#------------------------------------------------------------------------------
#$Date: 2020-11-26 07:08:40 +0200 (Thu, 26 Nov 2020) $
#$Revision: 259255 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/22/2022284.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_2022284
loop_
_publ_author_name
'Ye, Wenkang'
'She, Weiyi'
'Sung, Herman H.-Y.'
'Qian, Peiyuan'
'Williams, Ian D.'
_publ_section_title
;
Albofungin and chloroalbofungin: antibiotic crystals with 2D but not 3D
isostructurality
;
_journal_coeditor_code JX3059
_journal_issue 12
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 1100
_journal_page_last 1107
_journal_paper_doi 10.1107/S2053229620015041
_journal_volume 76
_journal_year 2020
_chemical_absolute_configuration unk
_chemical_formula_iupac 'C27 H23 Cl N2 O9'
_chemical_formula_moiety 'C27 H23 Cl N2 O9'
_chemical_formula_sum 'C27 H23 Cl N2 O9'
_chemical_formula_weight 554.94
_chemical_name_systematic
(1S,4R,8aR)-13-Amino-11-chloro-1,15,16-trihydroxy-4-methoxy-12-methyl-3,4,8a,13-tetrahydro-1H-xantheno[4',3',2':4,5][1,3]benzodioxino[7,6-g]isoquinoline-14,17(2H,9H)-dione
_space_group_crystal_system monoclinic
_space_group_IT_number 5
_space_group_name_Hall 'C 2y'
_space_group_name_H-M_alt 'C 1 2 1'
_atom_sites_solution_primary direct
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha 90
_cell_angle_beta 98.027(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 40.6637(9)
_cell_length_b 4.52749(12)
_cell_length_c 12.7049(3)
_cell_measurement_reflns_used 4359
_cell_measurement_temperature 100.01(10)
_cell_measurement_theta_max 72.4360
_cell_measurement_theta_min 3.5070
_cell_volume 2316.11(10)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2020)
;
_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)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015)
;
_diffrn_ambient_temperature 100.0
_diffrn_detector_area_resol_mean 5.1788
_diffrn_measured_fraction_theta_full 0.9486
_diffrn_measured_fraction_theta_max 0.9486
_diffrn_measurement_device 'kappa diffractometer'
_diffrn_measurement_device_type
'Rigaku OD SuperNova Dual source diffractometer with an Atlas detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0293
_diffrn_reflns_av_unetI/netI 0.0456
_diffrn_reflns_limit_h_max 49
_diffrn_reflns_limit_h_min -49
_diffrn_reflns_limit_k_max 5
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 8597
_diffrn_reflns_theta_full 72.6177
_diffrn_reflns_theta_max 72.62
_diffrn_reflns_theta_min 2.19
_exptl_absorpt_coefficient_mu 2.032
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.82030
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO (Rigaku OD, 2020)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.5913
_exptl_crystal_description needle
_exptl_crystal_F_000 1157.5525
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.2467
_refine_diff_density_min -0.1911
_refine_ls_abs_structure_details
;
Parsons et al. (2013)
;
_refine_ls_abs_structure_Flack 0.002(14)
_refine_ls_goodness_of_fit_ref 1.0170
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_constraints 28
_refine_ls_number_parameters 374
_refine_ls_number_reflns 4376
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.0170
_refine_ls_R_factor_all 0.0390
_refine_ls_R_factor_gt 0.0340
_refine_ls_shift/su_max 0.0006
_refine_ls_shift/su_mean 0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0798
_refine_ls_wR_factor_ref 0.0823
_reflns_number_gt 4010
_reflns_number_total 4376
_reflns_threshold_expression I>=2u(I)
