#------------------------------------------------------------------------------
#$Date: 2019-07-10 07:34:45 +0300 (Wed, 10 Jul 2019) $
#$Revision: 216919 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021724.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_2021724
loop_
_publ_author_name
'Palanisamy, Vasanthi'
'Sanphui, Palash'
'Prakash, Muthuramalingam'
'Chernyshev, Vladimir'
_publ_section_title
;
Multicomponent solid forms of the uric acid reabsorption inhibitor
lesinurad and cocrystal polymorphs with urea: DFT simulation and
solubility study
;
_journal_coeditor_code CU3152
_journal_issue 8
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229619008829
_journal_volume 75
_journal_year 2019
_chemical_formula_iupac 'C17 H14 Br N3 O2 S, C H4 N2 O'
_chemical_formula_moiety 'C17 H14 Br N3 O2 S, C H4 N2 O'
_chemical_formula_sum 'C18 H18 Br N5 O3 S'
_chemical_formula_weight 464.35
_chemical_name_common 'Lesinurad--urea (1/1)'
_chemical_name_systematic
;
2-{[5-Bromo-4-(4-cyclopropylnaphthalen-1-yl)-4H-1,2,4-triazol-\
3-yl]sulfanyl}acetic acid--urea (1/1)
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 90
_cell_angle_beta 103.193(4)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 10.9993(5)
_cell_length_b 15.2290(5)
_cell_length_c 24.0797(10)
_cell_measurement_reflns_used 4931
_cell_measurement_temperature 150.00(10)
_cell_measurement_theta_max 23.4870
_cell_measurement_theta_min 3.7100
_cell_volume 3927.1(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
olex2.refine (Bourhis et al., 2015)
;
_diffrn_ambient_temperature 150.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 8.0419
_diffrn_measured_fraction_theta_full 0.9973
_diffrn_measured_fraction_theta_max 0.9973
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Eos, Nova'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0930
_diffrn_reflns_av_unetI/netI 0.1116
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_number 33889
_diffrn_reflns_theta_full 27.4837
_diffrn_reflns_theta_max 27.48
_diffrn_reflns_theta_min 3.48
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 2.230
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.71544
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Rigaku OD, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.5706
_exptl_crystal_description needle
_exptl_crystal_F_000 1887.4843
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.10
_refine_diff_density_max 2.1798
_refine_diff_density_min -1.2896
_refine_ls_goodness_of_fit_ref 1.0493
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_constraints 62
_refine_ls_number_parameters 509
_refine_ls_number_reflns 8975
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.0493
_refine_ls_R_factor_all 0.1135
_refine_ls_R_factor_gt 0.0645
_refine_ls_shift/su_max 0.0022
_refine_ls_shift/su_mean 0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+2.5686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1086
_refine_ls_wR_factor_ref 0.1317
_reflns_number_gt 5645
_reflns_number_total 8975
_reflns_threshold_expression I>=2u(I)
_iucr_refine_instructions_details
;
TITL RED1 in P2(1)/c
CELL 0.71073 10.9993 15.229 24.0797 90 103.193 90
ZERR 8 0.0005 0.0005 0.001 0 0.004 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Br N O S
UNIT 144 144 8 40 24 8
L.S. 10
PLAN 20
BOND
fmap 2
acta
MERG 2
WGHT 0.031182 2.568618
FVAR 1.577124
REM
REM
REM
C1 1 -0.10449 0.10329 0.50006 11.00000 0.02237 0.02688 0.03310 =
0.01691 0.00673 0.00296
C2 1 0.03103 0.18854 0.55369 11.00000 0.03027 0.02775 0.02408 =
0.01272 0.00461 0.00852
C3 1 0.20477 0.24314 0.64677 11.00000 0.03251 0.04050 0.02787 =
0.00117 0.00610 0.00314
AFIX 23
H3a 2 0.13181 0.24044 0.66298 11.00000 -1.20000
H3b 2 0.25624 0.29172 0.66458 11.00000 -1.20000
AFIX 0
C4 1 0.27787 0.15846 0.65988 11.00000 0.02061 0.04069 0.02121 =
