#------------------------------------------------------------------------------
#$Date: 2020-08-29 08:09:17 +0300 (Sat, 29 Aug 2020) $
#$Revision: 255745 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/35/2243568.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_2243568
loop_
_publ_author_name
'Ouiyangkul, Passaporn'
'Saithong, Saowanit'
'Tantishaiyakul, Vimon'
_publ_section_title
;
Syntheses and crystal structures of hydrated and anhydrous 1:2 cocrystals
of oxyresveratrol and zwitterionic proline
;
_journal_coeditor_code HB7935
_journal_issue 9
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 1528
_journal_page_last 1534
_journal_paper_doi 10.1107/S2056989020011536
_journal_volume 76
_journal_year 2020
_chemical_absolute_configuration unk
_chemical_formula_iupac 'C14 H12 O4, 2C5 H9 N O2'
_chemical_formula_moiety 'C14 H12 O4, 2(C5 H9 N O2)'
_chemical_formula_sum 'C24 H30 N2 O8'
_chemical_formula_weight 474.50
_chemical_name_systematic
;
4-[(E)-2-(3,5-Dihydroxyphenyl)ethenyl]benzene-1,3-diol
bis[(S)-pyrrolidin-1-ium-2-carboxylate]
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.8293(2)
_cell_length_b 10.4915(2)
_cell_length_c 22.9863(6)
_cell_measurement_reflns_used 9885
_cell_measurement_temperature 297(2)
_cell_measurement_theta_max 33.70
_cell_measurement_theta_min 2.97
_cell_volume 2370.44(9)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 297(2)
_diffrn_detector
'PHOTON II Charge-Integrating Pixel Array area detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device 'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type 'Bruker D8 VENTURE'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'graphiteDouble Bounce Multilayer Mirror'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0190
_diffrn_reflns_av_unetI/netI 0.0139
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 22887
_diffrn_reflns_theta_full 24.990
_diffrn_reflns_theta_max 24.990
_diffrn_reflns_theta_min 2.975
_diffrn_source 'Sealed x-ray tube'
_exptl_absorpt_coefficient_mu 0.100
_exptl_absorpt_correction_T_max 0.7467
_exptl_absorpt_correction_T_min 0.6557
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.330
_exptl_crystal_description Block
_exptl_crystal_F_000 1008
_exptl_crystal_size_max 0.462
_exptl_crystal_size_mid 0.328
_exptl_crystal_size_min 0.188
_refine_diff_density_max 0.618
_refine_diff_density_min -0.223
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.088
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 317
_refine_ls_number_reflns 4084
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.089
_refine_ls_R_factor_all 0.0473
_refine_ls_R_factor_gt 0.0469
_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^)+(0.0845P)^2^+0.7969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1332
_refine_ls_wR_factor_ref 0.1338
_reflns_number_gt 4038
_reflns_number_total 4084
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb7935sup1.cif
_cod_data_source_block II
_cod_original_formula_sum 'C24 H30 N2 O8 '
_cod_database_code 2243568
_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 0.955
_shelx_estimated_absorpt_t_max 0.981
_shelx_hkl_file
;
3 0 0 4.70 0.80
3 0 0 4.20 0.60
3 0 0 3.50 0.50
-3 0 0 2.70 0.60
-3 0 0 3.00 0.80
-3 0 0 3.60 0.70
-4 0 0 283.17 9.00
4 0 0 326.97 8.90
4 0 0 294.07 9.30
-4 0 0 322.57 9.10
-4 0 0 295.57 9.20
-5 0 0 -0.50 0.90
5 0 0 -1.00 1.10
-5 0 0 -2.10 1.00
-5 0 0 0.90 0.90
6 0 0 3212.28 91.39
-6 0 0 3174.18 91.19
-6 0 0 3219.98 91.19
-6 0 0 3209.48 91.39
-7 0 0 -0.50 1.30
7 0 0 -3.10 1.60
-7 0 0 0.70 1.30
-7 0 0 -2.00 1.40
-8 0 0 102.39 4.30
-8 0 0 99.99 4.80
8 0 0 101.79 5.00
-8 0 0 106.59 4.50
9 0 0 -2.70 2.10
-9 0 0 -1.20 1.70
10 0 0 155.98 8.00
-10 0 0 147.49 6.20
11 0 0 1.00 2.60
-11 0 0 -1.00 2.10
12 0 0 200.68 8.50
-12 0 0 178.48 7.70
-13 0 0 1.70 2.60
13 0 0 3.00 3.10
-14 0 0 -0.70 2.70
14 0 0 -1.40 3.30
15 0 0 -2.30 3.60
-15 0 0 3.70 3.10
-3 -1 0 538.25 15.50
-3 1 0 541.65 15.60
3 1 0 547.35 15.50
3 -1 0 549.65 15.60
-3 1 0 548.65 15.60
-3 1 0 513.25 15.70
3 -1 0 533.25 15.70
3 -1 0 515.75 15.50
-4 1 0 2968.00 85.39
-4 -1 0 2940.81 84.99
-4 1 0 2971.00 85.29
4 1 0 2910.51 85.39
-4 -1 0 3066.59 84.99
-4 -1 0 3094.79 85.19
4 -1 0 3013.30 85.19
-4 1 0 3058.39 85.29
4 -1 0 2970.50 85.39
5 -1 0 829.42 24.00
-5 1 0 817.32 24.30
-5 1 0 799.32 24.10
5 -1 0 839.22 24.40
-5 1 0 855.11 24.20
-5 -1 0 842.22 23.90
-5 -1 0 854.01 23.90
5 -1 0 805.42 24.30
5 1 0 824.22 24.10
-5 -1 0 843.02 24.10
-6 -1 0 47.00 2.20
-6 1 0 44.10 2.70
-6 -1 0 47.40 2.20
-6 -1 0 40.30 2.60
-6 1 0 45.90 2.90
6 1 0 41.90 2.90
-6 1 0 42.90 2.70
6 -1 0 39.20 3.10
-7 -1 0 2318.57 65.59
-7 1 0 2333.57 65.89
7 1 0 2373.16 65.99
-7 -1 0 2285.97 65.59
-7 1 0 2301.57 66.09
7 -1 0 2246.08 65.39
7 -1 0 2310.57 66.19
-7 -1 0 2277.97 65.89
7 -1 0 2296.57 65.49
-7 1 0 2256.17 65.89
8 -1 0 2274.57 64.19
-8 -1 0 2222.78 63.59
-8 -1 0 2178.58 63.89
-8 1 0 2196.68 63.89
8 1 0 2248.08 63.89
-8 -1 0 2141.09 63.59
-8 1 0 2297.77 63.89
-9 -1 0 117.39 5.10
9 -1 0 125.79 6.40
9 1 0 141.19 6.10
-9 -1 0 135.39 5.30
-9 1 0 141.69 5.90
-10 -1 0 279.97 9.60
-10 1 0 290.67 10.10
10 -1 0 290.57 10.70
10 1 0 292.97 10.20
11 -1 0 99.29 6.40
-11 -1 0 102.99 5.10
11 1 0 108.79 6.00
-11 1 0 99.89 5.70
-12 -1 0 43.60 3.50
-12 1 0 46.40 4.80
12 1 0 41.70 3.90
12 -1 0 57.89 5.90
-13 -1 0 165.28 7.20