_iucr_refine_instructions_details
;
TITL ye18a_100K in C2 #5
REM reset to O17 #5
CELL 1.54184 40.66367 4.52749 12.70493 90 98.0267 90
ZERR 4 0.00093 0.00012 0.0003 0 0.0021 0
LATT -7
SYMM -X,+Y,-Z
SFAC C H Cl N O
UNIT 108 92 4 8 36
L.S. 20
PLAN 20
SIZE 0.03 0.03 0.18
BOND
fmap 2
acta
OMIT 18 -4 -9
OMIT 16 0 1
OMIT -2 0 3
OMIT -4 0 10
OMIT 0 0 3
OMIT 8 0 8
WGHT 0.039974 0
FVAR 4.216191
REM
REM
REM
Cl1 3 0.19848 0.49129 0.06464 11.00000 0.02757 0.04326 0.02025 =
-0.00461 0.00803 -0.00384
O1 5 0.22011 1.07557 0.47453 11.00000 0.01987 0.02321 0.02619 =
-0.00011 0.00387 -0.00045
N1 4 0.23576 0.96938 0.31406 11.00000 0.01701 0.02598 0.02512 =
0.00127 0.00358 -0.00006
C1 1 0.21491 0.93174 0.38929 11.00000 0.01860 0.02012 0.02037 =
0.00318 0.00187 0.00389
H3 2 0.18668 0.90892 0.53695 11.00000 0.05041
N2 4 0.26239 1.17403 0.33733 11.00000 0.02103 0.03317 0.02798 =
-0.00211 0.00415 -0.00752
C2 1 0.18820 0.72232 0.36416 11.00000 0.01729 0.02106 0.02080 =
0.00340 0.00387 0.00271
O3 5 0.17107 0.80000 0.53517 11.00000 0.02269 0.02127 0.02246 =
-0.00297 0.00643 -0.00234
C3 1 0.16744 0.65441 0.44249 11.00000 0.01882 0.01886 0.01833 =
0.00200 0.00282 0.00483
H10 2 0.15245 -0.00156 0.98101 11.00000 0.06939
C4 1 0.14256 0.44125 0.42244 11.00000 0.01864 0.01787 0.01961 =
0.00125 0.00267 0.00427
C5 1 0.12239 0.33024 0.50324 11.00000 0.01893 0.01859 0.01892 =
-0.00176 0.00373 0.00258
O6 5 0.16667 0.32233 0.64790 11.00000 0.02029 0.02924 0.01728 =
0.00114 0.00191 -0.00291
C6 1 0.13493 0.26434 0.60896 11.00000 0.01657 0.01990 0.02213 =
-0.00258 0.00374 0.00114
C7 1 0.11475 0.11142 0.67388 11.00000 0.02112 0.02575 0.01778 =
-0.00230 0.00512 0.00169
O8 5 0.15678 0.07046 0.82323 11.00000 0.02278 0.04267 0.02099 =
0.00207 0.00052 -0.00543
C8 1 0.12760 0.01644 0.78173 11.00000 0.02459 0.02534 0.02136 =
-0.00249 0.00409 -0.00096
H6 2 0.16831 0.25607 0.70750 11.00000 0.03612
C9 1 0.10473 -0.14357 0.83946 11.00000 0.02621 0.02251 0.02213 =
-0.00267 0.00678 0.00114
O10 5 0.13224 0.00393 1.01334 11.00000 0.03530 0.03502 0.02017 =
-0.00131 0.00369 -0.00585
C10 1 0.11600 -0.23239 0.95461 11.00000 0.02729 0.02747 0.02354 =
0.00154 0.00525 0.00154
AFIX 13
H10a 2 0.13137 -0.39953 0.95592 11.00000 -1.20000
AFIX 0
C11 1 0.08672 -0.32167 1.00992 11.00000 0.03376 0.03197 0.02090 =
0.00501 0.00765 0.00219
AFIX 23
H11a 2 0.09479 -0.41764 1.07681 11.00000 -1.20000
H11b 2 0.07447 -0.14670 1.02528 11.00000 -1.20000
AFIX 0
C12 1 0.06389 -0.52943 0.94111 11.00000 0.03398 0.02829 0.03198 =
0.00439 0.01285 -0.00230
AFIX 23
H12a 2 0.07636 -0.70185 0.92448 11.00000 -1.20000
H12b 2 0.04641 -0.59519 0.98029 11.00000 -1.20000
AFIX 0
O13 5 0.02297 -0.17818 0.85392 11.00000 0.02383 0.04429 0.03409 =
0.00232 0.01074 -0.00043
C13 1 0.04842 -0.38340 0.83836 11.00000 0.02997 0.03055 0.02504 =
-0.00436 0.01010 -0.00617
AFIX 13
H13 2 0.03912 -0.53608 0.78816 11.00000 -1.20000
AFIX 0
C14 1 0.07419 -0.21055 0.78996 11.00000 0.02588 0.02504 0.01999 =
0.00019 0.00719 0.00102
O15 5 0.06226 -0.13080 0.68890 11.00000 0.02170 0.03795 0.02014 =
0.00101 0.00656 -0.00676
C16 1 0.08250 0.02797 0.63209 11.00000 0.01860 0.02874 0.02216 =
0.00170 0.00678 -0.00265
O17 5 0.03783 0.00097 0.49037 11.00000 0.01640 0.04961 0.02609 =
0.00649 0.00105 -0.00888
C17 1 0.06968 0.09416 0.52776 11.00000 0.01554 0.03349 0.02515 =
-0.00085 0.00290 0.00004
C18 1 0.08955 0.23719 0.46459 11.00000 0.01815 0.02645 0.02107 =
-0.00073 0.00265 0.00350
O19 5 0.04824 0.09279 0.31809 11.00000 0.01900 0.04304 0.02213 =
0.00051 -0.00010 -0.00689