0.00562 -0.00015 0.00487
C5 1 0.02970 0.19424 0.44944 11.00000 0.02079 0.02256 0.02475 =
0.00369 0.00532 -0.00837
C6 1 0.08985 0.13784 0.42085 11.00000 0.03818 0.01402 0.04163 =
0.00498 0.01815 -0.00003
AFIX 43
H6 2 0.10290 0.07989 0.43291 11.00000 -1.20000
AFIX 0
C7 1 0.13199 0.16684 0.37344 11.00000 0.03490 0.02603 0.03769 =
0.00225 0.02158 0.00132
AFIX 43
H7 2 0.16936 0.12701 0.35324 11.00000 -1.20000
AFIX 0
C8 1 0.11937 0.25286 0.35610 11.00000 0.03595 0.02659 0.02377 =
0.00009 0.01270 -0.00420
C9 1 0.05626 0.31285 0.38532 11.00000 0.02342 0.02291 0.02720 =
0.00530 0.00948 -0.00497
C10 1 0.00766 0.28314 0.43232 11.00000 0.01604 0.02162 0.02068 =
0.00512 -0.00041 0.00082
C11 1 -0.05741 0.34290 0.45985 11.00000 0.01763 0.02775 0.02625 =
0.00651 0.00467 -0.00436
AFIX 43
H11 2 -0.09167 0.32352 0.48958 11.00000 -1.20000
AFIX 0
C12 1 -0.07061 0.42919 0.44320 11.00000 0.02691 0.03192 0.02918 =
-0.00152 0.00656 0.00190
AFIX 43
H12 2 -0.11336 0.46787 0.46180 11.00000 -1.20000
AFIX 0
C13 1 -0.02018 0.45927 0.39846 11.00000 0.03249 0.01995 0.03896 =
0.01029 0.00656 0.00215
AFIX 43
H13 2 -0.02781 0.51815 0.38802 11.00000 -1.20000
AFIX 0
C14 1 0.04047 0.40242 0.36989 11.00000 0.03532 0.02704 0.03210 =
0.00673 0.01274 -0.00141
AFIX 43
H14 2 0.07195 0.42322 0.33967 11.00000 -1.20000
AFIX 0
C15 1 0.17412 0.28544 0.30847 11.00000 0.03870 0.04176 0.03230 =
0.00930 0.01820 0.00784
AFIX 13
H15 2 0.11483 0.31003 0.27547 11.00000 -1.20000
AFIX 0
C16 1 0.28603 0.24099 0.29615 11.00000 0.04448 0.05190 0.03032 =
0.00972 0.02156 0.00891
AFIX 23
H16a 2 0.31945 0.19063 0.31932 11.00000 -1.20000
H16b 2 0.29256 0.23783 0.25670 11.00000 -1.20000
AFIX 0
C17 1 0.29908 0.32894 0.32412 11.00000 0.06345 0.04341 0.06436 =
0.01108 0.03144 -0.00220
AFIX 23
H17a 2 0.31346 0.37908 0.30161 11.00000 -1.20000
H17b 2 0.34036 0.33188 0.36423 11.00000 -1.20000
AFIX 0
C21 1 0.43017 0.39897 0.54182 11.00000 0.02496 0.02656 0.02145 =
-0.00140 0.00979 0.00013
C22 1 0.61342 0.35687 0.58664 11.00000 0.02964 0.02764 0.01903 =
-0.00399 0.00795 -0.00180
C23 1 0.80351 0.29903 0.67225 11.00000 0.02833 0.02777 0.02857 =
0.00122 0.00771 -0.00220
AFIX 23
H23a 2 0.85314 0.24646 0.68289 11.00000 -1.20000
H23b 2 0.72895 0.29394 0.68713 11.00000 -1.20000
AFIX 0
C24 1 0.87792 0.37854 0.69850 11.00000 0.02565 0.03138 0.01510 =
0.00468 0.00308 0.00170
C25 1 0.55545 0.31683 0.48275 11.00000 0.01845 0.02194 0.01869 =
-0.00524 0.00445 -0.00130
C26 1 0.61439 0.35849 0.44673 11.00000 0.03019 0.02016 0.03302 =
-0.00662 0.01055 -0.00486
AFIX 43
H26 2 0.64284 0.41576 0.45417 11.00000 -1.20000
AFIX 0
C27 1 0.63209 0.31439 0.39807 11.00000 0.03174 0.03075 0.01884 =
-0.00004 0.01243 -0.00795
AFIX 43
H27 2 0.67357 0.34330 0.37381 11.00000 -1.20000
AFIX 0
C28 1 0.59066 0.23025 0.38480 11.00000 0.01762 0.02561 0.01738 =
-0.00361 0.00356 -0.00032
C29 1 0.52560 0.18649 0.42229 11.00000 0.02027 0.02091 0.01665 =
-0.00422 0.00312 0.00125
C30 1 0.50808 0.22975 0.47223 11.00000 0.01736 0.01788 0.01898 =
-0.00361 0.00199 0.00020
C31 1 0.44529 0.18691 0.50923 11.00000 0.03301 0.02968 0.02145 =
-0.00197 0.00963 -0.00207
AFIX 43
H31 2 0.43608 0.21508 0.54229 11.00000 -1.20000
AFIX 0
C32 1 0.39780 0.10469 0.49726 11.00000 0.04541 0.03194 0.03819 =
0.00626 0.01586 -0.01116
AFIX 43
H32 2 0.35588 0.07707 0.52186 11.00000 -1.20000
AFIX 0
C33 1 0.41246 0.06192 0.44764 11.00000 0.04325 0.01792 0.04285 =
-0.00442 0.00826 -0.00595
AFIX 43
H33 2 0.37871 0.00618 0.43926 11.00000 -1.20000
AFIX 0
C34 1 0.47522 0.10055 0.41153 11.00000 0.03836 0.02383 0.02180 =
-0.00269 0.01098 -0.00231
AFIX 43
H34 2 0.48530 0.07028 0.37934 11.00000 -1.20000
AFIX 0
C35 1 0.61063 0.18711 0.33281 11.00000 0.03697 0.03507 0.01760 =
-0.01049 0.00947 -0.00019
AFIX 13
H35 2 0.58068 0.12638 0.32770 11.00000 -1.20000