13 -1 0 174.38 8.70
13 1 0 166.18 8.00
-13 1 0 163.98 7.80
-14 1 0 39.10 4.30
-14 -1 0 41.80 5.90
14 -1 0 40.80 4.70
14 1 0 37.50 4.10
-15 1 0 50.39 4.80
-15 -1 0 51.39 5.20
15 -1 0 52.89 5.20
15 1 0 49.20 4.80
-3 2 0 1378.46 40.50
3 -2 0 1413.26 40.50
3 -2 0 1427.96 40.50
-3 -2 0 1412.56 40.20
-3 2 0 1403.16 40.50
3 2 0 1456.05 40.20
3 -2 0 1396.66 40.50
4 -2 0 1085.19 30.20
-4 2 0 1042.10 30.30
-4 -2 0 1008.00 30.10
-4 2 0 1068.89 30.30
4 2 0 1050.49 29.90
-4 2 0 1022.50 30.30
4 -2 0 1033.20 30.30
4 -2 0 1058.99 30.20
-5 2 0 3592.04 103.79
-5 -2 0 3701.13 103.49
-5 2 0 3663.23 103.79
-5 2 0 3665.63 103.89
5 -2 0 3590.64 103.89
5 -2 0 3635.24 103.69
5 -2 0 3696.13 103.69
5 2 0 3618.14 103.49
-6 -2 0 1219.08 34.60
-6 -2 0 1231.18 35.00
6 2 0 1188.78 34.90
6 -2 0 1192.38 35.40
6 -2 0 1228.88 35.00
6 -2 0 1197.88 35.00
-6 2 0 1219.98 35.20
-6 2 0 1224.68 35.40
-7 -2 0 375.86 11.30
7 -2 0 391.56 12.30
-7 -2 0 380.06 11.30
7 2 0 389.16 11.80
-7 2 0 374.66 12.00
7 -2 0 367.26 11.60
-7 -2 0 378.76 11.70
7 -2 0 400.96 11.70
-7 2 0 371.06 12.00
8 -2 0 27.80 2.90
-8 -2 0 33.90 2.40
-8 -2 0 29.90 2.20
8 -2 0 26.00 2.30
-8 2 0 32.50 3.40
8 -2 0 25.60 2.10
-8 -2 0 30.10 2.70
8 2 0 21.10 2.30
9 2 0 770.42 22.80
-9 2 0 730.73 23.00
9 -2 0 790.12 22.20
9 -2 0 730.03 22.10
-9 -2 0 739.13 22.70
-9 -2 0 788.52 22.40
-10 -2 0 671.53 20.20
10 -2 0 687.03 21.30
10 2 0 679.83 20.70
-10 2 0 726.83 21.10
-10 -2 0 621.54 20.50
-11 2 0 372.16 13.00
11 -2 0 376.36 13.40
-11 -2 0 379.86 12.10
11 2 0 380.26 12.70
-12 -2 0 41.10 3.30
-12 2 0 39.40 4.00
12 -2 0 42.20 4.30
12 2 0 56.39 5.10
13 -2 0 32.10 4.50
-13 -2 0 39.00 4.00
-13 2 0 30.60 3.90
13 2 0 32.60 3.70
14 2 0 46.60 4.20
-14 -2 0 43.10 4.50
14 -2 0 41.60 6.00
-14 2 0 48.40 4.70
-15 2 0 8.60 3.70
15 -2 0 6.30 3.90
0 3 0 1.20 0.60
0 -3 0 4.30 0.90
0 -3 0 0.20 0.70
0 -3 0 1.30 0.70
0 3 0 2.20 0.80
-1 3 0 914.31 24.70
-1 -3 0 839.72 24.60
1 -3 0 894.61 24.70
-1 -3 0 861.41 24.40
1 -3 0 841.82 24.80
-1 -3 0 802.92 24.60
1 3 0 845.52 24.60
1 3 0 875.01 24.60
-2 3 0 1132.99 32.70
2 -3 0 1101.79 32.70
2 -3 0 1090.09 32.70
2 -3 0 1180.28 32.70
-2 3 0 1166.88 32.80
-2 -3 0 1104.19 32.30
-2 3 0 1167.28 32.70
-2 -3 0 1146.89 32.40
4 3 0 2565.44 71.09
4 -3 0 2474.65 71.69
-4 3 0 2488.45 71.69
-4 -3 0 2488.15 71.09
-4 3 0 2555.04 71.69
-4 3 0 2531.35 71.69
4 -3 0 2514.05 71.69
4 -3 0 2446.16 71.59
-5 -3 0 1404.56 40.10
5 -3 0 1412.66 40.60
-5 3 0 1407.86 40.50
5 3 0 1440.16 39.90
5 -3 0 1329.87 40.30
5 -3 0 1396.46 40.40
-6 3 0 70.49 3.70
-6 3 0 75.69 3.90
6 -3 0 77.99 4.20
6 3 0 79.49 3.10
-6 -3 0 74.99 3.00
6 -3 0 70.29 3.70
-6 3 0 70.99 3.80
6 -3 0 70.99 3.40
7 -3 0 -0.70 1.70
-7 -3 0 0.40 1.20
7 -3 0 -0.10 1.40
-7 3 0 3.30 2.00
7 3 0 2.70 1.50
7 -3 0 -1.40 2.00
-8 -3 0 139.09 5.30
8 3 0 139.29 5.50
-8 3 0 151.88 6.30
8 -3 0 134.49 5.40
-8 -3 0 148.49 4.90
8 -3 0 145.79 6.70
-8 -3 0 148.19 4.90
8 -3 0 151.98 5.70
9 3 0 209.58 7.40
-9 3 0 207.28 8.10
9 -3 0 208.78 7.40
9 -3 0 198.38 7.00
9 -3 0 210.58 8.50
-9 -3 0 185.88 7.40
-9 -3 0 218.58 6.80
-9 -3 0 196.18 6.70
-10 -3 0 4.90 1.80
-10 -3 0 5.40 1.50
-10 3 0 3.80 2.50
-10 -3 0 7.20 1.90
10 -3 0 5.00 1.50
10 -3 0 1.40 1.70
10 3 0 4.50 2.20
10 -3 0 2.30 2.80
-11 3 0 170.68 7.80
11 -3 0 173.08 8.30
11 3 0 168.18 6.90
-11 -3 0 165.18 6.20
12 -3 0 71.09 6.50
-12 3 0 59.89 5.60
-12 -3 0 47.20 3.70
13 -3 0 34.40 4.40
13 3 0 42.10 3.50
-13 -3 0 34.60 3.60
-13 3 0 32.80 4.10
-14 3 0 10.90 3.70
-14 -3 0 6.00 2.40
14 -3 0 12.40 4.20
15 -3 0 2.60 4.00
-15 3 0 4.00 3.70
-1 4 0 43.10 2.40
1 -4 0 47.40 2.40
1 4 0 39.70 1.90
1 4 0 40.50 2.00
1 4 0 39.90 1.60
-1 -4 0 40.80 2.10
-1 -4 0 38.80 1.70
-1 -4 0 38.30 2.00
1 -4 0 41.50 2.40
-1 4 0 41.10 2.30
-1 4 0 39.90 2.10
1 -4 0 37.40 2.20
2 -4 0 695.33 20.80
-2 4 0 740.33 20.80
2 -4 0 687.73 20.90
-2 -4 0 693.33 20.50
2 -4 0 700.93 20.80
-2 -4 0 708.53 20.50
-2 4 0 742.53 20.90
-3 -4 0 3533.25 101.09
3 -4 0 3567.24 101.59
-3 4 0 3625.84 101.69
3 -4 0 3520.15 101.69
3 -4 0 3519.25 101.59
-3 -4 0 3587.04 101.09
-3 4 0 3542.35 101.59
-3 4 0 3645.34 101.69
4 -4 0 6286.67 180.78
-4 4 0 6361.06 180.78
4 -4 0 6356.86 180.78
-4 4 0 6397.36 180.88
4 -4 0 6423.16 180.78
-5 4 0 2336.07 68.59
5 -4 0 2396.06 68.59
-5 4 0 2421.56 68.69
5 -4 0 2430.76 68.69
5 -4 0 2389.36 68.69
-5 4 0 2370.56 68.69
6 4 0 275.47 8.20
-6 -4 0 273.17 8.30
-6 4 0 273.87 9.30
6 -4 0 250.87 9.30
6 -4 0 277.37 9.40
6 -4 0 280.17 9.10
7 -4 0 258.27 9.50
7 4 0 270.77 8.20
7 -4 0 246.48 8.90
-7 4 0 272.27 9.40
7 -4 0 266.67 9.10
-7 -4 0 269.97 8.20
8 -4 0 32.30 3.40
-8 4 0 39.10 3.50
8 -4 0 32.30 3.00
-8 -4 0 39.70 2.50
8 -4 0 30.90 3.20
8 4 0 29.80 2.80
9 4 0 6.90 1.70
9 -4 0 9.40 1.90
9 -4 0 4.90 2.70
-9 -4 0 4.90 1.40
-9 4 0 6.10 2.50
-10 -4 0 12.20 2.00
-10 4 0 10.40 2.90
10 4 0 7.70 1.90
10 -4 0 12.60 2.30
-10 -4 0 12.40 1.60
10 -4 0 10.20 2.40
10 -4 0 11.20 3.10
11 4 0 117.99 5.10
-11 4 0 109.89 6.70
11 -4 0 118.69 5.20
11 -4 0 103.39 4.70
11 -4 0 118.49 7.30
-12 -4 0 382.66 12.60
-12 4 0 424.56 14.60
12 -4 0 411.86 14.90
13 -4 0 53.59 8.70
-13 -4 0 38.90 3.40
-13 4 0 41.50 4.80
14 -4 0 12.40 4.20
-14 4 0 1.60 3.70
0 5 0 0.00 1.10
0 -5 0 -0.90 1.10
0 5 0 -3.50 1.00
0 -5 0 -0.80 1.10
0 -5 0 0.80 1.20
-1 5 0 3099.39 86.99
1 5 0 3074.29 86.89
-1 -5 0 3033.40 86.99
-1 -5 0 3103.29 86.69
-1 5 0 3076.79 87.19
1 5 0 3045.40 86.69
