720 11.00000 0.05 0.14
Q5 1 0.8590 -0.0584 0.3593 11.00000 0.05 0.14
;
_shelx_res_checksum 98514
_shelxl_version_number .2013
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
C C1 0.2075(3) 0.01266(16) 0.03379(16) 0.0604(5) Uani d 1
C C2 0.2384(3) 0.05994(16) -0.06481(16) 0.0667(6) Uani d 1
H H2 0.2281 0.1319 -0.0926 0.080 Uiso calc 1
C C3 0.2854(3) -0.00171(14) -0.12258(14) 0.0574(5) Uani d 1
H H3 0.3067 0.0286 -0.1901 0.069 Uiso calc 1
C C4 0.3003(2) -0.10814(13) -0.07944(13) 0.0451(4) Uani d 1
C C5 0.2665(3) -0.15357(15) 0.02006(14) 0.0589(5) Uani d 1
H H5 0.2756 -0.2254 0.0484 0.071 Uiso calc 1
C C6 0.2191(3) -0.09221(17) 0.07755(15) 0.0645(6) Uani d 1
H H6 0.1956 -0.1218 0.1448 0.077 Uiso calc 1
C C7 0.5744(2) -0.10855(15) -0.24935(15) 0.0554(5) Uani d 1
H H7A 0.5199 -0.0457 -0.3017 0.083 Uiso calc 1
H H7B 0.6744 -0.1441 -0.2748 0.083 Uiso calc 1
H H7C 0.6049 -0.0907 -0.1968 0.083 Uiso calc 1
C C8 0.4564(2) -0.17840(12) -0.21012(12) 0.0407(4) Uani d 1
C C9 0.4406(2) -0.26215(13) -0.23169(13) 0.0434(4) Uani d 1
C C10 0.5329(2) -0.30726(13) -0.30344(13) 0.0459(4) Uani d 1
C C11 0.5127(2) -0.41066(14) -0.29353(14) 0.0484(4) Uani d 1
H H11 0.4446 -0.4428 -0.2426 0.058 Uiso calc 1
C C12 0.5872(2) -0.45986(13) -0.35404(13) 0.0466(4) Uani d 1
H H12 0.6513 -0.4247 -0.4056 0.056 Uiso calc 1
C C13 0.5791(2) -0.56363(13) -0.34807(13) 0.0452(4) Uani d 1
C C14 0.4970(3) -0.62760(15) -0.27110(14) 0.0562(5) Uani d 1
H H14 0.4438 -0.6037 -0.2214 0.067 Uiso calc 1
C C15 0.4930(3) -0.72559(16) -0.26704(16) 0.0636(5) Uani d 1
H H15 0.4386 -0.7682 -0.2152 0.076 Uiso calc 1
C C16 0.5715(3) -0.75854(15) -0.34159(17) 0.0614(5) Uani d 1
C C17 0.6531(3) -0.69911(16) -0.41866(16) 0.0638(5) Uani d 1
H H17 0.7049 -0.7236 -0.4682 0.077 Uiso calc 1
C C18 0.6566(3) -0.60140(15) -0.42123(14) 0.0549(5) Uani d 1
H H18 0.7123 -0.5599 -0.4733 0.066 Uiso calc 1
C C19 1.2425(2) -0.66173(15) 0.01546(14) 0.0517(4) Uani d 1
C C20 1.3283(3) -0.59030(17) 0.01026(15) 0.0616(5) Uani d 1
H H20 1.4229 -0.5834 -0.0306 0.074 Uiso calc 1
C C21 1.2736(3) -0.52812(16) 0.06637(14) 0.0586(5) Uani d 1
H H21 1.3317 -0.4792 0.0641 0.070 Uiso calc 1
C C22 1.1323(2) -0.53858(13) 0.12588(12) 0.0414(4) Uani d 1
C C23 1.0451(2) -0.61035(13) 0.12862(13) 0.0470(4) Uani d 1
H H23 0.9485 -0.6164 0.1678 0.056 Uiso calc 1