AFIX 0
C36 1 0.72628 0.20525 0.31125 11.00000 0.03840 0.05612 0.02592 =
-0.01575 0.01480 -0.00118
AFIX 23
H36a 2 0.78457 0.24859 0.33145 11.00000 -1.20000
H36b 2 0.76439 0.15639 0.29571 11.00000 -1.20000
AFIX 0
C37 1 0.60265 0.23681 0.27842 11.00000 0.04830 0.03963 0.01937 =
-0.00532 0.00743 0.00351
AFIX 23
H37a 2 0.56582 0.20718 0.24291 11.00000 -1.20000
H37b 2 0.58600 0.29935 0.27863 11.00000 -1.20000
AFIX 0
C40 1 0.52872 0.49463 0.25027 11.00000 0.02376 0.01831 0.01990 =
0.00147 0.00982 -0.00064
N1 4 -0.11917 0.09354 0.55236 11.00000 0.02694 0.03880 0.04040 =
0.02270 0.01620 0.00911
N2 4 -0.02959 0.14913 0.58705 11.00000 0.03615 0.03609 0.03238 =
0.00848 0.01516 0.00907
N3 4 -0.01312 0.16368 0.49808 11.00000 0.02590 0.02497 0.02350 =
0.00902 0.00602 0.00210
N4 4 0.55968 0.39232 0.62437 11.00000 0.02376 0.03439 0.02687 =
-0.00793 0.00679 0.00093
N5 4 0.43919 0.41910 0.59548 11.00000 0.02724 0.02828 0.02821 =
-0.00536 0.00923 0.00122
N6 4 0.53669 0.36034 0.53353 11.00000 0.02464 0.02332 0.01925 =
-0.00444 0.00435 0.00116
N11 4 0.63138 0.51558 0.29063 11.00000 0.02482 0.04595 0.02796 =
-0.01134 0.00970 -0.00738
AFIX 7
H11a 2 0.68262 0.54490 0.27547 11.00000 -1.20000
H11b 2 0.60886 0.54778 0.31602 11.00000 -1.20000
AFIX 0
N12 4 0.41747 0.50963 0.26117 11.00000 0.02446 0.03057 0.02295 =
-0.00381 0.01030 -0.00129
AFIX 93
H12a 2 0.41224 0.53215 0.29330 11.00000 -1.20000
H12b 2 0.35069 0.49683 0.23611 11.00000 -1.20000
AFIX 0
O1 5 0.23286 0.09126 0.67171 11.00000 0.02342 0.03835 0.05868 =
0.01930 0.01021 -0.00237
O2 5 0.39675 0.16737 0.65853 11.00000 0.02843 0.03502 0.04905 =
0.00959 0.00912 0.00199
AFIX 147
H2 2 0.43217 0.11986 0.66516 11.00000 -1.50000
AFIX 0
O3 5 0.99782 0.37013 0.70006 11.00000 0.02438 0.03448 0.03542 =
-0.01167 0.00610 -0.00202
AFIX 147
H3 2 1.03654 0.41022 0.71893 11.00000 -1.50000
AFIX 0
O4 5 0.83080 0.44117 0.71645 11.00000 0.02106 0.03005 0.04237 =
-0.00963 0.01325 0.00056
O5 5 0.53922 0.46065 0.20385 11.00000 0.02350 0.02610 0.02158 =
-0.00608 0.00916 -0.00447
S2 6 0.75922 0.30727 0.59523 11.00000 0.02553 0.04529 0.02394 =
-0.00955 0.00484 0.00528
Br2 3 0.29317 0.41848 0.48198 11.00000 0.02512 0.03039 0.03016 =
-0.00836 0.00362 0.00164
Br1 3 -0.18605 0.04226 0.43618 11.00000 0.03269 0.03354 0.04330 =
0.01186 0.00034 -0.01120
C41 1 0.12198 -0.03284 0.29262 11.00000 0.02298 0.02061 0.02059 =
0.00208 0.00305 -0.00712
N13 4 0.22248 -0.06606 0.32990 11.00000 0.03543 0.02956 0.02470 =
0.00525 0.00750 0.00355
AFIX 7
H13a 2 0.20164 -0.07858 0.36136 11.00000 -1.20000
H13b 2 0.24632 -0.11319 0.31566 11.00000 -1.20000
AFIX 0
N14 4 0.00954 -0.04346 0.30283 11.00000 0.02198 0.04935 0.02465 =
0.01390 0.00531 -0.00314
AFIX 93
H14a 2 0.00113 -0.07118 0.33285 11.00000 -1.20000
H14b 2 -0.05504 -0.02264 0.27944 11.00000 -1.20000
AFIX 0
O6 5 0.13806 0.00783 0.24932 11.00000 0.01987 0.03473 0.02621 =
0.00750 0.01130 0.00087
S1 6 0.15579 0.26295 0.57135 11.00000 0.03764 0.03713 0.02778 =
0.00754 0.00160 -0.00475
HKLF 4
END
Q1 1 0.083333 0.26 0.6 11 0.05 2.18
Q2 1 0.305556 0.42 0.4875 11 0.05 1.26
Q3 1 -0.194444 0.04 0.4375 11 0.05 1.24
Q4 1 0.166667 0.26 0.575 11 0.05 1.08
Q5 1 -0.138889 0.02 0.4 11 0.05 0.91
Q6 1 0.388889 0.56 0.225 11 0.05 0.91
Q7 1 0.888889 0.2 0.7625 11 0.05 0.88
Q8 1 0.25 0.22 0.25 11 0.05 0.88
Q9 1 0.111111 0.28 0.275 11 0.05 0.85
Q10 1 0.722222 0.52 0.2875 11 0.05 0.84
Q11 1 0.5 0.3 0.3125 11 0.05 0.81
Q12 1 -0.166667 0.08 0.475 11 0.05 0.8
Q13 1 0.444444 0.56 0.625 11 0.05 0.8
Q14 1 0 0 0.3 11 0.05 0.8
Q15 1 0.638889 0.28 0.4125 11 0.05 0.8
Q16 1 1 0.38 0.7125 11 0.05 0.79
Q17 1 0.166667 0.28 0.4 11 0.05 0.79
Q18 1 -0.055556 0.2 0.6 11 0.05 0.79
Q19 1 0.694444 0.38 0.6875 11 0.05 0.78
Q20 1 -0.083333 0.44 0.4 11 0.05 0.78
REM The information below was added by Olex2.