-1 5 0 3004.90 87.09
-1 -5 0 3085.89 86.99
1 -5 0 3022.00 87.19
1 5 0 3028.50 86.89
1 -5 0 3069.19 86.99
1 -5 0 3034.30 87.19
-2 5 0 587.24 17.40
2 -5 0 585.44 17.40
-2 -5 0 603.24 17.20
2 -5 0 583.54 17.70
-2 5 0 590.04 17.60
-2 5 0 590.54 17.60
-2 -5 0 582.14 17.20
2 -5 0 584.24 17.50
2 5 0 590.94 16.90
2 5 0 576.94 16.90
-3 -5 0 4025.90 113.99
-3 5 0 4025.40 114.59
-3 -5 0 4043.90 113.99
-3 5 0 4016.20 114.39
3 -5 0 3968.30 114.59
3 -5 0 4025.40 114.49
4 -5 0 756.42 22.40
4 -5 0 731.33 22.30
-4 5 0 739.73 22.40
-4 5 0 743.23 22.40
4 -5 0 767.22 22.40
-4 -5 0 753.82 21.60
-4 -5 0 748.03 21.60
-4 5 0 751.22 22.30
5 -5 0 1491.65 43.10
-5 5 0 1467.35 43.10
5 -5 0 1506.25 43.10
5 -5 0 1446.16 42.90
6 -5 0 266.27 9.10
6 -5 0 246.98 8.70
6 -5 0 252.37 9.20
-6 5 0 260.87 9.20
7 -5 0 350.86 11.80
7 -5 0 351.46 12.30
-7 5 0 355.36 12.10
-8 5 0 1102.79 32.90
8 -5 0 1091.59 32.60
8 -5 0 1097.29 33.00
9 -5 0 129.59 7.00
9 -5 0 128.99 6.10
-9 5 0 142.09 6.90
10 -5 0 28.70 3.80
10 -5 0 27.50 3.30
-10 5 0 26.00 3.50
-11 5 0 6.10 3.20
11 -5 0 7.00 2.40
11 -5 0 5.30 2.00
11 -5 0 5.10 3.40
12 -5 0 25.20 4.50
-12 5 0 22.70 4.20
12 -5 0 22.50 3.50
-13 5 0 218.58 10.40
13 -5 0 217.98 10.80
14 -5 0 7.70 4.20
-14 5 0 3.00 6.60
0 -6 0 3378.06 94.29
0 6 0 3307.87 94.49
0 -6 0 3267.77 94.69
0 6 0 3351.46 94.59
0 6 0 3277.77 94.29
0 -6 0 3321.97 94.59
-1 6 0 713.23 21.20
1 6 0 705.93 20.90
1 6 0 727.43 20.90
1 -6 0 714.43 21.30
1 -6 0 726.93 21.00
1 -6 0 724.93 21.30
-1 -6 0 726.53 20.60
-1 6 0 709.13 21.20
-1 -6 0 706.73 21.00
-1 6 0 704.93 20.90
-1 -6 0 726.93 21.10
1 6 0 690.53 20.90
2 -6 0 1084.49 32.50
-2 -6 0 1107.79 32.20
2 -6 0 1041.60 32.50
2 6 0 1099.39 31.80
2 6 0 1148.69 31.90
-2 6 0 1142.79 32.50
-2 6 0 1102.99 32.30
2 -6 0 1135.29 32.30
-2 -6 0 1137.79 32.20
-3 -6 0 267.47 9.30
3 -6 0 290.07 9.70
3 -6 0 277.07 9.50
-3 6 0 288.17 9.60
3 -6 0 288.57 9.50
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1 -3 9 1910.81 57.69
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1 3 -9 2066.79 57.69
-1 -3 -9 2071.99 57.59
-1 3 9 1987.40 57.69
1 3 -9 2033.30 57.69
-1 3 9 2037.20 57.69
1 -3 9 2011.90 57.79
-1 -3 9 2033.00 57.69
1 -3 -9 2041.50 57.69
-1 3 -9 2016.10 57.79
-1 -3 9 1974.60 57.79
1 3 9 2052.09 57.49
1 3 9 2008.80 57.49
1 -3 -9 1991.80 57.69
1 -3 -9 1996.50 57.79
-1 3 -9 1986.10 57.79
2 3 -9 1926.71 53.79
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2 3 -9 1894.81 53.79
-2 3 9 1904.01 53.89
2 -3 9 1815.02 53.79
-2 -3 -9 1868.61 53.59
2 -3 9 1884.81 53.89
-2 3 -9 1924.21 53.89
2 3 9 1850.31 53.39
-2 -3 9 1804.32 53.79
2 -3 -9 1888.71 53.89
-2 3 -9 1826.72 53.89
2 -3 -9 1863.51 53.89
-2 -3 9 1931.81 53.89
2 -3 -9 1860.91 53.89
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4 -3 9 78.49 3.80
-4 -3 -9 83.39 3.10
-4 -3 -9 81.89 3.00
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4 -3 9 67.49 3.40
4 3 -9 88.49 3.30
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4 3 -9 81.89 3.30
4 -3 -9 80.59 4.00
4 -3 -9 82.49 3.70
-4 3 -9 73.49 3.80
4 -3 -9 78.59 4.00
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5 3 -9 65.99 3.10
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5 -3 9 56.79 3.30
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5 3 -9 76.69 3.00
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5 -3 9 73.89 3.70
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5 -3 -9 66.79 4.00
5 -3 -9 63.79 3.90
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6 -3 9 46.70 3.00
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6 -3 -9 44.90 3.20
6 -3 -9 53.39 3.90
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6 -3 -9 47.60 4.00
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7 -3 9 488.15 15.40
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8 -3 9 115.99 4.70
8 3 -9 124.99 5.30
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8 -3 -9 116.99 5.60
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8 -3 -9 119.89 6.20
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9 -3 9 264.07 8.80
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9 -3 -9 256.87 10.40
9 -3 -9 268.77 9.70
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11 -3 -9 51.79 4.70
11 -3 -9 45.70 3.50
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12 -3 -9 110.79 5.00
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13 -3 -9 2.40 3.80
14 3 -9 29.50 4.00
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14 -3 -9 42.20 5.40
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0 4 -9 1.50 1.20
0 -4 -9 2.70 1.10
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1 4 -9 7360.56 216.88
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1 -4 9 7333.27 217.28
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1 4 9 7865.61 216.68
1 -4 -9 7602.74 217.28
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1 4 9 7630.14 216.68
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2 -4 9 3321.57 94.19
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2 4 -9 3298.87 93.89
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2 -4 -9 3213.18 94.09
2 4 9 3339.77 93.59
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2 -4 -9 3261.77 94.09
2 -4 -9 3329.67 94.09
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3 -4 9 144.59 5.70
