#------------------------------------------------------------------------------
#$Date: 2020-08-29 08:09:17 +0300 (Sat, 29 Aug 2020) $
#$Revision: 255745 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/35/2243567.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_2243567
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, H2 O'
_chemical_formula_moiety 'C14 H12 O4, 2(C5 H9 N O2), H2 O'
_chemical_formula_sum 'C24 H32 N2 O9'
_chemical_formula_weight 492.51
_chemical_name_systematic
;
4-[(E)-2-(3,5-Dihydroxyphenyl)ethenyl]benzene-1,3-diol
bis[(S)-pyrrolidin-1-ium-2-carboxylate] monohydrate
;
_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 9.9759(2)
_cell_length_b 10.6052(2)
_cell_length_c 22.8535(4)
_cell_measurement_reflns_used 9870
_cell_measurement_temperature 297(2)
_cell_measurement_theta_max 27.21
_cell_measurement_theta_min 3.29
_cell_volume 2417.82(8)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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 0.0243
_diffrn_reflns_av_unetI/netI 0.0154
_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 27568
_diffrn_reflns_theta_full 25.000
_diffrn_reflns_theta_max 25.000
_diffrn_reflns_theta_min 2.942
_diffrn_source 'Sealed x-ray tube'
_exptl_absorpt_coefficient_mu 0.104
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.7157
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.353
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Rod
_exptl_crystal_F_000 1048
_exptl_crystal_size_max 0.330
_exptl_crystal_size_mid 0.225
_exptl_crystal_size_min 0.114
_refine_diff_density_max 0.349
_refine_diff_density_min -0.312
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.049
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 332
_refine_ls_number_reflns 4237
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.064
_refine_ls_R_factor_all 0.0459
_refine_ls_R_factor_gt 0.0439
_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^)+(0.0603P)^2^+1.0192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1149
_refine_ls_wR_factor_ref 0.1167
_reflns_number_gt 4046
_reflns_number_total 4237
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb7935sup1.cif
_cod_data_source_block I
_cod_database_code 2243567
_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 0.967
_shelx_estimated_absorpt_t_max 0.988
_shelx_hkl_file
;
2 0 0 3094.79 70.89
-2 0 0 3081.49 70.89
3 0 0 4.10 1.50
-3 0 0 1.30 1.40
-4 0 0 965.90 24.20
4 0 0 957.00 24.30
5 0 0 -0.20 1.80
-5 0 0 1.20 1.90
-6 0 0 388.56 12.70
6 0 0 419.56 13.00
7 0 0 1.10 2.40
-7 0 0 -0.70 1.80
-8 0 0 24.70 3.90
8 0 0 16.80 3.80
9 0 0 0.20 2.80
-10 0 0 35.70 5.00
10 0 0 26.10 4.70