REM
REM R1 = 0.0645 for 5645 Fo > 4sig(Fo) and 0.1135 for all 8975 data
REM 509 parameters refined using 0 restraints
REM Highest difference peak 2.1798, deepest hole -1.2896
REM Mean Shift 0.0000, Max Shift 0.0022.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.1135
REM R1_gt = 0.0645
REM wR_ref = 0.1317
REM GOOF = 1.0493
REM Shift_max = 0.0022
REM Shift_mean = 0.0000
REM Reflections_all = 8975
REM Reflections_gt = 5645
REM Parameters = 509
REM Hole = -1.2896
REM Peak = 2.1798
REM Flack = n/a
;
_cod_data_source_file cu3152sup1.cif
_cod_data_source_block LESUREFormII
_cod_database_code 2021724
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2
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_occupancy
C C1 -0.1045(5) 0.1033(3) 0.5001(2) 0.0274(12) Uani 1.000000
C C2 0.0310(5) 0.1885(3) 0.5537(2) 0.0276(12) Uani 1.000000
C C3 0.2048(5) 0.2431(3) 0.6468(2) 0.0338(13) Uani 1.000000
H H3a 0.1318(5) 0.2404(3) 0.6630(2) 0.0405(15) Uiso 1.000000
H H3b 0.2562(5) 0.2917(3) 0.6646(2) 0.0405(15) Uiso 1.000000
C C4 0.2779(5) 0.1585(3) 0.6599(2) 0.0283(12) Uani 1.000000
C C5 0.0297(4) 0.1942(3) 0.44944(19) 0.0227(11) Uani 1.000000
C C6 0.0898(5) 0.1378(3) 0.4208(2) 0.0298(12) Uani 1.000000
H H6 0.1029(5) 0.0799(3) 0.4329(2) 0.0358(15) Uiso 1.000000
C C7 0.1320(5) 0.1668(3) 0.3734(2) 0.0307(12) Uani 1.000000
H H7 0.1694(5) 0.1270(3) 0.3532(2) 0.0369(14) Uiso 1.000000
C C8 0.1194(5) 0.2529(3) 0.3561(2) 0.0278(12) Uani 1.000000
C C9 0.0563(4) 0.3129(3) 0.3853(2) 0.0239(11) Uani 1.000000
C C10 0.0077(4) 0.2831(3) 0.43232(18) 0.0202(10) Uani 1.000000
C C11 -0.0574(4) 0.3429(3) 0.4598(2) 0.0239(11) Uani 1.000000
H H11 -0.0917(4) 0.3235(3) 0.4896(2) 0.0287(13) Uiso 1.000000
C C12 -0.0706(5) 0.4292(3) 0.4432(2) 0.0293(12) Uani 1.000000
H H12 -0.1134(5) 0.4679(3) 0.4618(2) 0.0352(14) Uiso 1.000000
C C13 -0.0202(5) 0.4593(3) 0.3985(2) 0.0307(12) Uani 1.000000
H H13 -0.0278(5) 0.5182(3) 0.3880(2) 0.0369(15) Uiso 1.000000
C C14 0.0405(5) 0.4024(3) 0.3699(2) 0.0307(12) Uani 1.000000
H H14 0.0720(5) 0.4232(3) 0.3397(2) 0.0368(15) Uiso 1.000000
C C15 0.1741(5) 0.2854(3) 0.3085(2) 0.0360(13) Uani 1.000000
H H15 0.1148(5) 0.3100(3) 0.2755(2) 0.0432(16) Uiso 1.000000
C C16 0.2860(5) 0.2410(3) 0.2962(2) 0.0401(14) Uani 1.000000
H H16a 0.3195(5) 0.1906(3) 0.3193(2) 0.0482(17) Uiso 1.000000
H H16b 0.2926(5) 0.2378(3) 0.2567(2) 0.0482(17) Uiso 1.000000
C C17 0.2991(6) 0.3289(4) 0.3241(3) 0.0544(17) Uani 1.000000
H H17a 0.3135(6) 0.3791(4) 0.3016(3) 0.065(2) Uiso 1.000000
H H17b 0.3404(6) 0.3319(4) 0.3642(3) 0.065(2) Uiso 1.000000
C C21 0.4302(5) 0.3990(3) 0.54182(19) 0.0236(11) Uani 1.000000
C C22 0.6134(5) 0.3569(3) 0.58664(19) 0.0251(11) Uani 1.000000
C C23 0.8035(5) 0.2990(3) 0.67225(19) 0.0280(12) Uani 1.000000
H H23a 0.8531(5) 0.2465(3) 0.68289(19) 0.0336(14) Uiso 1.000000
H H23b 0.7290(5) 0.2939(3) 0.68713(19) 0.0336(14) Uiso 1.000000