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3 -4 9 140.29 5.50
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3 -4 -9 138.69 5.50
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3 -4 -9 139.39 5.40
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4 -4 9 500.65 15.00
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4 -4 9 446.76 14.80
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4 -4 -9 468.45 14.90
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5 -4 9 124.49 5.20
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5 -4 -9 129.09 5.70
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6 -4 9 181.18 6.60
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11 -4 -9 43.00 4.70
11 -4 -9 43.10 4.60
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1 -5 9 555.94 17.20
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1 5 -9 585.44 17.00
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1 -5 -9 575.64 16.90
1 -5 -9 547.35 17.00
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3 -5 9 545.95 17.40
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3 5 -9 571.04 17.10
3 -5 -9 570.94 17.60
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7 -5 -9 163.88 7.70
7 -5 -9 166.98 7.40
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8 -5 -9 24.30 3.30
8 -5 -9 21.20 3.10
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9 -5 9 34.90 3.90
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9 -5 -9 37.10 4.20
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9 -5 -9 38.00 3.70
10 -5 9 79.39 6.30
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10 -5 -9 69.69 6.30
10 -5 -9 65.79 5.30
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11 -5 -9 142.79 8.50
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12 -5 -9 61.09 5.00
12 -5 -9 51.29 5.60
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0 -6 -9 533.15 16.70
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0 -6 -9 524.45 16.60
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1 -6 9 1958.80 56.09
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1 6 -9 1880.71 55.69
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1 -6 -9 1956.10 55.69
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1 -6 -9 1940.71 55.89
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0 2 -35 121.59 8.50
0 2 35 112.99 8.00
-1 2 35 74.29 7.60
-1 -2 -35 73.29 7.70
1 -2 35 84.39 8.20
1 2 -35 75.99 7.70
-1 -2 35 80.89 8.40
-1 2 -35 85.09 7.90
1 2 35 73.19 7.10
1 -2 -35 82.49 7.90
2 2 -35 29.90 4.80
2 -2 35 19.00 4.60
-2 -2 -35 28.00 4.80
-2 2 35 17.10 4.80
-2 2 -35 20.70 4.30
-2 -2 35 19.60 5.40
2 -2 -35 23.80 4.70
2 -2 -35 19.70 4.60
2 2 35 16.80 4.00
0 3 35 11.60 4.20
0 -3 -35 7.60 4.20
0 -3 35 3.20 4.40
0 3 -35 7.20 4.40
-1 -3 -35 24.60 4.70
1 3 -35 21.20 4.50
1 -3 35 28.40 5.20
-1 3 35 25.20 4.70
1 -3 -35 29.30 4.90
1 -3 -35 29.70 5.00
-1 3 -35 34.20 5.10
-1 -3 35 29.00 5.50
1 3 35 32.70 4.60
2 -3 35 0.00 4.20
-2 -3 35 2.80 4.50
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 28405
_shelx_res_file
;
TITL 3_0m_a.res in P2(1)2(1)2(1)
shelx.res
created by SHELXL-2018/3 at 10:21:13 on 15-Mar-2020
CELL 0.71073 9.8293 10.4915 22.9863 90.000 90.000 90.000
ZERR 4.00 0.0002 0.0002 0.0006 0.000 0.000 0.000
LATT -1
SYMM 1/2 + X, 1/2 - Y, - Z
SYMM - X, 1/2 + Y, 1/2 - Z
SYMM 1/2 - X, - Y, 1/2 + Z
SFAC C H N O
UNIT 96 120 8 32
MERG 2
OMIT -3.00 50.00
OMIT 1 3 0
OMIT 3 0 3
OMIT 1 0 3
OMIT 3 2 8
OMIT -3 2 8
OMIT 2 5 0
OMIT 2 4 0
OMIT 4 0 2
OMIT 0 2 3
OMIT 4 0 4
OMIT 0 7 2
DFIX 0.82 0.02 O2 H2'
DFIX 0.82 0.02 O4 H4'
MPLA C1 C2 C3 C4 C5 C6
MPLA C9 C10 C11 C12 C13 C14
HTAB O1 O8
EQIV $1 -x+1/2, -y+1, z+1/2
HTAB N1 O5_$1
EQIV $2 -x, y-1/2, -z+3/2
HTAB N1 O8_$2
EQIV $3 -x+1, y-1/2, -z+1/2
HTAB N2 O4_$3
EQIV $4 x+1/2, -y+1/2, -z+1
HTAB N2 O6_$4
EQIV $5 -x, y+1/2, -z+1/2
HTAB O3 O2_$5
HTAB C6 O6
HTAB O2 O6
EQIV $6 x+1/2, -y+3/2, -z+1
HTAB O4 O7_$6
FMAP 2
PLAN 20
SIZE 0.188 0.328 0.462
ACTA
BOND $H
CONF
LIST 4
L.S. 10
TEMP 24.00
WGHT 0.084500 0.796900
FVAR 1.52644
O1 4 0.125998 0.612842 0.619863 11.00000 0.06275 0.06737 =
0.02411 0.00426 0.00386 0.01266
AFIX 148
H1' 2 0.070676 0.668770 0.642726 11.00000 -1.50000
AFIX 0
N1 3 -0.070462 0.484434 0.795716 11.00000 0.04696 0.02984 =
0.02909 -0.00073 0.00206 0.00011
AFIX 23
H1A 2 -0.014333 0.419063 0.801444 11.00000 -1.20000
H1B 2 -0.056256 0.541800 0.823585 11.00000 -1.20000
AFIX 0
C1 1 0.112605 0.642744 0.563065 11.00000 0.03659 0.04487 =
0.02418 -0.00044 0.00011 -0.00391
O2 4 0.256479 0.531846 0.424955 11.00000 0.04390 0.05694 =
0.02723 -0.00575 -0.00436 0.01944
N2 3 0.783703 0.323452 0.466305 11.00000 0.02970 0.04993 =
0.03721 0.00291 0.00034 0.00401
AFIX 23
H2A 2 0.772557 0.318253 0.427954 11.00000 -1.20000
H2B 2 0.837980 0.260292 0.477681 11.00000 -1.20000
AFIX 0
C2 1 0.026524 0.738227 0.543404 11.00000 0.04943 0.05345 =
0.03304 -0.00228 0.00882 0.01418
AFIX 43
H2 2 -0.024706 0.785813 0.569582 11.00000 -1.20000
AFIX 0
O3 4 -0.249486 0.979817 0.193777 11.00000 0.04586 0.06683 =
0.03573 0.01722 -0.00276 0.00362
AFIX 148
H3' 2 -0.248972 0.987476 0.156195 11.00000 -1.50000
AFIX 0
C3 1 0.017992 0.761599 0.484432 11.00000 0.05169 0.04944 =
0.03548 0.00306 0.00194 0.01930
AFIX 43
H3 2 -0.041818 0.824262 0.471595 11.00000 -1.20000
AFIX 0