11 0 0 -1.40 3.30
-2 -1 0 979.70 22.70
2 1 0 985.80 22.50
-2 -1 0 951.80 23.50
2 -1 0 975.50 23.40
-2 1 0 985.90 23.40
-2 -1 0 983.10 22.70
2 1 0 1006.20 23.60
-3 1 0 52.49 3.50
-3 -1 0 51.59 2.00
3 1 0 50.59 3.60
-3 -1 0 53.89 2.10
3 -1 0 59.79 3.50
-3 -1 0 57.29 3.50
4 1 0 59.49 4.20
-4 -1 0 59.89 4.10
4 -1 0 61.59 3.90
-4 1 0 63.59 4.10
5 1 0 667.93 18.50
-5 1 0 698.93 18.40
-5 -1 0 661.03 18.40
5 -1 0 665.73 18.30
6 1 0 3.10 2.20
6 -1 0 3.00 2.20
-6 -1 0 3.90 2.30
-6 1 0 3.00 2.20
-7 1 0 157.38 7.70
-7 -1 0 158.98 7.80
7 1 0 159.68 7.90
7 -1 0 168.28 7.90
8 1 0 690.93 21.00
-8 1 0 709.03 20.90
-8 -1 0 730.53 21.20
8 -1 0 662.03 20.60
9 -1 0 40.70 5.10
-9 -1 0 27.90 5.00
9 1 0 51.69 5.90
-9 1 0 32.60 4.80
-10 1 0 19.70 4.40
10 1 0 17.80 4.40
11 1 0 32.30 5.70
12 1 0 9.60 4.40
0 2 0 1213.68 29.40
0 -2 0 1273.77 29.40
0 2 0 1282.37 29.40
0 -2 0 1263.47 29.40
1 -2 0 4391.16 98.59
1 2 0 4281.57 98.69
-1 2 0 4337.57 98.69
-1 -2 0 4371.66 98.79
1 2 0 4221.58 98.69
-1 -2 0 4254.37 98.69
1 -2 0 4387.56 98.59
-1 2 0 4412.16 98.69
-3 2 0 44.70 2.10
-3 2 0 44.10 2.10
3 2 0 43.50 3.30
-3 -2 0 45.50 2.60
3 2 0 44.60 2.20
-3 2 0 43.70 3.20
3 2 0 44.90 2.20
-3 -2 0 42.40 2.50
-4 -2 0 117.99 5.40
-4 -2 0 109.59 4.00
4 2 0 114.99 5.40
-4 2 0 114.89 5.20
-4 2 0 111.89 3.40
-4 -2 0 111.59 4.00
-5 -2 0 997.10 27.20
-5 -2 0 1061.59 25.00
-5 2 0 1054.99 26.80
5 2 0 1056.69 27.20
-5 -2 0 1068.79 24.90
-6 2 0 897.91 24.20
6 2 0 912.51 24.60
-6 -2 0 915.21 21.90
-6 -2 0 912.41 21.90
-6 -2 0 907.61 24.60
-7 -2 0 121.59 6.90
7 2 0 122.39 7.10
-7 2 0 120.09 6.90
-7 -2 0 121.69 4.40
-7 -2 0 114.39 4.40
-8 -2 0 90.89 3.90
8 2 0 85.29 6.70
-8 -2 0 92.59 3.90
-8 2 0 93.89 6.80
9 2 0 32.40 4.80
-9 -2 0 28.70 2.90
-9 2 0 28.30 4.70
-9 -2 0 28.30 2.50
10 2 0 140.19 9.20
-10 2 0 142.09 9.40
-10 -2 0 141.89 5.30
11 2 0 56.19 6.50
-11 -2 0 50.49 3.60
12 2 0 6.90 3.70
0 -3 0 1.10 1.40
0 3 0 1.70 1.50
0 3 0 2.40 1.50
0 -3 0 -0.70 1.30
-1 3 0 3276.97 76.39
-1 3 0 3318.57 76.29
-1 -3 0 3284.87 76.39
1 -3 0 3318.17 76.29
1 3 0 3406.66 76.49
-1 -3 0 3325.57 76.49
1 3 0 3247.48 76.39
1 -3 0 3387.46 76.29
2 3 0 2150.08 48.90
-2 -3 0 2118.29 49.10
2 3 0 2102.39 49.00
-2 3 0 2114.79 48.90
2 -3 0 2103.89 48.70
-2 3 0 2078.49 48.80
2 -3 0 2072.79 48.60
-2 -3 0 2082.89 49.00
3 3 0 9948.30 222.48
3 -3 0 9857.31 221.98
-3 3 0 9858.21 223.08
-3 3 0 9912.31 222.48
3 -3 0 9311.37 221.88
-3 -3 0 9665.73 222.78
3 3 0 9867.81 222.48
-3 -3 0 9999.00 222.78
-3 3 0 9781.72 222.38
4 3 0 1043.30 26.60
-4 3 0 1039.30 24.80
-4 -3 0 1032.80 25.20
-4 3 0 1017.80 26.00
-4 3 0 1054.79 24.80
4 3 0 1048.60 24.70
-4 -3 0 1042.40 25.20
4 3 0 1044.80 24.70