C C24 0.8779(5) 0.3785(3) 0.69850(19) 0.0243(11) Uani 1.000000
C C25 0.5555(4) 0.3168(3) 0.48275(18) 0.0197(10) Uani 1.000000
C C26 0.6144(5) 0.3585(3) 0.4467(2) 0.0273(11) Uani 1.000000
H H26 0.6428(5) 0.4158(3) 0.4542(2) 0.0327(14) Uiso 1.000000
C C27 0.6321(5) 0.3144(3) 0.39807(19) 0.0260(11) Uani 1.000000
H H27 0.6736(5) 0.3433(3) 0.37381(19) 0.0312(13) Uiso 1.000000
C C28 0.5907(4) 0.2303(3) 0.38480(18) 0.0203(10) Uani 1.000000
C C29 0.5256(4) 0.1865(3) 0.42229(18) 0.0195(10) Uani 1.000000
C C30 0.5081(4) 0.2298(3) 0.47223(18) 0.0184(10) Uani 1.000000
C C31 0.4453(5) 0.1869(3) 0.50923(19) 0.0275(11) Uani 1.000000
H H31 0.4361(5) 0.2151(3) 0.54229(19) 0.0330(14) Uiso 1.000000
C C32 0.3978(5) 0.1047(3) 0.4973(2) 0.0375(14) Uani 1.000000
H H32 0.3559(5) 0.0771(3) 0.5219(2) 0.0450(16) Uiso 1.000000
C C33 0.4125(5) 0.0619(3) 0.4476(2) 0.0349(13) Uani 1.000000
H H33 0.3787(5) 0.0062(3) 0.4393(2) 0.0419(16) Uiso 1.000000
C C34 0.4752(5) 0.1005(3) 0.41153(19) 0.0273(12) Uani 1.000000
H H34 0.4853(5) 0.0703(3) 0.37934(19) 0.0328(14) Uiso 1.000000
C C35 0.6106(5) 0.1871(3) 0.33281(19) 0.0294(12) Uani 1.000000
H H35 0.5807(5) 0.1264(3) 0.32770(19) 0.0352(14) Uiso 1.000000
C C36 0.7263(5) 0.2052(4) 0.3112(2) 0.0389(14) Uani 1.000000
H H36a 0.7846(5) 0.2486(4) 0.3314(2) 0.0467(16) Uiso 1.000000
H H36b 0.7644(5) 0.1564(4) 0.2957(2) 0.0467(16) Uiso 1.000000
C C37 0.6026(5) 0.2368(3) 0.2784(2) 0.0358(13) Uani 1.000000
H H37a 0.5658(5) 0.2072(3) 0.2429(2) 0.0430(16) Uiso 1.000000
H H37b 0.5860(5) 0.2993(3) 0.2786(2) 0.0430(16) Uiso 1.000000
C C40 0.5287(4) 0.4946(3) 0.25027(19) 0.0199(10) Uani 1.000000
N N1 -0.1192(4) 0.0935(3) 0.55236(18) 0.0340(11) Uani 1.000000
N N2 -0.0296(4) 0.1491(3) 0.58705(17) 0.0337(11) Uani 1.000000
N N3 -0.0131(4) 0.1637(2) 0.49808(16) 0.0247(9) Uani 1.000000
N N4 0.5597(4) 0.3923(2) 0.62437(17) 0.0282(10) Uani 1.000000
N N5 0.4392(4) 0.4191(2) 0.59548(17) 0.0274(9) Uani 1.000000
N N6 0.5367(4) 0.3603(2) 0.53353(15) 0.0225(9) Uani 1.000000
N N11 0.6314(4) 0.5156(3) 0.29063(17) 0.0323(10) Uani 1.000000
H H11a 0.6826(14) 0.545(2) 0.2755(3) 0.0388(12) Uiso 1.000000
H H11b 0.6089(5) 0.548(2) 0.3160(8) 0.0388(12) Uiso 1.000000
N N12 0.4175(4) 0.5096(2) 0.26117(16) 0.0252(9) Uani 1.000000
H H12a 0.4122(4) 0.5322(2) 0.29330(16) 0.0303(11) Uiso 1.000000
H H12b 0.3507(4) 0.4968(2) 0.23611(16) 0.0303(11) Uiso 1.000000
O O1 0.2329(3) 0.0913(2) 0.67171(16) 0.0400(10) Uani 1.000000
O O2 0.3967(3) 0.1674(2) 0.65853(16) 0.0375(9) Uani 1.000000
H H2 0.4322(13) 0.1199(8) 0.665(2) 0.0562(14) Uiso 1.000000
O O3 0.9978(3) 0.3701(2) 0.70006(15) 0.0315(8) Uani 1.000000
H H3 1.0365(6) 0.410(2) 0.7189(19) 0.0473(13) Uiso 1.000000
O O4 0.8308(3) 0.4412(2) 0.71645(14) 0.0302(8) Uani 1.000000
O O5 0.5392(3) 0.46065(19) 0.20385(12) 0.0231(7) Uani 1.000000
S S2 0.75922(12) 0.30727(9) 0.59523(5) 0.0317(3) Uani 1.000000
Br Br2 0.29317(5) 0.41848(3) 0.48198(2) 0.02899(14) Uani 1.000000