O4 4 0.163703 0.750151 0.154159 11.00000 0.06173 0.08247 =
0.03563 0.00223 0.01126 0.01229
C4 1 0.094858 0.695684 0.443064 11.00000 0.03690 0.04260 =
0.02738 0.00214 -0.00072 0.00436
O5 4 0.572907 0.417315 0.410218 11.00000 0.04673 0.08193 =
0.03110 0.01588 0.00147 0.00975
C5 1 0.181219 0.600168 0.464205 11.00000 0.02609 0.03851 =
0.02808 -0.00533 0.00086 -0.00009
O6 4 0.419792 0.368630 0.478226 11.00000 0.03014 0.05785 =
0.05172 0.01399 0.00514 0.00708
C6 1 0.190256 0.573328 0.523245 11.00000 0.03180 0.03751 =
0.02942 0.00091 -0.00351 0.00280
AFIX 43
H6 2 0.247994 0.509154 0.536261 11.00000 -1.20000
AFIX 0
O7 4 -0.089208 0.740570 0.785913 11.00000 0.06428 0.03567 =
0.03816 -0.00748 0.01023 -0.00331
C7 1 0.087471 0.724093 0.380769 11.00000 0.04353 0.04250 =
0.02968 0.00199 0.00314 0.00828
AFIX 43
H7 2 0.156958 0.691646 0.357645 11.00000 -1.20000
AFIX 0
O8 4 -0.029636 0.742813 0.692415 11.00000 0.08343 0.03360 =
0.03469 0.00410 0.01230 -0.00456
C8 1 -0.007558 0.790967 0.354016 11.00000 0.03744 0.05231 =
0.02954 0.00229 0.00168 0.00592
AFIX 43
H8 2 -0.075927 0.825377 0.377158 11.00000 -1.20000
AFIX 0
C9 1 -0.015873 0.816376 0.291177 11.00000 0.03807 0.04031 =
0.02975 0.00337 0.00082 -0.00199
C10 1 -0.123434 0.890870 0.270467 11.00000 0.03661 0.04360 =
0.03102 0.00302 0.00200 -0.00003
AFIX 43
H10 2 -0.185411 0.926232 0.296429 11.00000 -1.20000
AFIX 0
C11 1 -0.137760 0.912091 0.211094 11.00000 0.03756 0.04063 =
0.03150 0.00897 -0.00390 -0.00567
C12 1 -0.042872 0.864431 0.172347 11.00000 0.05179 0.04779 =
0.02359 0.00624 -0.00103 -0.00864
AFIX 43
H12 2 -0.051837 0.880042 0.132705 11.00000 -1.20000
AFIX 0
C13 1 0.066032 0.793009 0.193067 11.00000 0.04848 0.04496 =
0.03237 -0.00008 0.00748 -0.00224
C14 1 0.079270 0.766540 0.251775 11.00000 0.04166 0.04478 =
0.03329 0.00399 0.00179 0.00138
AFIX 43
H14 2 0.150671 0.716115 0.265004 11.00000 -1.20000
AFIX 0
C15 1 0.538808 0.372191 0.456880 11.00000 0.03052 0.03888 =
0.02937 0.00289 -0.00077 0.00195
C16 1 0.649624 0.315027 0.496515 11.00000 0.03229 0.04577 =
0.03539 0.01045 0.00010 0.00180
AFIX 13
H16 2 0.628213 0.226093 0.505799 11.00000 -1.20000
AFIX 0
C17 1 0.671354 0.391919 0.552576 11.00000 0.05781 0.10264 =
0.02945 -0.00195 -0.00438 0.00445
AFIX 23
H17A 2 0.588047 0.434238 0.564351 11.00000 -1.20000
H17B 2 0.701960 0.337248 0.583990 11.00000 -1.20000
AFIX 0
C18 1 0.778635 0.487087 0.536704 11.00000 0.11073 0.12057 =
0.09316 -0.06247 0.02265 -0.05155
AFIX 23
H18A 2 0.737801 0.570706 0.532318 11.00000 -1.20000
H18B 2 0.845990 0.491800 0.567471 11.00000 -1.20000
AFIX 0
C19 1 0.843950 0.449710 0.482470 11.00000 0.05351 0.06307 =
0.08265 -0.00333 0.00480 -0.01803
AFIX 23
H19A 2 0.941535 0.442251 0.487748 11.00000 -1.20000
H19B 2 0.826332 0.512272 0.452326 11.00000 -1.20000
AFIX 0
C20 1 -0.045618 0.542555 0.737198 11.00000 0.04043 0.02941 =
0.02801 -0.00174 0.00352 -0.00220
AFIX 13
H20 2 0.044694 0.517884 0.723075 11.00000 -1.20000
AFIX 0
C21 1 -0.155300 0.484873 0.697882 11.00000 0.07818 0.05335 =
0.04343 -0.00787 -0.01741 -0.01390
AFIX 23
H21A 2 -0.208778 0.551754 0.679827 11.00000 -1.20000
H21B 2 -0.113911 0.433781 0.667490 11.00000 -1.20000
AFIX 0
C22 1 -0.242896 0.404089 0.735644 11.00000 0.07286 0.08851 =
0.08774 0.00830 -0.02745 -0.04444
AFIX 23
H22A 2 -0.338064 0.418173 0.726516 11.00000 -1.20000
H22B 2 -0.222303 0.314678 0.729493 11.00000 -1.20000
AFIX 0
C23 1 -0.214935 0.440012 0.796995 11.00000 0.04896 0.05668 =
0.06930 0.01180 0.01882 -0.00527
AFIX 23
H23A 2 -0.225509 0.367342 0.822688 11.00000 -1.20000
H23B 2 -0.275284 0.507642 0.809722 11.00000 -1.20000
AFIX 0
C24 1 -0.055863 0.687523 0.740159 11.00000 0.04196 0.03206 =
0.03086 -0.00231 0.00386 -0.00601
H2' 2 0.311059 0.483694 0.440792 11.00000 -1.50000
H4' 2 0.233860 0.736243 0.177462 11.00000 -1.50000
HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00
REM 3_0m_a.res in P2(1)2(1)2(1)
REM wR2 = 0.1338, GooF = S = 1.088, Restrained GooF = 1.089 for all data
REM R1 = 0.0469 for 4038 Fo > 4sig(Fo) and 0.0473 for all 4084 data
REM 317 parameters refined using 2 restraints
END
WGHT 0.0845 0.7966
REM Highest difference peak 0.618, deepest hole -0.223, 1-sigma level 0.044
Q1 1 0.3430 0.6399 0.1221 11.00000 0.05 0.62
Q2 1 0.0864 0.3538 0.6031 11.00000 0.05 0.61
Q3 1 0.0780 0.7364 0.1350 11.00000 0.05 0.49
Q4 1 0.0094 0.7336 0.7920 11.00000 0.05 0.26
Q5 1 -0.0115 0.7907 0.1807 11.00000 0.05 0.20
Q6 1 0.0220 0.7635 0.2283 11.00000 0.05 0.18
Q7 1 -0.1240 0.8596 0.1729 11.00000 0.05 0.18
Q8 1 0.7547 0.4908 0.4448 11.00000 0.05 0.17
Q9 1 -0.0568 0.6082 0.7378 11.00000 0.05 0.16
Q10 1 0.7942 0.5458 0.5591 11.00000 0.05 0.15
Q11 1 0.8840 0.4201 0.5143 11.00000 0.05 0.15
Q12 1 -0.2445 0.4787 0.7198 11.00000 0.05 0.15
Q13 1 0.7008 0.5763 0.4855 11.00000 0.05 0.15
Q14 1 0.7175 0.4714 0.5377 11.00000 0.05 0.14
Q15 1 0.0587 0.6881 0.4154 11.00000 0.05 0.14
Q16 1 -0.0625 0.9443 0.1962 11.00000 0.05 0.14
Q17 1 0.0645 0.7280 0.6842 11.00000 0.05 0.13
Q18 1 0.4197 0.3425 0.5195 11.00000 0.05 0.13
Q19 1 0.9247 0.5941 0.5820 11.00000 0.05 0.13
Q20 1 -0.4190 0.4435 0.7992 11.00000 0.05 0.12
;
_shelx_res_checksum 10440
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, 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_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.1260(3) 0.6128(3) 0.61986(10) 0.0514(7) Uani d 1 . .