-5 -3 0 282.47 8.30
-5 3 0 290.57 7.80
-5 -3 0 286.77 8.40
5 3 0 270.37 11.10
-5 3 0 288.67 9.60
-5 3 0 292.77 7.80
-6 -3 0 166.48 5.80
6 3 0 164.58 7.80
-6 3 0 159.18 5.10
-6 -3 0 167.78 5.80
-6 3 0 167.88 5.10
-6 3 0 158.48 7.20
-7 -3 0 4.80 1.80
-7 3 0 2.80 2.30
-7 -3 0 3.10 1.80
-7 3 0 6.30 1.50
7 3 0 5.70 2.90
-8 3 0 21.30 3.80
8 3 0 28.10 4.20
-8 -3 0 25.50 2.70
-8 -3 0 22.50 2.60
-9 -3 0 248.98 8.20
-9 3 0 264.77 11.70
9 3 0 248.08 11.60
-9 -3 0 256.67 8.30
-10 -3 0 0.00 2.00
-10 3 0 1.40 3.00
-10 -3 0 -0.70 1.90
10 3 0 -0.20 5.90
-11 -3 0 1.70 2.00
11 3 0 2.40 3.70
-11 -3 0 2.40 1.90
-12 -3 0 23.60 3.10
12 3 0 23.10 6.20
-12 -3 0 23.00 2.90
0 4 0 3125.19 72.79
0 -4 0 3149.28 72.79
0 4 0 3090.09 72.79
0 -4 0 3190.38 72.79
-1 4 0 69.79 3.80
1 4 0 67.69 3.80
1 -4 0 61.49 3.60
1 4 0 59.19 3.60
-1 4 0 65.39 3.80
-1 -4 0 59.49 3.70
1 -4 0 65.59 3.70
2 -4 0 1984.70 45.20
-2 4 0 1905.11 45.30
-2 -4 0 1959.60 45.60
2 -4 0 1886.31 45.10
-2 4 0 1898.21 45.40
2 4 0 1925.81 45.40
2 4 0 1940.91 45.50
-2 -4 0 1889.31 45.50
3 4 0 592.24 15.20
-3 4 0 579.04 15.10
3 4 0 595.04 16.10
-3 4 0 581.64 15.20
3 -4 0 586.34 14.70
3 -4 0 596.84 14.80
-3 -4 0 565.24 15.40
-3 -4 0 583.54 15.40
3 4 0 601.44 15.30
4 4 0 6794.42 154.18
-4 -4 0 6841.52 154.68
4 4 0 6773.02 154.08
-4 -4 0 6650.43 154.58
4 4 0 6696.63 155.68
-4 4 0 6788.42 155.08
-4 4 0 6704.33 154.18
4 -4 0 6789.32 153.28
-4 4 0 6799.12 154.28
4 -4 0 6694.33 153.28
5 4 0 612.04 15.50
5 4 0 631.64 15.50
-5 4 0 625.84 17.20
-5 -4 0 618.74 16.40
-5 4 0 619.74 15.90
-5 4 0 621.84 15.90
5 4 0 593.04 17.80
-5 -4 0 635.14 16.50
-6 -4 0 101.99 4.80
6 4 0 98.99 6.20
-6 -4 0 102.59 4.90
-6 4 0 102.39 5.90
-6 4 0 99.39 4.30
-6 4 0 98.69 4.30
-7 -4 0 158.78 6.30
7 4 0 156.48 8.20
-7 4 0 160.38 5.60
-7 4 0 153.18 7.60
-7 4 0 159.68 5.50
-8 4 0 124.99 7.60
8 4 0 130.89 8.30
-8 4 0 117.19 4.90
-8 -4 0 126.79 5.70
-8 -4 0 127.39 5.90
-8 4 0 127.89 5.10
-9 4 0 14.90 2.20
9 4 0 16.90 4.30
-9 4 0 17.10 2.20
-9 -4 0 14.30 2.60
-9 4 0 20.70 4.60
-9 -4 0 14.70 2.80
10 4 0 1.20 3.30
-10 -4 0 1.60 2.10
-10 -4 0 1.00 3.50
-10 4 0 0.20 3.40
11 4 0 1.70 3.30
-11 -4 0 1.90 2.20
-11 -4 0 -2.10 2.20
12 4 0 15.90 5.20
-12 -4 0 19.40 3.20
-12 -4 0 25.80 3.50
0 5 0 -0.80 1.70
0 5 0 -0.90 1.70
0 -5 0 0.90 1.70
0 -5 0 2.40 1.80
-1 5 0 1388.86 33.40
1 -5 0 1387.56 33.20
-1 5 0 1324.07 33.20
1 5 0 1332.17 33.30
1 5 0 1366.96 33.40
-1 -5 0 1346.77 33.40
1 -5 0 1390.56 33.30
-1 -5 0 1400.36 33.50
-2 5 0 77.29 4.40
2 5 0 79.49 4.30
-2 -5 0 71.89 4.40
2 5 0 77.29 4.40
2 -5 0 72.49 4.00
2 -5 0 75.79 4.10
-2 -5 0 77.59 4.50
-2 5 0 72.09 4.20
-3 5 0 26.40 3.00
-3 -5 0 13.60 4.20