C19 1 0.07782 0.26480 0.34700 11.00000 0.01918 0.02886 0.02359 =
0.00373 0.00186 -0.00259
AFIX 13
H19 2 0.07359 0.47242 0.32791 11.00000 -1.20000
AFIX 0
C20 1 0.10496 0.14154 0.28837 11.00000 0.01859 0.02505 0.01998 =
0.00094 0.00234 -0.00118
AFIX 23
H20a 2 0.10964 -0.06206 0.30904 11.00000 -1.20000
H20b 2 0.09791 0.14763 0.21224 11.00000 -1.20000
AFIX 0
C21 1 0.13571 0.32931 0.31717 11.00000 0.01917 0.01843 0.02014 =
0.00085 0.00204 0.00094
H2a 2 0.28257 1.07131 0.35816 11.00000 0.02780
H2b 2 0.25908 1.26264 0.39287 11.00000 0.04181
C22 1 0.15515 0.39689 0.24019 11.00000 0.02099 0.02199 0.01987 =
-0.00109 0.00163 0.00362
AFIX 43
H22 2 0.15020 0.31582 0.17258 11.00000 -1.20000
AFIX 0
C23 1 0.18232 0.58695 0.26309 11.00000 0.02123 0.02194 0.01776 =
0.00224 0.00315 0.00389
C24 1 0.20483 0.65625 0.18962 11.00000 0.02187 0.02928 0.01947 =
0.00114 0.00373 0.00402
C25 1 0.23123 0.83926 0.21444 11.00000 0.02157 0.02909 0.02209 =
0.00252 0.00286 0.00129
C26 1 0.25678 0.90260 0.14341 11.00000 0.02335 0.04631 0.02700 =
-0.00142 0.00803 -0.00041
AFIX 137
H26a 2 0.26274 1.10777 0.14868 11.00000 -1.50000
H26b 2 0.27612 0.78383 0.16470 11.00000 -1.50000
H26c 2 0.24787 0.85686 0.07126 11.00000 -1.50000
AFIX 0
C27 1 0.02588 0.13509 0.39095 11.00000 0.01902 0.04976 0.02802 =
0.00513 0.00254 -0.00340
AFIX 23
H27a 2 0.00455 0.05010 0.36291 11.00000 -1.20000
H27b 2 0.02273 0.34496 0.40122 11.00000 -1.20000
AFIX 0
C28 1 -0.00812 -0.31878 0.85507 11.00000 0.02641 0.07727 0.04697 =
0.02686 0.00415 -0.00582
AFIX 137
H28a 2 -0.01599 -0.39419 0.78549 11.00000 -1.50000
H28b 2 -0.00562 -0.47868 0.90518 11.00000 -1.50000
H28c 2 -0.02381 -0.17870 0.87534 11.00000 -1.50000
AFIX 0
HKLF 4
END
Q1 1 0.172 0.5 0.075 11 0.05 0.25
Q2 1 0.224 0.466667 0.05 11 0.05 0.24
Q3 1 0.28 1 0.175 11 0.05 0.23
Q4 1 0.1 0.033333 0.65 11 0.05 0.23
Q5 1 0.124 0.233333 0.3 11 0.05 0.22
Q6 1 0.284 0.7 0.2 11 0.05 0.22
Q7 1 0.212 0.633333 0.1 11 0.05 0.21
Q8 1 0.188 0.633333 0.325 11 0.05 0.2
Q9 1 0.148 0.233333 0.15 11 0.05 0.2
Q10 1 0.176 0.733333 0.4 11 0.05 0.2
Q11 1 0.204 0.766667 0.375 11 0.05 0.2
Q12 1 0.124 0.366667 0.575 11 0.05 0.2
Q13 1 0.196 0.566667 0.225 11 0.05 0.2
Q14 1 0.04 0.2 0.25 11 0.05 0.19
Q15 1 0.172 0.433333 0.25 11 0.05 0.18
Q16 1 0.036 -0.1 0.7 11 0.05 0.18
Q17 1 0.148 0.633333 0.425 11 0.05 0.18
Q18 1 0.1 0.3 0.475 11 0.05 0.17
Q19 1 0.228 0.633333 0.2 11 0.05 0.17
Q20 1 0.236 0.9 0.375 11 0.05 0.17
REM The information below was added by Olex2.
REM
REM R1 = 0.0340 for 4010 Fo > 4sig(Fo) and 0.0390 for all 4376 data
REM 374 parameters refined using 1 restraints
REM Highest difference peak 0.2467, deepest hole -0.1911
REM Mean Shift 0.0000, Max Shift 0.0006.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0390
REM R1_gt = 0.0340
REM wR_ref = 0.0823
REM GOOF = 1.0170
REM Shift_max = 0.0006
REM Shift_mean = 0.0000
REM Reflections_all = 4376
REM Reflections_gt = 4010
REM Parameters = 374
REM Hole = -0.1911
REM Peak = 0.2467
REM Flack = 0.002(14)
;
_cod_data_source_file jx3059sup1.cif
_cod_data_source_block ye18a_100K
_cod_original_cell_volume 2316.12(10)
_cod_original_sg_symbol_Hall ' C 2y'
_cod_database_code 2022284
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z
3 x+1/2,y+1/2,z
4 -x+1/2,y+1/2,-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_occupancy
Cl Cl1 0.198485(13) 0.49129(11) 0.06464(4) 0.02992(13) Uani 1.000000
O O1 0.22011(3) 1.0756(3) 0.47453(12) 0.0230(3) Uani 1.000000
N N1 0.23576(4) 0.9694(4) 0.31406(14) 0.0226(4) Uani 1.000000