H H1' 0.071(6) 0.669(5) 0.6427(14) 0.077 Uiso calc 1 . .
N N1 -0.0705(3) 0.4844(2) 0.79572(11) 0.0353(6) Uani d 1 . .
H H1A -0.014333 0.419063 0.801444 0.042 Uiso calc 1 . .
H H1B -0.056256 0.541800 0.823585 0.042 Uiso calc 1 . .
C C1 0.1126(3) 0.6427(3) 0.56307(13) 0.0352(7) Uani d 1 . .
O O2 0.2565(2) 0.5318(3) 0.42496(9) 0.0427(6) Uani d 1 . .
N N2 0.7837(3) 0.3235(3) 0.46631(12) 0.0389(6) Uani d 1 . .
H H2A 0.772557 0.318253 0.427954 0.047 Uiso calc 1 . .
H H2B 0.837980 0.260292 0.477681 0.047 Uiso calc 1 . .
C C2 0.0265(4) 0.7382(4) 0.54340(14) 0.0453(8) Uani d 1 . .
H H2 -0.024706 0.785813 0.569582 0.054 Uiso calc 1 . .
O O3 -0.2495(3) 0.9798(3) 0.19378(11) 0.0495(6) Uani d 1 . .
H H3' -0.249(3) 0.987(5) 0.156(3) 0.074 Uiso calc 1 . .
C C3 0.0180(4) 0.7616(4) 0.48443(14) 0.0455(8) Uani d 1 . .
H H3 -0.041818 0.824262 0.471595 0.055 Uiso calc 1 . .
O O4 0.1637(3) 0.7502(3) 0.15416(11) 0.0599(8) Uani d 1 . .
C C4 0.0949(3) 0.6957(3) 0.44306(13) 0.0356(7) Uani d 1 . .
O O5 0.5729(3) 0.4173(3) 0.41022(10) 0.0533(7) Uani d 1 . .
C C5 0.1812(3) 0.6002(3) 0.46420(13) 0.0309(6) Uani d 1 . .
O O6 0.4198(2) 0.3686(3) 0.47823(11) 0.0466(6) Uani d 1 . .
C C6 0.1903(3) 0.5733(3) 0.52325(13) 0.0329(6) Uani d 1 . .
H H6 0.247994 0.509154 0.536261 0.039 Uiso calc 1 . .
O O7 -0.0892(3) 0.7406(2) 0.78591(10) 0.0460(6) Uani d 1 . .
C C7 0.0875(4) 0.7241(3) 0.38077(13) 0.0386(7) Uani d 1 . .
H H7 0.156958 0.691646 0.357645 0.046 Uiso calc 1 . .
O O8 -0.0296(3) 0.7428(2) 0.69242(10) 0.0506(7) Uani d 1 . .
C C8 -0.0076(3) 0.7910(4) 0.35402(14) 0.0398(7) Uani d 1 . .
H H8 -0.075927 0.825377 0.377158 0.048 Uiso calc 1 . .
C C9 -0.0159(3) 0.8164(3) 0.29118(14) 0.0360(7) Uani d 1 . .
C C10 -0.1234(3) 0.8909(3) 0.27047(14) 0.0371(7) Uani d 1 . .
H H10 -0.185411 0.926232 0.296429 0.044 Uiso calc 1 . .
C C11 -0.1378(3) 0.9121(3) 0.21109(14) 0.0366(7) Uani d 1 . .
C C12 -0.0429(4) 0.8644(3) 0.17235(13) 0.0411(8) Uani d 1 . .
H H12 -0.051837 0.880042 0.132705 0.049 Uiso calc 1 . .
C C13 0.0660(4) 0.7930(3) 0.19307(14) 0.0419(7) Uani d 1 . .
C C14 0.0793(4) 0.7665(3) 0.25177(14) 0.0399(7) Uani d 1 . .
H H14 0.150671 0.716115 0.265004 0.048 Uiso calc 1 . .
C C15 0.5388(3) 0.3722(3) 0.45688(13) 0.0329(6) Uani d 1 . .
C C16 0.6496(3) 0.3150(3) 0.49651(14) 0.0378(7) Uani d 1 . .
H H16 0.628213 0.226093 0.505799 0.045 Uiso calc 1 . .
C C17 0.6714(5) 0.3919(6) 0.55258(16) 0.0633(12) Uani d 1 . .
H H17A 0.588047 0.434238 0.564351 0.076 Uiso calc 1 . .
H H17B 0.701960 0.337248 0.583990 0.076 Uiso calc 1 . .
C C18 0.7786(8) 0.4871(8) 0.5367(3) 0.108(3) Uani d 1 . .
H H18A 0.737801 0.570706 0.532318 0.130 Uiso calc 1 . .
H H18B 0.845990 0.491800 0.567471 0.130 Uiso calc 1 . .
C C19 0.8440(5) 0.4497(5) 0.4825(2) 0.0664(12) Uani d 1 . .
H H19A 0.941535 0.442251 0.487748 0.080 Uiso calc 1 . .
H H19B 0.826332 0.512272 0.452326 0.080 Uiso calc 1 . .
C C20 -0.0456(3) 0.5426(3) 0.73720(12) 0.0326(6) Uani d 1 . .
H H20 0.044694 0.517884 0.723075 0.039 Uiso calc 1 . .
C C21 -0.1553(5) 0.4849(4) 0.69788(18) 0.0583(10) Uani d 1 . .
H H21A -0.208778 0.551754 0.679827 0.070 Uiso calc 1 . .
H H21B -0.113911 0.433781 0.667490 0.070 Uiso calc 1 . .
C C22 -0.2429(6) 0.4041(6) 0.7356(2) 0.0830(17) Uani d 1 . .
H H22A -0.338064 0.418173 0.726516 0.100 Uiso calc 1 . .
H H22B -0.222303 0.314678 0.729493 0.100 Uiso calc 1 . .
C C23 -0.2149(4) 0.4400(4) 0.7970(2) 0.0583(10) Uani d 1 . .
H H23A -0.225509 0.367342 0.822688 0.070 Uiso calc 1 . .
H H23B -0.275284 0.507642 0.809722 0.070 Uiso calc 1 . .
C C24 -0.0559(3) 0.6875(3) 0.74016(13) 0.0350(7) Uani d 1 . .
H H2' 0.311(4) 0.484(4) 0.4408(18) 0.052 Uiso d 1 . .