C C24 1.1016(2) -0.67331(15) 0.07298(14) 0.0534(5) Uani d 1
H H24 1.0446 -0.7226 0.0747 0.064 Uiso calc 1
C C25 0.9663(3) -0.58167(13) 0.34081(14) 0.0547(5) Uani d 1
H H25A 0.8549 -0.5847 0.3290 0.082 Uiso calc 1
H H25B 0.9730 -0.5846 0.4076 0.082 Uiso calc 1
H H25C 1.0483 -0.6400 0.3318 0.082 Uiso calc 1
C C26 1.0016(2) -0.48221(13) 0.26976(12) 0.0413(4) Uani d 1
C C27 0.9802(2) -0.38655(13) 0.27927(13) 0.0463(4) Uani d 1
C C28 0.9078(2) -0.35116(13) 0.36098(13) 0.0478(4) Uani d 1
C C29 0.9169(3) -0.24485(14) 0.34965(14) 0.0526(4) Uani d 1
H H29 0.9774 -0.2092 0.2962 0.063 Uiso calc 1
C C30 0.8435(2) -0.19792(14) 0.41170(13) 0.0494(4) Uani d 1
H H30 0.7826 -0.2348 0.4641 0.059 Uiso calc 1
C C31 0.8486(2) -0.09345(13) 0.40616(13) 0.0468(4) Uani d 1
C C32 0.9495(3) -0.03399(15) 0.33795(15) 0.0558(5) Uani d 1
H H32 1.0171 -0.0611 0.2938 0.067 Uiso calc 1
C C33 0.9505(3) 0.06391(16) 0.33501(16) 0.0609(5) Uani d 1
H H33 1.0179 0.1031 0.2895 0.073 Uiso calc 1
C C34 0.8501(3) 0.10242(14) 0.40055(16) 0.0572(5) Uani d 1
C C35 0.7489(3) 0.04812(15) 0.46811(16) 0.0614(5) Uani d 1
H H35 0.6812 0.0765 0.5114 0.074 Uiso calc 1
C C36 0.7492(3) -0.05020(14) 0.47070(14) 0.0556(5) Uani d 1
H H36 0.6811 -0.0884 0.5168 0.067 Uiso calc 1
N N1 0.34173(18) -0.17422(11) -0.13693(11) 0.0452(3) Uani d 1
N N2 0.2574(2) -0.25153(13) -0.11516(13) 0.0586(4) Uani d 1
N N3 0.3186(2) -0.30441(12) -0.17205(12) 0.0549(4) Uani d 1
N N4 1.07488(19) -0.46919(11) 0.17951(10) 0.0453(3) Uani d 1
N N5 1.0991(2) -0.36974(12) 0.13550(11) 0.0628(5) Uani d 1
N N6 1.0419(2) -0.32099(12) 0.19610(12) 0.0606(4) Uani d 1
O O1 0.62385(19) -0.26083(11) -0.36626(10) 0.0658(4) Uani d 1
O O2 0.84447(19) -0.40717(10) 0.43345(10) 0.0636(4) Uani d 1
F F1 0.1592(2) 0.07284(11) 0.09065(10) 0.0896(4) Uani d 1
F F2 0.5683(2) -0.85579(10) -0.33684(12) 0.0940(5) Uani d 1
F F3 1.29847(17) -0.72282(11) -0.04006(10) 0.0808(4) Uani d 1
F F4 0.85150(19) 0.19891(9) 0.39781(11) 0.0828(4) Uani d 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0705(13) 0.0620(12) 0.0615(12) -0.0169(10) 0.0053(10) -0.0377(11)
C2 0.0948(16) 0.0473(11) 0.0667(13) -0.0239(11) 0.0071(12) -0.0275(10)
C3 0.0817(14) 0.0459(10) 0.0473(10) -0.0225(10) 0.0058(10) -0.0167(9)
C4 0.0502(10) 0.0429(9) 0.0470(10) -0.0160(7) 0.0068(8) -0.0202(8)
C5 0.0767(14) 0.0467(10) 0.0513(11) -0.0178(9) 0.0158(10) -0.0177(9)