Br Br1 -0.18605(5) 0.04226(3) 0.43618(2) 0.03785(16) Uani 1.000000
C C41 0.1220(5) -0.0328(3) 0.29262(19) 0.0217(10) Uani 1.000000
N N13 0.2225(4) -0.0661(2) 0.32990(17) 0.0298(10) Uani 1.000000
H H13a 0.2016(10) -0.079(2) 0.3614(5) 0.0358(12) Uiso 1.000000
H H13b 0.246(2) -0.1132(13) 0.3157(6) 0.0358(12) Uiso 1.000000
N N14 0.0095(4) -0.0435(3) 0.30283(17) 0.0320(10) Uani 1.000000
H H14a 0.0011(4) -0.0712(3) 0.33285(17) 0.0384(12) Uiso 1.000000
H H14b -0.0550(4) -0.0226(3) 0.27944(17) 0.0384(12) Uiso 1.000000
O O6 0.1381(3) 0.0078(2) 0.24932(13) 0.0260(8) Uani 1.000000
S S1 0.15579(13) 0.26295(8) 0.57135(5) 0.0351(3) Uani 1.000000
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 0.022(3) 0.027(3) 0.033(3) 0.003(2) 0.007(2) 0.017(2)
C2 0.030(3) 0.028(3) 0.024(3) 0.009(2) 0.005(2) 0.013(2)
C3 0.033(3) 0.041(3) 0.028(3) 0.003(2) 0.006(3) 0.001(2)
C4 0.021(3) 0.041(3) 0.021(3) 0.005(2) 0.000(2) 0.006(2)
C5 0.021(3) 0.023(2) 0.025(3) -0.008(2) 0.005(2) 0.004(2)
C6 0.038(3) 0.014(2) 0.042(3) 0.000(2) 0.018(3) 0.005(2)
C7 0.035(3) 0.026(3) 0.038(3) 0.001(2) 0.022(3) 0.002(2)
C8 0.036(3) 0.027(3) 0.024(3) -0.004(2) 0.013(2) 0.000(2)
C9 0.023(3) 0.023(2) 0.027(3) -0.005(2) 0.009(2) 0.005(2)
C10 0.016(2) 0.022(2) 0.021(2) 0.0008(18) 0.000(2) 0.0051(19)
C11 0.018(3) 0.028(3) 0.026(3) -0.004(2) 0.005(2) 0.007(2)
C12 0.027(3) 0.032(3) 0.029(3) 0.002(2) 0.007(2) -0.002(2)
C13 0.032(3) 0.020(2) 0.039(3) 0.002(2) 0.007(3) 0.010(2)
C14 0.035(3) 0.027(3) 0.032(3) -0.001(2) 0.013(3) 0.007(2)
C15 0.039(3) 0.042(3) 0.032(3) 0.008(3) 0.018(3) 0.009(2)
C16 0.044(4) 0.052(4) 0.030(3) 0.009(3) 0.022(3) 0.010(3)
C17 0.063(5) 0.043(4) 0.064(4) -0.002(3) 0.031(4) 0.011(3)
C21 0.025(3) 0.027(3) 0.021(3) 0.000(2) 0.010(2) -0.001(2)
C22 0.030(3) 0.028(3) 0.019(2) -0.002(2) 0.008(2) -0.004(2)
C23 0.028(3) 0.028(3) 0.029(3) -0.002(2) 0.008(2) 0.001(2)
C24 0.026(3) 0.031(3) 0.015(2) 0.002(2) 0.003(2) 0.005(2)
C25 0.018(2) 0.022(2) 0.019(2) -0.0013(19) 0.004(2) -0.0052(19)
C26 0.030(3) 0.020(2) 0.033(3) -0.005(2) 0.011(3) -0.007(2)
C27 0.032(3) 0.031(3) 0.019(2) -0.008(2) 0.012(2) 0.000(2)
C28 0.018(3) 0.026(2) 0.017(2) -0.0003(19) 0.004(2) -0.0036(19)
C29 0.020(3) 0.021(2) 0.017(2) 0.0013(19) 0.003(2) -0.0042(18)
C30 0.017(2) 0.018(2) 0.019(2) 0.0002(18) 0.002(2) -0.0036(18)
C31 0.033(3) 0.030(3) 0.021(3) -0.002(2) 0.010(2) -0.002(2)
C32 0.045(4) 0.032(3) 0.038(3) -0.011(3) 0.016(3) 0.006(2)
C33 0.043(4) 0.018(3) 0.043(3) -0.006(2) 0.008(3) -0.004(2)
C34 0.038(3) 0.024(3) 0.022(3) -0.002(2) 0.011(2) -0.003(2)
C35 0.037(3) 0.035(3) 0.018(2) 0.000(2) 0.009(2) -0.010(2)
C36 0.038(3) 0.056(4) 0.026(3) -0.001(3) 0.015(3) -0.016(3)
C37 0.048(4) 0.040(3) 0.019(3) 0.004(3) 0.007(3) -0.005(2)
C40 0.024(3) 0.018(2) 0.020(2) -0.0006(19) 0.010(2) 0.0015(19)
N1 0.027(3) 0.039(3) 0.040(3) 0.009(2) 0.016(2) 0.023(2)
N2 0.036(3) 0.036(2) 0.032(2) 0.009(2) 0.015(2) 0.008(2)