C C1 0.21491(5) 0.9317(5) 0.38929(16) 0.0198(4) Uani 1.000000
H H3 0.1867(8) 0.909(8) 0.537(3) 0.050(10) Uiso 1.000000
N N2 0.26239(5) 1.1740(4) 0.33733(16) 0.0273(4) Uani 1.000000
C C2 0.18820(5) 0.7223(5) 0.36416(17) 0.0196(4) Uani 1.000000
O O3 0.17107(4) 0.8000(3) 0.53517(12) 0.0218(3) Uani 1.000000
C C3 0.16744(5) 0.6544(5) 0.44249(16) 0.0186(4) Uani 1.000000
H H10 0.1524(8) -0.002(10) 0.981(3) 0.069(11) Uiso 1.000000
C C4 0.14256(5) 0.4413(4) 0.42244(16) 0.0187(4) Uani 1.000000
C C5 0.12239(5) 0.3302(5) 0.50324(16) 0.0187(4) Uani 1.000000
O O6 0.16667(4) 0.3223(3) 0.64790(12) 0.0223(3) Uani 1.000000
C C6 0.13493(5) 0.2643(5) 0.60896(17) 0.0194(4) Uani 1.000000
C C7 0.11475(5) 0.1114(5) 0.67388(17) 0.0213(4) Uani 1.000000
O O8 0.15678(4) 0.0705(4) 0.82323(12) 0.0291(4) Uani 1.000000
C C8 0.12760(5) 0.0164(5) 0.78173(16) 0.0237(4) Uani 1.000000
H H6 0.1683(7) 0.256(7) 0.708(3) 0.036(8) Uiso 1.000000
C C9 0.10473(5) -0.1436(5) 0.83946(17) 0.0233(5) Uani 1.000000
O O10 0.13224(4) 0.0039(4) 1.01334(11) 0.0302(4) Uani 1.000000
C C10 0.11600(6) -0.2324(5) 0.95461(17) 0.0259(5) Uani 1.000000
H H10a 0.13137(6) -0.3995(5) 0.95592(17) 0.0311(6) Uiso 1.000000
C C11 0.08672(6) -0.3217(5) 1.00992(18) 0.0285(5) Uani 1.000000
H H11a 0.09479(6) -0.4176(5) 1.07681(18) 0.0342(6) Uiso 1.000000
H H11b 0.07447(6) -0.1467(5) 1.02528(18) 0.0342(6) Uiso 1.000000
C C12 0.06389(6) -0.5294(6) 0.94111(18) 0.0306(5) Uani 1.000000
H H12a 0.07636(6) -0.7019(6) 0.92448(18) 0.0368(6) Uiso 1.000000
H H12b 0.04641(6) -0.5952(6) 0.98029(18) 0.0368(6) Uiso 1.000000
O O13 0.02297(4) -0.1782(4) 0.85392(14) 0.0334(4) Uani 1.000000
C C13 0.04842(6) -0.3834(5) 0.83836(18) 0.0279(5) Uani 1.000000
H H13 0.03912(6) -0.5361(5) 0.78816(18) 0.0335(6) Uiso 1.000000
C C14 0.07419(5) -0.2105(5) 0.78996(17) 0.0233(5) Uani 1.000000
O O15 0.06226(4) -0.1308(4) 0.68890(12) 0.0263(4) Uani 1.000000
C C16 0.08250(5) 0.0280(5) 0.63209(16) 0.0228(4) Uani 1.000000
O O17 0.03783(3) 0.0010(4) 0.49037(12) 0.0309(4) Uani 1.000000
C C17 0.06968(5) 0.0942(5) 0.52776(18) 0.0247(5) Uani 1.000000
C C18 0.08955(5) 0.2372(5) 0.46459(17) 0.0219(5) Uani 1.000000
O O19 0.04824(4) 0.0928(4) 0.31809(12) 0.0283(4) Uani 1.000000
C C19 0.07782(5) 0.2648(5) 0.34700(17) 0.0240(5) Uani 1.000000
H H19 0.07359(5) 0.4724(5) 0.32791(17) 0.0288(6) Uiso 1.000000
C C20 0.10496(5) 0.1415(5) 0.28837(17) 0.0212(4) Uani 1.000000
H H20a 0.10964(5) -0.0621(5) 0.30904(17) 0.0255(5) Uiso 1.000000
H H20b 0.09791(5) 0.1476(5) 0.21224(17) 0.0255(5) Uiso 1.000000
C C21 0.13571(5) 0.3293(5) 0.31717(17) 0.0193(4) Uani 1.000000
H H2a 0.2826(7) 1.071(7) 0.358(2) 0.028(7) Uiso 1.000000
H H2b 0.2591(7) 1.263(8) 0.393(3) 0.042(9) Uiso 1.000000
C C22 0.15515(5) 0.3969(5) 0.24019(17) 0.0211(4) Uani 1.000000
H H22 0.15020(5) 0.3158(5) 0.17258(17) 0.0253(5) Uiso 1.000000
C C23 0.18232(5) 0.5870(5) 0.26309(16) 0.0203(4) Uani 1.000000
C C24 0.20483(5) 0.6562(5) 0.18962(17) 0.0235(5) Uani 1.000000
C C25 0.23123(5) 0.8393(5) 0.21444(17) 0.0243(5) Uani 1.000000
C C26 0.25678(6) 0.9026(6) 0.14341(19) 0.0318(6) Uani 1.000000
H H26a 0.2627(3) 1.1078(11) 0.1487(11) 0.0477(9) Uiso 1.000000
H H26b 0.2761(2) 0.784(3) 0.1647(10) 0.0477(9) Uiso 1.000000
H H26c 0.24787(18) 0.857(4) 0.0713(3) 0.0477(9) Uiso 1.000000
C C27 0.02588(5) 0.1351(6) 0.39095(19) 0.0323(6) Uani 1.000000
H H27a 0.00455(5) 0.0501(6) 0.36291(19) 0.0388(7) Uiso 1.000000
H H27b 0.02273(5) 0.3450(6) 0.40122(19) 0.0388(7) Uiso 1.000000
C C28 -0.00812(6) -0.3188(7) 0.8551(2) 0.0503(9) Uani 1.000000