3 5 0 22.80 2.80
-3 5 0 23.60 2.80
3 -5 0 23.10 2.50
3 5 0 19.40 2.70
-3 -5 0 25.90 3.10
3 -5 0 32.60 2.90
4 -5 0 3.90 1.60
-4 -5 0 -1.30 2.00
4 5 0 1.80 1.90
-4 5 0 6.60 2.10
-4 -5 0 1.60 2.00
4 5 0 -0.10 1.70
-4 5 0 4.30 2.00
4 -5 0 1.80 1.50
-4 5 0 2.70 2.00
-5 5 0 676.23 17.10
5 5 0 636.64 18.70
5 5 0 630.54 16.60
-5 5 0 635.54 16.90
-5 -5 0 653.43 17.50
-5 5 0 641.94 17.90
5 5 0 640.14 16.60
-5 -5 0 619.34 17.40
-6 -5 0 48.40 4.10
-6 5 0 49.10 4.70
6 5 0 42.90 3.00
6 5 0 42.00 4.50
-6 -5 0 48.00 4.20
-6 5 0 48.10 3.60
6 5 0 45.80 3.10
-6 5 0 49.99 3.80
-7 5 0 39.10 4.60
-7 5 0 39.00 3.30
-7 -5 0 33.80 3.60
-7 5 0 37.00 3.50
-7 -5 0 35.70 6.20
7 5 0 37.10 5.00
-8 5 0 193.98 9.40
-8 -5 0 205.08 8.10
-8 -5 0 197.18 7.90
-8 5 0 190.68 9.30
-8 5 0 205.98 7.30
8 5 0 191.78 10.10
-9 5 0 14.90 2.50
-9 5 0 17.80 2.60
-9 -5 0 15.40 3.10
9 5 0 18.40 4.60
-9 -5 0 19.20 3.20
-10 5 0 -3.00 2.80
-10 5 0 1.80 1.90
-10 -5 0 0.70 2.20
10 5 0 1.50 3.10
-10 5 0 1.40 1.90
-10 -5 0 4.10 2.50
-11 5 0 0.00 1.80
-11 -5 0 -2.60 2.20
11 5 0 -2.50 3.50
-11 -5 0 0.70 2.60
-11 5 0 2.50 2.10
-12 -5 0 7.60 3.10
12 5 0 15.50 5.30
-12 -5 0 12.40 3.10
0 6 0 1436.56 35.30
0 6 0 1372.66 35.00
0 -6 0 1445.56 35.10
0 -6 0 1435.66 35.10
1 6 0 12.30 2.40
-1 -6 0 11.60 3.00
-1 6 0 9.30 2.40
-1 6 0 15.50 2.70
1 6 0 13.00 2.60
1 -6 0 11.40 4.00
1 -6 0 11.30 2.40
-1 -6 0 9.40 2.50
-2 6 0 1426.46 35.30
-2 -6 0 1472.75 37.20
-2 6 0 1449.95 35.50
2 6 0 1387.76 35.80
2 6 0 1440.66 35.30
2 -6 0 1469.15 35.20
-2 -6 0 1386.96 35.40
2 -6 0 1434.56 35.00
-3 6 0 5.50 2.20
3 -6 0 11.00 2.20
3 6 0 8.60 2.50
-3 6 0 4.10 2.40
-3 -6 0 9.10 2.60
3 -6 0 5.60 2.10
-3 -6 0 5.70 2.40
3 6 0 6.60 2.30
-4 -6 0 6.80 2.50
4 -6 0 6.20 1.90
4 6 0 7.90 2.80
-4 -6 0 9.80 2.60
-4 6 0 6.90 2.30
4 6 0 4.40 3.80
4 6 0 4.90 2.30
-4 6 0 6.40 2.40
4 -6 0 5.10 1.90
-5 6 0 168.68 7.00
-5 -6 0 176.18 7.40
5 6 0 178.58 8.40
5 6 0 181.88 6.90
-5 6 0 177.28 7.20
-5 -6 0 188.18 7.70
5 -6 0 172.18 5.70
5 6 0 178.58 6.80
-5 6 0 192.98 11.30
5 -6 0 169.28 5.70
-6 -6 0 423.86 13.20
6 6 0 426.76 14.60
-6 -6 0 400.06 13.00
-6 6 0 414.06 12.60
6 6 0 414.06 11.90
-6 6 0 412.76 12.50
6 6 0 406.36 11.80
-6 6 0 418.96 13.40
-7 6 0 -2.10 2.20
7 6 0 -4.50 2.60
-7 -6 0 1.70 2.60
-7 -6 0 -0.70 2.20
7 6 0 0.40 1.50
-7 6 0 0.60 2.00
7 6 0 1.00 1.50
-7 6 0 3.50 2.60
-8 6 0 55.49 4.30
8 6 0 65.39 6.90
-8 -6 0 47.30 4.70
-8 -6 0 50.59 5.10
-8 6 0 51.09 4.60
-8 6 0 56.99 5.90
-9 6 0 20.40 4.20
-9 -6 0 27.50 4.00
-9 -6 0 24.50 3.70
-9 6 0 19.70 3.00
10 6 0 7.90 4.10
-10 6 0 13.10 2.80
-10 6 0 9.30 2.60
-10 -6 0 13.80 3.20
-11 -6 0 22.10 3.50
-11 6 0 14.00 2.70
-11 -6 0 14.40 3.30
11 6 0 10.20 4.90