H H4' 0.234(3) 0.736(5) 0.1775(16) 0.052 Uiso 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
O1 0.0627(15) 0.0674(16) 0.0241(11) 0.0127(14) 0.0039(11) 0.0043(11)
N1 0.0470(15) 0.0298(11) 0.0291(12) 0.0001(11) 0.0021(11) -0.0007(10)
C1 0.0366(15) 0.0449(17) 0.0242(14) -0.0039(13) 0.0001(12) -0.0004(12)
O2 0.0439(13) 0.0569(15) 0.0272(11) 0.0194(11) -0.0044(10) -0.0057(10)
N2 0.0297(13) 0.0499(15) 0.0372(14) 0.0040(12) 0.0003(11) 0.0029(12)
C2 0.0494(18) 0.0534(19) 0.0330(16) 0.0142(16) 0.0088(14) -0.0023(15)
O3 0.0459(13) 0.0668(16) 0.0357(12) 0.0036(12) -0.0028(10) 0.0172(12)
C3 0.0517(19) 0.0494(18) 0.0355(17) 0.0193(17) 0.0019(14) 0.0031(15)
O4 0.0617(17) 0.082(2) 0.0356(13) 0.0123(16) 0.0113(12) 0.0022(14)
C4 0.0369(15) 0.0426(16) 0.0274(14) 0.0044(13) -0.0007(12) 0.0021(12)
O5 0.0467(13) 0.0819(19) 0.0311(11) 0.0097(13) 0.0015(10) 0.0159(12)
C5 0.0261(13) 0.0385(15) 0.0281(14) -0.0001(12) 0.0009(11) -0.0053(12)
O6 0.0301(11) 0.0578(14) 0.0517(14) 0.0071(11) 0.0051(10) 0.0140(11)
C6 0.0318(14) 0.0375(15) 0.0294(15) 0.0028(12) -0.0035(12) 0.0009(12)
O7 0.0643(16) 0.0357(11) 0.0382(12) -0.0033(11) 0.0102(11) -0.0075(10)
C7 0.0435(16) 0.0425(16) 0.0297(14) 0.0083(14) 0.0031(13) 0.0020(13)
O8 0.0834(19) 0.0336(11) 0.0347(12) -0.0046(12) 0.0123(12) 0.0041(10)
C8 0.0374(16) 0.0523(18) 0.0295(15) 0.0059(14) 0.0017(12) 0.0023(14)
C9 0.0381(16) 0.0403(15) 0.0297(15) -0.0020(13) 0.0008(13) 0.0034(13)
C10 0.0366(16) 0.0436(16) 0.0310(15) 0.0000(14) 0.0020(12) 0.0030(13)
C11 0.0376(16) 0.0406(16) 0.0315(15) -0.0057(13) -0.0039(13) 0.0090(13)
C12 0.0518(19) 0.0478(17) 0.0236(14) -0.0086(16) -0.0010(13) 0.0062(13)
C13 0.0485(19) 0.0450(17) 0.0324(16) -0.0022(15) 0.0075(14) -0.0001(13)
C14 0.0417(16) 0.0448(17) 0.0333(15) 0.0014(14) 0.0018(13) 0.0040(13)
C15 0.0305(15) 0.0389(15) 0.0294(15) 0.0020(13) -0.0008(12) 0.0029(12)
C16 0.0323(15) 0.0458(17) 0.0354(17) 0.0018(13) 0.0001(13) 0.0105(14)
C17 0.058(2) 0.103(3) 0.0294(17) 0.004(2) -0.0044(16) -0.002(2)
C18 0.111(5) 0.121(5) 0.093(4) -0.052(4) 0.023(4) -0.062(4)
C19 0.054(2) 0.063(3) 0.083(3) -0.018(2) 0.005(2) -0.003(2)
C20 0.0404(15) 0.0294(13) 0.0280(14) -0.0022(12) 0.0035(12) -0.0017(11)
C21 0.078(3) 0.053(2) 0.043(2) -0.014(2) -0.0174(19) -0.0079(17)
C22 0.073(3) 0.089(3) 0.088(4) -0.044(3) -0.027(3) 0.008(3)
C23 0.049(2) 0.057(2) 0.069(3) -0.0053(18) 0.0188(19) 0.012(2)
C24 0.0420(16) 0.0321(14) 0.0309(14) -0.0060(13) 0.0039(13) -0.0023(12)
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'
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
C1 O1 H1' . . 109.5 ?
C23 N1 C20 . . 107.4(3) ?
C23 N1 H1A . . 110.2 ?
C20 N1 H1A . . 110.2 ?
C23 N1 H1B . . 110.2 ?
C20 N1 H1B . . 110.2 ?
H1A N1 H1B . . 108.5 ?
O1 C1 C2 . . 122.9(3) ?
O1 C1 C6 . . 117.4(3) ?
C2 C1 C6 . . 119.8(3) ?
C5 O2 H2' . . 112(3) ?
C16 N2 C19 . . 106.6(3) ?
C16 N2 H2A . . 110.4 ?
C19 N2 H2A . . 110.4 ?
C16 N2 H2B . . 110.4 ?
C19 N2 H2B . . 110.4 ?
H2A N2 H2B . . 108.6 ?
C3 C2 C1 . . 119.0(3) ?
C3 C2 H2 . . 120.5 ?
C1 C2 H2 . . 120.5 ?
C11 O3 H3' . . 109.5 ?
C2 C3 C4 . . 123.2(3) ?
C2 C3 H3 . . 118.4 ?
C4 C3 H3 . . 118.4 ?
C13 O4 H4' . . 102(3) ?
C3 C4 C5 . . 116.5(3) ?
C3 C4 C7 . . 122.5(3) ?
C5 C4 C7 . . 121.0(3) ?
O2 C5 C6 . . 120.2(3) ?
O2 C5 C4 . . 118.3(3) ?
C6 C5 C4 . . 121.5(3) ?
C5 C6 C1 . . 120.0(3) ?
C5 C6 H6 . . 120.0 ?
C1 C6 H6 . . 120.0 ?
C8 C7 C4 . . 126.8(3) ?
C8 C7 H7 . . 116.6 ?
C4 C7 H7 . . 116.6 ?
C7 C8 C9 . . 126.4(3) ?
C7 C8 H8 . . 116.8 ?
C9 C8 H8 . . 116.8 ?
C10 C9 C14 . . 119.5(3) ?
C10 C9 C8 . . 118.5(3) ?
C14 C9 C8 . . 122.0(3) ?
C11 C10 C9 . . 120.0(3) ?
C11 C10 H10 . . 120.0 ?
C9 C10 H10 . . 120.0 ?
O3 C11 C12 . . 122.8(3) ?
O3 C11 C10 . . 116.8(3) ?
C12 C11 C10 . . 120.4(3) ?
C11 C12 C13 . . 119.6(3) ?
C11 C12 H12 . . 120.2 ?
C13 C12 H12 . . 120.2 ?
C14 C13 O4 . . 119.9(3) ?
C14 C13 C12 . . 121.0(3) ?
O4 C13 C12 . . 119.1(3) ?
C13 C14 C9 . . 119.5(3) ?
C13 C14 H14 . . 120.3 ?
C9 C14 H14 . . 120.3 ?
O5 C15 O6 . . 127.2(3) ?
O5 C15 C16 . . 118.5(3) ?
O6 C15 C16 . . 114.3(3) ?
N2 C16 C17 . . 103.7(3) ?
N2 C16 C15 . . 109.0(3) ?
C17 C16 C15 . . 113.0(3) ?
N2 C16 H16 . . 110.3 ?
C17 C16 H16 . . 110.3 ?
C15 C16 H16 . . 110.3 ?
C18 C17 C16 . . 104.1(3) ?
C18 C17 H17A . . 110.9 ?
C16 C17 H17A . . 110.9 ?
C18 C17 H17B . . 110.9 ?
C16 C17 H17B . . 110.9 ?
H17A C17 H17B . . 109.0 ?
C19 C18 C17 . . 109.8(4) ?
C19 C18 H18A . . 109.7 ?
C17 C18 H18A . . 109.7 ?
C19 C18 H18B . . 109.7 ?
C17 C18 H18B . . 109.7 ?
H18A C18 H18B . . 108.2 ?
C18 C19 N2 . . 106.0(4) ?
C18 C19 H19A . . 110.5 ?
N2 C19 H19A . . 110.5 ?
C18 C19 H19B . . 110.5 ?
N2 C19 H19B . . 110.5 ?
H19A C19 H19B . . 108.7 ?
N1 C20 C24 . . 110.8(2) ?
N1 C20 C21 . . 104.7(3) ?