H H28a -0.0160(3) -0.394(5) 0.7855(6) 0.0755(13) Uiso 1.000000
H H28b -0.00562(14) -0.479(4) 0.9052(15) 0.0755(13) Uiso 1.000000
H H28c -0.02381(18) -0.1787(16) 0.8753(19) 0.0755(13) Uiso 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
Cl1 0.0276(3) 0.0433(3) 0.0203(2) -0.0038(2) 0.00803(18) -0.0046(3)
O1 0.0199(7) 0.0232(9) 0.0262(8) -0.0005(6) 0.0039(6) -0.0001(6)
N1 0.0170(8) 0.0260(10) 0.0251(9) -0.0001(8) 0.0036(6) 0.0013(9)
C1 0.0186(9) 0.0201(11) 0.0204(10) 0.0039(8) 0.0019(7) 0.0032(8)
N2 0.0210(10) 0.0332(12) 0.0280(10) -0.0075(8) 0.0041(8) -0.0021(9)
C2 0.0173(9) 0.0211(11) 0.0208(10) 0.0027(8) 0.0039(8) 0.0034(8)
O3 0.0227(8) 0.0213(8) 0.0225(8) -0.0023(7) 0.0064(6) -0.0030(6)
C3 0.0188(9) 0.0189(11) 0.0183(10) 0.0048(8) 0.0028(8) 0.0020(8)
C4 0.0186(9) 0.0179(11) 0.0196(10) 0.0043(8) 0.0027(7) 0.0012(8)
C5 0.0189(9) 0.0186(10) 0.0189(10) 0.0026(8) 0.0037(8) -0.0018(9)
O6 0.0203(7) 0.0292(9) 0.0173(8) -0.0029(6) 0.0019(6) 0.0011(7)
C6 0.0166(9) 0.0199(11) 0.0221(10) 0.0011(8) 0.0037(8) -0.0026(9)
C7 0.0211(10) 0.0257(12) 0.0178(10) 0.0017(9) 0.0051(8) -0.0023(8)
O8 0.0228(7) 0.0427(11) 0.0210(7) -0.0054(7) 0.0005(6) 0.0021(7)
C8 0.0246(10) 0.0253(12) 0.0214(10) -0.0010(9) 0.0041(8) -0.0025(10)
C9 0.0262(11) 0.0225(11) 0.0221(11) 0.0011(9) 0.0068(8) -0.0027(9)
O10 0.0353(8) 0.0350(9) 0.0202(7) -0.0058(8) 0.0037(6) -0.0013(8)
C10 0.0273(11) 0.0275(12) 0.0235(11) 0.0015(9) 0.0052(9) 0.0015(9)
C11 0.0338(12) 0.0320(14) 0.0209(11) 0.0022(10) 0.0076(9) 0.0050(10)
C12 0.0340(12) 0.0283(13) 0.0320(11) -0.0023(11) 0.0129(9) 0.0044(11)
O13 0.0238(8) 0.0443(11) 0.0341(9) -0.0004(8) 0.0107(7) 0.0023(8)
C13 0.0300(11) 0.0305(13) 0.0250(11) -0.0062(10) 0.0101(9) -0.0044(10)
C14 0.0259(11) 0.0250(12) 0.0200(10) 0.0010(9) 0.0072(8) 0.0002(9)
O15 0.0217(7) 0.0379(10) 0.0201(7) -0.0068(7) 0.0066(6) 0.0010(7)
C16 0.0186(9) 0.0287(12) 0.0222(10) -0.0027(9) 0.0068(7) 0.0017(10)
O17 0.0164(7) 0.0496(11) 0.0261(8) -0.0089(8) 0.0010(6) 0.0065(9)
C17 0.0155(9) 0.0335(13) 0.0251(11) 0.0000(9) 0.0029(8) -0.0008(9)
C18 0.0181(10) 0.0264(12) 0.0211(10) 0.0035(8) 0.0027(8) -0.0007(9)
O19 0.0190(7) 0.0430(11) 0.0221(7) -0.0069(7) -0.0001(6) 0.0005(7)
C19 0.0192(10) 0.0289(13) 0.0236(11) -0.0026(9) 0.0019(8) 0.0037(10)
C20 0.0186(9) 0.0250(11) 0.0200(10) -0.0012(9) 0.0023(8) 0.0009(9)
C21 0.0192(9) 0.0184(10) 0.0201(10) 0.0009(8) 0.0020(7) 0.0009(8)
C22 0.0210(10) 0.0220(11) 0.0199(10) 0.0036(8) 0.0016(8) -0.0011(8)
C23 0.0212(9) 0.0219(11) 0.0178(10) 0.0039(8) 0.0032(7) 0.0022(8)
C24 0.0219(10) 0.0293(12) 0.0195(10) 0.0040(9) 0.0037(8) 0.0011(9)
C25 0.0216(10) 0.0291(12) 0.0221(11) 0.0013(9) 0.0029(8) 0.0025(10)
C26 0.0234(11) 0.0463(17) 0.0270(11) -0.0004(10) 0.0080(9) -0.0014(10)
C27 0.0190(10) 0.0498(16) 0.0280(12) -0.0034(11) 0.0025(9) 0.0051(11)
C28 0.0264(13) 0.077(2) 0.0470(17) -0.0058(14) 0.0041(11) 0.0269(16)
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
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'
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'
0.01920 0.00962 'nternational Tables '
Cl 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940 47.77840
-9.55739974976
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
0.36843 0.69943 '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'
0.05239 0.03377 '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'
0.03256 0.01839 'International Tables V'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 N1 C1 . . 117.47(17) ?