N3 0.026(2) 0.025(2) 0.024(2) 0.0021(17) 0.006(2) 0.0090(17)
N4 0.024(2) 0.034(2) 0.027(2) 0.0009(18) 0.007(2) -0.0079(18)
N5 0.027(2) 0.028(2) 0.028(2) 0.0012(18) 0.009(2) -0.0054(18)
N6 0.025(2) 0.023(2) 0.019(2) 0.0012(17) 0.0044(19) -0.0044(16)
N11 0.025(3) 0.046(3) 0.028(2) -0.007(2) 0.010(2) -0.011(2)
N12 0.024(2) 0.031(2) 0.023(2) -0.0013(18) 0.010(2) -0.0038(17)
O1 0.023(2) 0.038(2) 0.059(3) -0.0024(16) 0.010(2) 0.0193(18)
O2 0.028(2) 0.035(2) 0.049(2) 0.0020(16) 0.009(2) 0.0096(18)
O3 0.024(2) 0.034(2) 0.035(2) -0.0020(15) 0.0061(18) -0.0117(16)
O4 0.0211(19) 0.0300(19) 0.042(2) 0.0006(14) 0.0133(17) -0.0096(16)
O5 0.0235(19) 0.0261(17) 0.0216(17) -0.0045(14) 0.0092(16) -0.0061(14)
S2 0.0255(7) 0.0453(8) 0.0239(7) 0.0053(6) 0.0048(6) -0.0096(6)
Br2 0.0251(3) 0.0304(3) 0.0302(3) 0.0016(2) 0.0036(2) -0.0084(2)
Br1 0.0327(3) 0.0335(3) 0.0433(3) -0.0112(2) 0.0003(3) 0.0119(2)
C41 0.023(3) 0.021(2) 0.021(2) -0.007(2) 0.003(2) 0.0021(19)
N13 0.035(3) 0.030(2) 0.025(2) 0.0035(19) 0.008(2) 0.0053(18)
N14 0.022(2) 0.049(3) 0.025(2) -0.003(2) 0.005(2) 0.0139(19)
O6 0.0199(19) 0.0347(18) 0.0262(18) 0.0009(14) 0.0113(16) 0.0075(15)
S1 0.0376(9) 0.0371(7) 0.0278(7) -0.0048(6) 0.0016(7) 0.0075(6)
loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870 51.65120
0.215599998832
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
0.00347 0.00161 'nternational Tables '
H 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236 57.79970
0.0030380000826
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
0.00000 0.00000 'International Tables'
O 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390 32.90890
0.250800013542
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
0.01158 0.00611 'International Tables V'
N 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750 0.58260
-11.5290002823
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
0.00653 0.00323 'International Tables V'
S 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360 56.17200
0.866900026798
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
0.12424 0.12443 'International Tables V'
Br 17.17890 5.23580 5.63770 3.98510 2.17230 16.57960 0.26090 41.43280
2.95569992065
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
-0.28346 2.55990 'International Tables'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N3 C1 N1 111.1(4)
Br1 C1 N1 126.8(4)
Br1 C1 N3 122.0(4)
N3 C2 N2 111.0(4)
S1 C2 N2 129.1(4)
S1 C2 N3 119.9(4)
S1 C3 C4 112.1(3)
O1 C4 C3 123.2(5)
O2 C4 C3 112.9(4)
O2 C4 O1 123.9(5)
C10 C5 C6 121.6(4)
N3 C5 C6 119.7(4)
N3 C5 C10 118.7(4)
C7 C6 C5 120.2(4)
C8 C7 C6 121.4(5)
C9 C8 C7 119.2(4)
C15 C8 C7 121.3(4)
C15 C8 C9 119.5(4)
C10 C9 C8 120.0(4)
C14 C9 C8 122.2(4)
C14 C9 C10 117.9(4)
C9 C10 C5 117.5(4)
C11 C10 C5 123.3(4)
C11 C10 C9 119.2(4)
C12 C11 C10 120.7(4)
C13 C12 C11 120.4(5)
C14 C13 C12 120.3(4)
C13 C14 C9 121.5(5)
C16 C15 C8 119.8(4)
C17 C15 C8 117.5(5)