C24 C20 C21 . . 111.9(3) ?
N1 C20 H20 . . 109.7 ?
C24 C20 H20 . . 109.7 ?
C21 C20 H20 . . 109.7 ?
C22 C21 C20 . . 106.8(3) ?
C22 C21 H21A . . 110.4 ?
C20 C21 H21A . . 110.4 ?
C22 C21 H21B . . 110.4 ?
C20 C21 H21B . . 110.4 ?
H21A C21 H21B . . 108.6 ?
C23 C22 C21 . . 107.6(3) ?
C23 C22 H22A . . 110.2 ?
C21 C22 H22A . . 110.2 ?
C23 C22 H22B . . 110.2 ?
C21 C22 H22B . . 110.2 ?
H22A C22 H22B . . 108.5 ?
C22 C23 N1 . . 103.7(3) ?
C22 C23 H23A . . 111.0 ?
N1 C23 H23A . . 111.0 ?
C22 C23 H23B . . 111.0 ?
N1 C23 H23B . . 111.0 ?
H23A C23 H23B . . 109.0 ?
O7 C24 O8 . . 125.8(3) ?
O7 C24 C20 . . 120.3(3) ?
O8 C24 C20 . . 113.8(3) ?
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
O1 C1 . 1.349(4) ?
O1 H1' . 0.96(6) ?
N1 C23 . 1.495(5) n
N1 C20 . 1.497(4) n
N1 H1A . 0.8900 ?
N1 H1B . 0.8900 ?
C1 C2 . 1.387(5) ?
C1 C6 . 1.397(5) ?
O2 C5 . 1.369(4) ?
O2 H2' . 0.82(2) ?
N2 C16 . 1.492(4) n
N2 C19 . 1.498(5) n
N2 H2A . 0.8900 ?
N2 H2B . 0.8900 ?
C2 C3 . 1.380(5) ?
C2 H2 . 0.9300 ?
O3 C11 . 1.367(4) ?
O3 H3' . 0.87(6) ?
C3 C4 . 1.398(5) ?
C3 H3 . 0.9300 ?
O4 C13 . 1.387(4) ?
O4 H4' . 0.89(2) ?
C4 C5 . 1.400(4) ?
C4 C7 . 1.464(4) ?
O5 C15 . 1.219(4) n
C5 C6 . 1.389(4) ?
O6 C15 . 1.269(4) n
C6 H6 . 0.9300 ?
O7 C24 . 1.234(4) n
C7 C8 . 1.320(5) ?
C7 H7 . 0.9300 ?
O8 C24 . 1.268(4) n
C8 C9 . 1.471(4) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.398(5) ?
C9 C14 . 1.403(5) ?
C10 C11 . 1.390(4) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.383(5) ?
C12 C13 . 1.391(5) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.384(4) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.541(4) ?
C16 C17 . 1.535(5) ?
C16 H16 . 0.9800 ?
C17 C18 . 1.497(8) ?
C17 H17A . 0.9700 ?
C17 H17B . 0.9700 ?
C18 C19 . 1.456(8) ?
C18 H18A . 0.9700 ?
C18 H18B . 0.9700 ?
C19 H19A . 0.9700 ?
C19 H19B . 0.9700 ?
C20 C24 . 1.526(4) ?
C20 C21 . 1.531(5) ?
C20 H20 . 0.9800 ?
C21 C22 . 1.488(7) ?
C21 H21A . 0.9700 ?
C21 H21B . 0.9700 ?
C22 C23 . 1.485(7) ?
C22 H22A . 0.9700 ?
C22 H22B . 0.9700 ?
C23 H23A . 0.9700 ?
C23 H23B . 0.9700 ?
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
_geom_hbond_publ_flag
O1 H1' O8 . 0.96 1.70 2.642(4) 169 yes
O2 H2' O6 . 0.82(2) 1.83(3) 2.647(3) 175(5) yes
O3 H3' O2 3 0.87 1.92 2.784(3) 171 yes
O4 H4' O7 2_566 0.89(2) 1.95(3) 2.794(4) 159(4) yes
N1 H1B O5 4_565 0.89 2.04 2.827(3) 146 yes
N1 H1A O8 3_546 0.89 1.90 2.733(4) 154 yes
N2 H2A O4 3_645 0.89 2.11 2.920(4) 150 yes
N2 H2B O6 2_556 0.89 1.87 2.734(4) 163 yes
C6 H6 O6 . 0.93 2.61 3.282(4) 130 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1 C1 C2 C3 . . . . -179.3(4) ?
C6 C1 C2 C3 . . . . 0.9(5) ?
C1 C2 C3 C4 . . . . -1.7(6) ?
C2 C3 C4 C5 . . . . 1.4(6) ?
C2 C3 C4 C7 . . . . -178.2(4) ?
C3 C4 C5 O2 . . . . 178.9(3) ?
C7 C4 C5 O2 . . . . -1.5(5) ?
C3 C4 C5 C6 . . . . -0.4(5) ?
C7 C4 C5 C6 . . . . 179.3(3) ?
O2 C5 C6 C1 . . . . -179.6(3) ?
C4 C5 C6 C1 . . . . -0.3(5) ?
O1 C1 C6 C5 . . . . -179.7(3) ?
C2 C1 C6 C5 . . . . 0.1(5) ?
C3 C4 C7 C8 . . . . -15.6(6) ?
C5 C4 C7 C8 . . . . 164.8(3) ?
C4 C7 C8 C9 . . . . -178.4(3) ?
C7 C8 C9 C10 . . . . -179.2(4) ?
C7 C8 C9 C14 . . . . 1.8(6) ?
C14 C9 C10 C11 . . . . 1.8(5) ?
C8 C9 C10 C11 . . . . -177.2(3) ?
C9 C10 C11 O3 . . . . 176.4(3) ?
C9 C10 C11 C12 . . . . -2.8(5) ?
O3 C11 C12 C13 . . . . -178.0(3) ?
C10 C11 C12 C13 . . . . 1.1(5) ?
C11 C12 C13 C14 . . . . 1.4(5) ?
C11 C12 C13 O4 . . . . -177.3(3) ?
O4 C13 C14 C9 . . . . 176.4(3) ?
C12 C13 C14 C9 . . . . -2.3(5) ?
C10 C9 C14 C13 . . . . 0.7(5) ?
C8 C9 C14 C13 . . . . 179.7(3) ?
C19 N2 C16 C17 . . . . -31.3(4) ?
C19 N2 C16 C15 . . . . 89.3(3) ?
O5 C15 C16 N2 . . . . -2.2(4) ?
O6 C15 C16 N2 . . . . 179.3(3) ?
O5 C15 C16 C17 . . . . 112.5(4) ?
O6 C15 C16 C17 . . . . -66.0(4) ?
N2 C16 C17 C18 . . . . 27.9(5) ?
C15 C16 C17 C18 . . . . -89.9(5) ?
C16 C17 C18 C19 . . . . -14.9(8) ?
C17 C18 C19 N2 . . . . -4.2(8) ?
C16 N2 C19 C18 . . . . 22.5(6) ?
C23 N1 C20 C24 . . . . 99.1(3) ?
C23 N1 C20 C21 . . . . -21.8(4) ?
N1 C20 C21 C22 . . . . 3.7(5) ?
C24 C20 C21 C22 . . . . -116.5(4) ?
C20 C21 C22 C23 . . . . 15.9(6) ?
C21 C22 C23 N1 . . . . -29.0(5) ?
C20 N1 C23 C22 . . . . 31.5(4) ?
N1 C20 C24 O7 . . . . -4.1(4) ?
C21 C20 C24 O7 . . . . 112.4(4) ?
N1 C20 C24 O8 . . . . 176.9(3) ?
C21 C20 C24 O8 . . . . -66.5(4) ?
_cod_database_fobs_code 2243568