C25 N1 C1 . . 124.52(18) ?
C25 N1 N2 . . 117.82(18) ?
N1 C1 O1 . . 119.31(18) ?
C2 C1 O1 . . 124.20(19) ?
C2 C1 N1 . . 116.49(18) ?
C3 C2 C1 . . 119.21(18) ?
C23 C2 C1 . . 120.82(19) ?
C23 C2 C3 . . 119.97(19) ?
O3 C3 C2 . . 120.27(18) ?
C4 C3 C2 . . 120.43(18) ?
C4 C3 O3 . . 119.28(19) ?
C5 C4 C3 . . 124.26(18) ?
C21 C4 C3 . . 117.41(19) ?
C21 C4 C5 . . 118.31(18) ?
C6 C5 C4 . . 124.87(17) ?
C18 C5 C4 . . 116.34(17) ?
C18 C5 C6 . . 117.83(19) ?
O6 C6 C5 . . 120.95(19) ?
C7 C6 C5 . . 119.85(18) ?
C7 C6 O6 . . 118.98(18) ?
C8 C7 C6 . . 121.83(18) ?
C16 C7 C6 . . 119.90(19) ?
C16 C7 C8 . . 118.09(19) ?
O8 C8 C7 . . 122.1(2) ?
C9 C8 C7 . . 116.67(18) ?
C9 C8 O8 . . 121.28(19) ?
C10 C9 C8 . . 119.15(18) ?
C14 C9 C8 . . 119.3(2) ?
C14 C9 C10 . . 121.5(2) ?
O10 C10 C9 . . 111.25(19) ?
C11 C10 C9 . . 111.34(18) ?
C11 C10 O10 . . 107.19(18) ?
C12 C11 C10 . . 110.85(19) ?
C13 C12 C11 . . 111.9(2) ?
C28 O13 C13 . . 112.0(2) ?
O13 C13 C12 . . 112.72(19) ?
C14 C13 C12 . . 110.42(18) ?
C14 C13 O13 . . 106.14(19) ?
C13 C14 C9 . . 125.1(2) ?
O15 C14 C9 . . 124.5(2) ?
O15 C14 C13 . . 110.35(17) ?
C16 O15 C14 . . 118.43(16) ?
O15 C16 C7 . . 122.85(18) ?
C17 C16 C7 . . 120.83(19) ?
C17 C16 O15 . . 116.28(17) ?
C27 O17 C17 . . 111.22(17) ?
O17 C17 C16 . . 118.14(19) ?
C18 C17 C16 . . 119.03(18) ?
C18 C17 O17 . . 122.77(19) ?
C17 C18 C5 . . 122.52(19) ?
C19 C18 C5 . . 118.02(19) ?
C19 C18 C17 . . 119.06(18) ?
C27 O19 C19 . . 110.80(17) ?
O19 C19 C18 . . 110.24(18) ?
C20 C19 C18 . . 107.68(17) ?
C20 C19 O19 . . 108.34(18) ?
C21 C20 C19 . . 107.87(17) ?
C20 C21 C4 . . 118.33(19) ?
C22 C21 C4 . . 122.23(19) ?
C22 C21 C20 . . 119.37(18) ?
C23 C22 C21 . . 120.33(19) ?
C22 C23 C2 . . 118.97(19) ?
C24 C23 C2 . . 117.10(19) ?
C24 C23 C22 . . 123.93(19) ?
C23 C24 Cl1 . . 118.30(16) ?
C25 C24 Cl1 . . 119.03(17) ?
C25 C24 C23 . . 122.6(2) ?
C24 C25 N1 . . 118.2(2) ?
C26 C25 N1 . . 117.05(19) ?
C26 C25 C24 . . 124.8(2) ?
O19 C27 O17 . . 110.84(18) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cl1 C24 . 1.741(2) ?
O1 C1 . 1.256(3) ?
N1 C1 . 1.374(3) ?
N1 N2 . 1.424(2) ?
N1 C25 . 1.385(3) ?
C1 C2 . 1.444(3) ?
C2 C3 . 1.426(3) ?
C2 C23 . 1.413(3) ?
O3 C3 . 1.339(3) ?
C3 C4 . 1.396(3) ?
C4 C5 . 1.488(3) ?
C4 C21 . 1.421(3) ?
C5 C6 . 1.401(3) ?
C5 C18 . 1.421(3) ?
O6 C6 . 1.342(2) ?
C6 C7 . 1.422(3) ?
C7 C8 . 1.461(3) ?
C7 C16 . 1.396(3) ?
O8 C8 . 1.253(3) ?
C8 C9 . 1.456(3) ?
C9 C10 . 1.525(3) ?
C9 C14 . 1.346(3) ?
O10 C10 . 1.414(3) ?
C10 C11 . 1.519(3) ?
C11 C12 . 1.511(3) ?
C12 C13 . 1.519(3) ?
O13 C13 . 1.425(3) ?
O13 C28 . 1.417(3) ?
C13 C14 . 1.506(3) ?