C17 C15 C16 59.9(4)
C17 C16 C15 60.1(4)
C16 C17 C15 60.0(4)
N6 C21 N5 111.8(4)
Br2 C21 N5 126.4(4)
Br2 C21 N6 121.8(3)
N6 C22 N4 110.8(4)
S2 C22 N4 130.3(4)
S2 C22 N6 119.0(3)
S2 C23 C24 111.4(3)
O3 C24 C23 112.1(4)
O4 C24 C23 122.9(5)
O4 C24 O3 125.0(4)
C30 C25 C26 122.1(4)
N6 C25 C26 120.6(4)
N6 C25 C30 117.3(4)
C27 C26 C25 119.3(4)
C28 C27 C26 122.7(4)
C29 C28 C27 118.2(4)
C35 C28 C27 120.5(4)
C35 C28 C29 121.2(4)
C30 C29 C28 119.9(4)
C34 C29 C28 122.8(4)
C34 C29 C30 117.3(4)
C29 C30 C25 117.8(4)
C31 C30 C25 122.1(4)
C31 C30 C29 120.1(4)
C32 C31 C30 120.8(4)
C33 C32 C31 119.6(5)
C34 C33 C32 121.2(4)
C33 C34 C29 121.0(4)
C36 C35 C28 120.8(4)
C37 C35 C28 121.8(4)
C37 C35 C36 59.4(3)
C37 C36 C35 60.0(3)
C36 C37 C35 60.5(3)
N12 C40 N11 118.3(4)
O5 C40 N11 120.3(4)
O5 C40 N12 121.4(4)
N2 N1 C1 106.0(4)
N1 N2 C2 107.3(4)
C2 N3 C1 104.5(4)
C5 N3 C1 128.7(4)
C5 N3 C2 126.8(4)
N5 N4 C22 107.4(4)
N4 N5 C21 105.7(4)
C22 N6 C21 104.3(4)
C25 N6 C21 127.8(4)
C25 N6 C22 126.7(4)
C23 S2 C22 100.2(2)
N14 C41 N13 119.2(4)
O6 C41 N13 119.0(4)
O6 C41 N14 121.8(4)
C3 S1 C2 100.0(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.314(6)
C1 N3 1.371(6)
C1 Br1 1.845(5)
C2 N2 1.302(6)
C2 N3 1.369(6)
C2 S1 1.756(5)
C3 C4 1.514(6)
C3 S1 1.798(5)
C4 O1 1.199(6)
C4 O2 1.322(6)
C5 C6 1.363(6)
C5 C10 1.420(6)
C5 N3 1.436(6)
C6 C7 1.398(6)
C7 C8 1.372(6)
C8 C9 1.426(6)
C8 C15 1.497(7)
C9 C10 1.431(6)
C9 C14 1.414(6)
C10 C11 1.413(6)
C11 C12 1.372(6)
C12 C13 1.397(7)
C13 C14 1.370(7)
C15 C16 1.493(7)
C15 C17 1.495(8)
C16 C17 1.491(7)
C21 N5 1.310(5)
C21 N6 1.366(6)
C21 Br2 1.856(5)
C22 N4 1.308(6)
C22 N6 1.363(5)
C22 S2 1.742(5)
C23 C24 1.516(6)
C23 S2 1.811(5)
C24 O3 1.317(6)
C24 O4 1.211(5)
C25 C26 1.354(6)
C25 C30 1.426(6)
C25 N6 1.446(5)
C26 C27 1.402(6)
C27 C28 1.373(6)
C28 C29 1.437(6)
C28 C35 1.474(6)
C29 C30 1.422(6)
C29 C34 1.422(6)
C30 C31 1.406(6)
C31 C32 1.362(6)
C32 C33 1.402(7)
C33 C34 1.361(7)
C35 C36 1.505(7)
C35 C37 1.498(6)
C36 C37 1.488(7)
C40 N11 1.349(6)
C40 N12 1.329(6)
C40 O5 1.261(5)
N1 N2 1.418(6)
N4 N5 1.409(5)
C41 N13 1.353(6)
C41 N14 1.325(6)
C41 O6 1.259(5)
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_meas
_refln_F_squared_sigma
0 0 4 19806.1 1083.54
0 0 5 94.3432 140.189
0 0 -5 111.556 119.465
0 0 -6 3719.98 566.072
0 0 6 3637.43 580.282
0 0 -7 510.622 293.845
0 0 7 636.482 295.61
0 0 -8 80110.5 2495.78
0 0 -8 83273.5 3079.87
0 0 8 79564.5 3145.42
0 0 9 98.3509 159.234
0 0 -9 69.1391 126.632
0 0 -9 409.013 312.749
0 0 -10 9932.89 1205.87
0 0 -10 9542.71 968.35
0 0 -11 310.814 290.958
0 0 -11 44.2394 192.419
0 0 -12 9679.16 1306.86
0 0 -12 9193.04 1046.57
0 0 -13 197.268 257.242
0 0 -13 91.7453 268.683
0 0 -14 7630.88 1255.88
0 0 -14 8938.98 1266.56
0 0 -14 10328.1 1210.56
0 0 -15 658.613 453.924
0 0 -15 -382.285 309.742
0 0 -15 184.972 164.461
0 0 -16 5938.11 1119.51
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