C6 0.0807(15) 0.0627(13) 0.0494(11) -0.0168(11) 0.0130(10) -0.0232(10)
C7 0.0626(12) 0.0536(11) 0.0584(11) -0.0315(9) 0.0137(9) -0.0214(9)
C8 0.0446(9) 0.0378(8) 0.0396(8) -0.0150(7) 0.0058(7) -0.0119(7)
C9 0.0486(10) 0.0383(9) 0.0441(9) -0.0165(7) 0.0061(7) -0.0135(7)
C10 0.0508(10) 0.0415(9) 0.0459(9) -0.0147(8) 0.0056(8) -0.0154(8)
C11 0.0548(10) 0.0448(10) 0.0503(10) -0.0186(8) 0.0080(8) -0.0201(8)
C12 0.0534(10) 0.0427(9) 0.0441(9) -0.0136(8) 0.0024(8) -0.0154(8)
C13 0.0494(10) 0.0434(9) 0.0434(9) -0.0112(7) 0.0010(8) -0.0167(8)
C14 0.0694(13) 0.0512(11) 0.0520(11) -0.0205(9) 0.0122(9) -0.0222(9)
C15 0.0754(14) 0.0521(11) 0.0656(13) -0.0279(10) 0.0132(11) -0.0191(10)
C16 0.0702(13) 0.0431(10) 0.0762(14) -0.0150(9) -0.0031(11) -0.0260(10)
C17 0.0777(14) 0.0532(11) 0.0676(13) -0.0141(10) 0.0098(11) -0.0339(11)
C18 0.0654(12) 0.0490(10) 0.0509(10) -0.0154(9) 0.0099(9) -0.0205(9)
C19 0.0542(11) 0.0545(11) 0.0509(10) -0.0130(9) 0.0063(9) -0.0260(9)
C20 0.0556(11) 0.0835(15) 0.0582(12) -0.0335(11) 0.0210(9) -0.0338(11)
C21 0.0649(12) 0.0717(13) 0.0562(11) -0.0410(10) 0.0155(10) -0.0293(10)
C22 0.0491(9) 0.0405(9) 0.0368(8) -0.0168(7) 0.0013(7) -0.0127(7)
C23 0.0494(10) 0.0464(10) 0.0497(10) -0.0193(8) 0.0099(8) -0.0197(8)
C24 0.0593(11) 0.0508(10) 0.0608(11) -0.0248(9) 0.0106(9) -0.0272(9)
C25 0.0724(13) 0.0399(9) 0.0494(10) -0.0208(9) 0.0156(9) -0.0126(8)
C26 0.0470(9) 0.0380(9) 0.0384(8) -0.0143(7) 0.0024(7) -0.0112(7)
C27 0.0602(11) 0.0378(9) 0.0424(9) -0.0185(8) 0.0013(8) -0.0121(7)
C28 0.0579(11) 0.0399(9) 0.0460(10) -0.0137(8) 0.0012(8) -0.0151(8)
C29 0.0681(12) 0.0442(10) 0.0484(10) -0.0203(9) 0.0048(9) -0.0167(8)
C30 0.0587(11) 0.0440(10) 0.0459(10) -0.0146(8) 0.0020(8) -0.0159(8)
C31 0.0558(10) 0.0409(9) 0.0444(9) -0.0111(8) -0.0017(8) -0.0163(8)
C32 0.0642(12) 0.0547(11) 0.0561(11) -0.0203(9) 0.0095(9) -0.0271(9)
C33 0.0696(13) 0.0536(11) 0.0655(13) -0.0276(10) 0.0049(10) -0.0211(10)
C34 0.0723(13) 0.0405(10) 0.0627(12) -0.0126(9) -0.0131(10) -0.0205(9)
C35 0.0789(14) 0.0496(11) 0.0587(12) -0.0101(10) 0.0024(10) -0.0275(10)
C36 0.0706(13) 0.0474(10) 0.0488(10) -0.0163(9) 0.0077(9) -0.0184(9)
N1 0.0529(8) 0.0399(7) 0.0481(8) -0.0206(6) 0.0114(7) -0.0185(7)
N2 0.0677(10) 0.0558(9) 0.0683(10) -0.0358(8) 0.0276(8) -0.0333(9)
N3 0.0636(10) 0.0495(9) 0.0645(10) -0.0296(7) 0.0232(8) -0.0301(8)