C14 O15 . 1.357(3) ?
O15 C16 . 1.372(3) ?
C16 C17 . 1.388(3) ?
O17 C17 . 1.382(2) ?
O17 C27 . 1.424(3) ?
C17 C18 . 1.378(3) ?
C18 C19 . 1.509(3) ?
O19 C19 . 1.437(2) ?
O19 C27 . 1.399(3) ?
C19 C20 . 1.521(3) ?
C20 C21 . 1.514(3) ?
C21 C22 . 1.375(3) ?
C22 C23 . 1.399(3) ?
C23 C24 . 1.430(3) ?
C24 C25 . 1.358(3) ?
C25 C26 . 1.496(3) ?
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
O10 H10 O8 . 0.97(3) 2.06(4) 2.756(2) 127(3)
O3 H3 O1 . 0.80(3) 1.83(3) 2.561(2) 151(4)
O6 H6 O8 . 0.81(4) 1.81(4) 2.583(2) 159(3)
N2 H2b O1 4_556 0.84(4) 2.27(3) 3.009(2) 147(3)
N2 H2a O6 4_556 0.95(3) 2.36(3) 3.277(3) 162(2)
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_meas
_refln_F_squared_sigma
0 0 -1 215208 2848.15
0 0 -2 961.054 287.049
0 0 -3 12830.7 885.236
0 0 -4 -132.057 365.013
0 0 4 -53.2315 247.396
0 0 5 7208.99 669.315
0 0 -5 6640.27 903.067
0 0 6 434045 6944.66
0 0 -6 444337 8621.44
0 0 -7 77982.9 3488.4
0 0 7 70419.1 2389.22
0 0 -9 10835.8 1059.48
0 0 -9 10791.2 1005.6
0 0 -9 9830.5 850.393
0 0 -10 8770.17 1137.28
0 0 -10 9647.39 1067.31
0 0 -10 8196.64 798.43
0 0 -10 9194.87 920.181
0 0 -11 13138.8 1457.72
0 0 -11 13997.2 1214.72
0 0 -11 11764.5 1017.65
0 0 -11 12950.6 1294.39
0 0 -12 1675.68 942.215
0 0 -12 1339.16 613.541
0 0 -12 1173.96 512.492
0 0 -12 451.494 381.02
0 0 -13 31806.3 1430.06
0 0 -13 30501.8 1818.16
0 0 -14 2160.31 510.484
0 -2 0 12107.5 1246.83
0 2 0 14557.4 1007.49
0 -2 -1 51879.6 2504.82
0 -2 1 51937.3 2458.16
0 2 -1 50626.6 1715.6
0 2 1 49793.4 2179.97
0 -2 2 19758.1 1518.7
0 -2 -2 21585.4 1678.29
0 2 2 23121.1 1597.16
0 -2 3 3642.56 711.218
0 2 3 4276.74 779.035
0 -2 -3 4302.67 876.275
0 2 4 38639.5 2490.57
0 -2 4 36531.7 1928.16
0 2 5 8280.52 1296.13
0 2 6 23528.4 2209.62
0 2 -7 7507.97 796.857
0 2 -7 6706.43 816.286
0 -2 -7 8820.24 910.074
0 2 -7 7870.11 852.206
0 2 -7 7313.48 808.799
0 2 -7 6497.28 845.07
0 2 7 7959.16 1389.3
0 -2 -7 7495.89 927.379
0 -2 -8 9996.05 1114.61
0 2 -8 10397.7 995.984
0 -2 -8 8242.74 1032.28
0 2 8 11377.4 1663.53
0 2 -8 11136.7 1051.07
0 2 -8 10469 1125.16
0 2 -8 11908.3 1172.17
0 2 9 17924.8 1919.84
0 -2 -9 12815.1 1349.15
0 2 -9 17289.7 1351.46
0 -2 -9 17486 1486.36
0 2 -9 16270.8 1409.54
0 2 -9 18156.8 1429.54
0 2 -9 17179.7 1477.1
0 -2 -10 2113.35 699.753
0 2 -10 1259.85 642.588
0 2 -10 1527.88 589.243
0 2 -10 1422.3 583.373
0 2 -10 3266.96 1235.3
0 2 -11 27183.7 1697.35
0 2 -11 27748.9 1800.95
0 2 -11 26649.2 1963.8
0 -2 -11 25878.9 1943.61
0 2 -11 26990.4 1810.06
0 2 -12 9620.61 958.853
0 2 -12 8488.59 1108.47
0 -2 -12 9255.71 1195.42
0 2 -12 7365.01 1042.6
0 -2 -13 5278.47 811.436
0 2 -13 3984.64 722.893
0 2 -13 5125.33 642.93
0 2 -13 4738.11 763.914
0 2 -14 6594.96 675.282
0 -2 -14 7568.5 748.482
0 4 0 13696.7 1002.54
0 -4 0 9935.45 1281.86
0 -4 -1 10239.7 1378.55
0 4 -1 9842.09 938.762
0 4 -2 36728.5 1830.83
0 -4 -2 31997 2412.38
0 4 -3 15742.4 1298.88
0 -4 -3 13133.8 1833.89
0 4 -4 4023.93 764.168
0 -4 -4 4221.91 590.728
0 4 -4 4426.55 918.67
0 -4 -4 3187.44 1038.01
0 4 -5 4958.17 997.12
0 -4 -5 4886.11 1232.3