N4 0.0620(9) 0.0388(7) 0.0398(7) -0.0238(7) 0.0061(7) -0.0132(6)
N5 0.1073(14) 0.0463(9) 0.0442(9) -0.0409(9) 0.0165(9) -0.0161(7)
N6 0.0997(13) 0.0444(9) 0.0451(9) -0.0340(9) 0.0108(9) -0.0162(7)
O1 0.0836(10) 0.0560(8) 0.0648(9) -0.0332(7) 0.0338(8) -0.0273(7)
O2 0.0879(10) 0.0489(8) 0.0548(8) -0.0250(7) 0.0209(7) -0.0193(7)
F1 0.1226(12) 0.0847(9) 0.0852(9) -0.0274(8) 0.0181(8) -0.0605(8)
F2 0.1197(12) 0.0538(7) 0.1244(12) -0.0332(8) 0.0155(9) -0.0458(8)
F3 0.0878(9) 0.0880(9) 0.0915(9) -0.0308(7) 0.0328(7) -0.0623(8)
F4 0.1129(11) 0.0499(7) 0.0981(10) -0.0264(7) -0.0075(8) -0.0345(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
F1 C1 C6 118.35(19)
F1 C1 C2 118.77(19)
C6 C1 C2 122.86(18)
C1 C2 C3 118.45(19)
C1 C2 H2 120.8
C3 C2 H2 120.8
C4 C3 C2 119.59(18)
C4 C3 H3 120.2
C2 C3 H3 120.2
C5 C4 C3 120.70(17)
C5 C4 N1 117.69(15)
C3 C4 N1 121.52(16)
C4 C5 C6 119.75(18)
C4 C5 H5 120.1
C6 C5 H5 120.1
C1 C6 C5 118.65(19)
C1 C6 H6 120.7
C5 C6 H6 120.7
C8 C7 H7A 109.5
C8 C7 H7B 109.5
H7A C7 H7B 109.5
C8 C7 H7C 109.5
H7A C7 H7C 109.5
H7B C7 H7C 109.5
N1 C8 C9 103.99(14)
N1 C8 C7 124.74(15)
C9 C8 C7 131.19(15)
N3 C9 C8 109.02(15)
N3 C9 C10 120.88(15)
C8 C9 C10 130.09(15)
O1 C10 C9 120.54(15)
O1 C10 C11 122.96(16)
C9 C10 C11 116.48(15)
C12 C11 C10 122.81(16)
C12 C11 H11 118.6
C10 C11 H11 118.6
C11 C12 C13 126.70(17)
C11 C12 H12 116.7
C13 C12 H12 116.7
C18 C13 C14 117.89(16)
C18 C13 C12 119.41(16)
C14 C13 C12 122.69(16)
C15 C14 C13 121.32(18)
C15 C14 H14 119.3
C13 C14 H14 119.3
C16 C15 C14 118.13(19)
C16 C15 H15 120.9
C14 C15 H15 120.9
C17 C16 F2 119.13(19)
C17 C16 C15 122.97(18)
F2 C16 C15 117.90(19)
C16 C17 C18 118.12(19)
C16 C17 H17 120.9
C18 C17 H17 120.9
C17 C18 C13 121.57(18)
C17 C18 H18 119.2
C13 C18 H18 119.2
C20 C19 F3 118.33(16)
C20 C19 C24 122.52(17)
F3 C19 C24 119.15(17)
C19 C20 C21 119.01(17)
C19 C20 H20 120.5
C21 C20 H20 120.5
C20 C21 C22 119.83(17)
C20 C21 H21 120.1
C22 C21 H21 120.1
C23 C22 C21 120.20(16)
C23 C22 N4 121.59(15)
C21 C22 N4 118.11(15)
C22 C23 C24 119.75(16)
C22 C23 H23 120.1
C24 C23 H23 120.1
C19 C24 C23 118.68(17)
C19 C24 H24 120.7
C23 C24 H24 120.7
C26 C25 H25A 109.5
C26 C25 H25B 109.5
H25A C25 H25B 109.5
C26 C25 H25C 109.5
H25A C25 H25C 109.5
H25B C25 H25C 109.5
N4 C26 C27 103.98(14)
N4 C26 C25 125.31(15)
C27 C26 C25 130.60(16)
N6 C27 C26 108.92(15)
N6 C27 C28 120.75(15)
C26 C27 C28 130.32(15)
O2 C28 C27 121.35(15)
O2 C28 C29 122.77(17)
C27 C28 C29 115.88(15)
C30 C29 C28 123.18(17)
C30 C29 H29 118.4
C28 C29 H29 118.4
C29 C30 C31 126.38(17)
C29 C30 H30 116.8
C31 C30 H30 116.8
C36 C31 C32 117.71(16)
C36 C31 C30 119.36(16)
C32 C31 C30 122.93(16)
C33 C32 C31 121.17(18)
C33 C32 H32 119.4
C31 C32 H32 119.4
C34 C33 C32 118.52(19)
C34 C33 H33 120.7
C32 C33 H33 120.7
F4 C34 C35 118.76(19)
F4 C34 C33 118.50(19)
C35 C34 C33 122.74(17)
C34 C35 C36 118.30(19)
C34 C35 H35 120.8
C36 C35 H35 120.8
C35 C36 C31 121.56(18)
C35 C36 H36 119.2
C31 C36 H36 119.2
C8 N1 N2 110.51(13)
C8 N1 C4 132.05(14)
N2 N1 C4 117.40(13)
N3 N2 N1 107.40(13)
N2 N3 C9 109.07(14)
C26 N4 N5 110.53(14)
C26 N4 C22 132.38(14)
N5 N4 C22 117.07(13)
N6 N5 N4 107.30(13)
N5 N6 C27 109.27(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 F1 1.359(2)
C1 C6 1.362(3)
C1 C2 1.364(3)
C2 C3 1.385(3)
C2 H2 0.9300
C3 C4 1.377(2)
C3 H3 0.9300
C4 C5 1.376(3)
C4 N1 1.430(2)
C5 C6 1.379(3)
C5 H5 0.9300
C6 H6 0.9300
C7 C8 1.488(2)
C7 H7A 0.9600
C7 H7B 0.9600
C7 H7C 0.9600
C8 N1 1.353(2)
C8 C9 1.375(2)
C9 N3 1.365(2)
C9 C10 1.465(2)
C10 O1 1.222(2)
C10 C11 1.471(2)
C11 C12 1.324(2)
C11 H11 0.9300
C12 C13 1.460(2)
C12 H12 0.9300
C13 C18 1.387(2)
C13 C14 1.392(2)
C14 C15 1.378(3)
C14 H14 0.9300
C15 C16 1.371(3)
C15 H15 0.9300
C16 C17 1.360(3)
C16 F2 1.362(2)
C17 C18 1.380(3)
C17 H17 0.9300
C18 H18 0.9300
C19 C20 1.355(3)
C19 F3 1.358(2)
C19 C24 1.363(3)
C20 C21 1.376(3)
C20 H20 0.9300
C21 C22 1.378(2)
C21 H21 0.9300
C22 C23 1.377(2)
C22 N4 1.431(2)
C23 C24 1.381(2)
C23 H23 0.9300
C24 H24 0.9300
C25 C26 1.485(2)
C25 H25A 0.9600
C25 H25B 0.9600
C25 H25C 0.9600
C26 N4 1.352(2)
C26 C27 1.378(2)
C27 N6 1.365(2)
C27 C28 1.467(2)
C28 O2 1.220(2)
C28 C29 1.476(2)
C29 C30 1.319(2)
C29 H29 0.9300
C30 C31 1.465(2)
C30 H30 0.9300
C31 C36 1.388(2)
C31 C32 1.398(3)
C32 C33 1.375(3)
C32 H32 0.9300
C33 C34 1.367(3)
C33 H33 0.9300
C34 F4 1.357(2)
C34 C35 1.361(3)
C35 C36 1.380(3)
C35 H35 0.9300
C36 H36 0.9300
N1 N2 1.3701(19)
N2 N3 1.294(2)
N4 N5 1.3735(19)
N5 N6 1.292(2)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C24 H24 F1 1_645 0.93 2.73 3.418(2) 132
C35 H35 F2 1_566 0.93 2.70 3.608(2) 164
C2 H2 F3 1_465 0.93 2.65 3.395(2) 137
C17 H17 F4 1_544 0.93 2.62 3.546(2) 178
_cod_database_fobs_code 1548682