0 4 -5 4585.49 804.516
0 4 -6 22530.5 1656.9
0 -4 -6 21860.2 2241.95
0 -4 6 22635.8 1174.11
0 4 -6 24322.7 1667.65
0 4 -7 29625.1 1808.54
0 4 -7 30673 1452.36
0 -4 -7 27975.4 2399.14
0 4 -8 1129.25 391.567
0 -4 -8 657.438 644.889
0 4 -8 950.284 608.819
0 4 -9 2001.48 608.06
0 4 -9 1128.89 373.403
0 -4 -9 1611.47 695.862
0 4 -10 763.437 418.074
0 -4 -10 1471.02 543.585
0 4 -10 1250.5 339.463
1 -1 -15 2347.33 466.563
1 -1 -14 3189.49 676.251
1 1 -14 4441.97 799.542
1 1 -13 14361.7 1402.7
1 1 -13 14454.7 982.453
1 -1 -13 14478.7 1437.32
1 1 -13 14068.7 1063.64
1 1 -13 14675.4 1299.9
1 1 -12 5741.14 943.289
1 1 -12 4160.37 739.724
1 1 -12 4540.81 700.034
1 1 -12 5071.84 1079.21
1 -1 -11 26719.8 1987.83
1 1 -11 25963.5 1595.76
1 1 -11 24986.1 1491
1 1 -11 25452.3 1819.43
1 1 -11 24952.6 1787.01
1 1 -10 66356.5 2481.97
1 1 -10 65099.7 2679.74
1 1 -10 64718.4 2829.09
1 1 -10 66589.2 2434.27
1 -1 -10 64891.6 2934.34
1 1 -9 24683.6 1378.26
1 1 -9 22942.8 1528.45
1 1 -9 20791 1532.59
-1 1 9 21646.3 1840.11
1 -1 -9 21809.4 1582.34
1 1 -9 23121.1 1368.4
-1 1 8 7725.21 1158.66
-1 1 7 218.646 451.438
-1 1 6 113725 3888.23
-1 -1 6 107391 2744.09
1 1 -6 115990 4091.74
-1 -1 5 102657 2661.23
1 1 -5 107323 3555.24
-1 1 5 105662 3565.81
1 1 -4 25538.7 1531.14
-1 -1 4 27977.5 1270.23
-1 1 4 25607 1589.12
-1 1 3 71839.1 2435.5
1 1 -3 67897.9 2190.33
1 -1 -2 128867 2976.13
1 1 -2 121020 2502.97
1 1 -1 677468 7920.49
1 -1 -1 698173 9186.69
-1 -1 1 676204 9042.45
-1 1 0 145226 2572.92
1 -1 0 141107 2984.08
-1 1 0 142340 1953.02
-1 -1 0 144044 3080.43
-1 -1 -1 282788 4745.88
1 -1 1 276493 4471.42
-1 1 -1 272895 3851.22
-1 1 -1 267317 3574.54
-1 -1 -2 28294.4 1332.57
-1 1 -2 29974.9 1200.78
1 -1 2 28780.4 1167.12
-1 -1 -3 88753.4 2514.4
-1 1 -3 93214.4 2577.35
1 -1 4 12468.4 794.461
-1 1 -4 8380.17 924.172
1 1 5 94161.5 3488.26
1 -1 5 103881 2395.85
-1 1 -5 97907.2 3435.62
-1 1 -6 230507 6022.81
1 1 6 227502 5900.56
1 1 7 102337 3909.15
-1 1 -7 105944 4275.72
1 1 8 7287.71 1114.51
-1 -1 -9 5312.11 850.399
-1 1 -9 6695.26 751.47
1 1 9 7021.36 1122.85
-1 1 -9 7196.5 965.856
-1 1 -9 4823.21 795.76
-1 1 -9 5670.86 747.008
-1 1 -10 3104.57 826.074
-1 1 -10 3556.48 666.747
-1 1 -10 3184.02 653.027
-1 -1 -10 4488.33 878.502
-1 1 -10 3416.99 841.382
-1 1 -11 37679.4 2164.88
-1 -1 -11 39929.6 2417.67
-1 1 -11 35671.7 2192.4
-1 1 -11 38842.2 1847.11
-1 1 -11 37339.9 1965.55
-1 1 -12 14397.5 1465.77
-1 -1 -12 18931.6 1714.64
-1 1 -12 18881.3 1558.52
-1 1 -12 16677.3 1313.82
-1 1 -12 17777.2 1189.1
-1 1 -13 7229.38 972.652
-1 1 -13 8749.06 1128.34
-1 1 -13 6534.91 775.682
-1 1 -13 7053.49 690.884
-1 1 -14 9745.42 1018.47
-1 -1 -14 7868.7 937.344
-1 -1 -15 5728.46 599.205
1 3 -13 2676.14 439.15
1 -3 -12 10599.9 801.824
1 3 -12 10750.8 909.494
1 3 -12 8833.97 795.156
1 3 -12 8891.29 845.879
1 -3 -11 21702.2 1350.09
1 3 -11 19498 1354.94
1 3 -11 21453.7 1447.09
1 3 -11 22686.6 1416.86
1 3 -10 9556.57 1055.67
1 3 -10 8139.41 1103.91
1 -3 -10 9417.53 1010.51
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