-11 6 0 12.60 3.10
0 -7 0 -2.30 1.90
0 -7 0 -0.60 2.00
0 7 0 6.30 2.40
0 7 0 2.80 2.00
-1 7 0 168.98 7.30
1 -7 0 179.18 7.20
1 7 0 158.78 6.90
1 -7 0 164.98 7.00
-1 7 0 164.28 7.10
-1 -7 0 155.38 7.00
-1 -7 0 166.88 7.20
1 7 0 164.48 7.20
2 -7 0 98.69 5.40
-2 7 0 106.29 5.70
-2 -7 0 106.59 5.80
2 7 0 104.99 5.90
2 7 0 109.59 5.70
2 -7 0 104.19 5.60
-2 -7 0 106.59 5.90
-2 7 0 112.09 5.90
3 -7 0 49.99 4.00
-3 -7 0 41.70 4.20
-3 7 0 50.59 4.40
-3 7 0 45.20 4.50
-3 -7 0 49.30 4.60
3 7 0 42.90 4.40
3 7 0 45.50 4.20
-4 -7 0 38.90 4.10
4 7 0 44.80 4.60
4 -7 0 45.40 3.70
4 7 0 45.70 4.40
-4 -7 0 34.50 4.10
4 -7 0 37.50 3.70
4 7 0 41.40 4.10
-4 7 0 37.10 3.90
-4 7 0 42.20 4.00
5 7 0 6.40 2.50
-5 -7 0 4.70 2.90
-5 7 0 7.60 2.70
5 7 0 6.80 2.70
-5 7 0 3.70 2.70
-5 -7 0 4.70 2.60
5 -7 0 7.40 2.00
5 7 0 1.50 2.60
5 -7 0 7.60 2.00
-5 7 0 6.70 2.60
-6 7 0 43.90 4.40
-6 -7 0 46.30 4.60
6 7 0 44.70 4.20
-6 7 0 47.30 4.70
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5 -2 9 36.30 2.60
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5 -2 9 34.90 2.60
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-5 -2 9 34.50 3.40
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-6 2 9 103.39 6.60
6 -2 9 124.79 7.10
-6 -2 -9 115.39 5.50
6 2 9 106.29 6.70
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6 2 9 112.69 4.20
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-6 -2 9 117.89 5.20
6 2 9 113.19 4.10
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-7 -2 -9 186.28 7.30
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7 -2 9 193.18 8.40
-7 -2 9 195.58 7.10
-7 -2 9 205.88 9.50
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-7 2 -9 183.48 7.20
7 2 9 200.28 9.40
8 -2 9 79.19 6.20
-8 -2 -9 75.39 5.00
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-8 2 9 74.29 4.20
-8 -2 9 68.89 4.60
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-8 -2 9 80.99 4.60
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-8 2 -9 80.69 4.90
-9 -2 -9 20.20 3.10
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9 -2 9 18.40 3.70
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-9 -2 -9 16.30 3.00
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10 -2 9 1.60 3.30
-10 -2 -9 4.20 2.10
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12 -2 9 8.80 4.00
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0 -3 -9 992.00 24.60
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0 -3 -9 958.20 24.40
0 3 9 980.20 24.50
0 -3 9 976.00 24.50
0 -3 9 968.70 24.50
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1 -3 9 958.30 24.70
1 3 -9 997.50 24.80
1 -3 9 997.20 24.80
1 3 -9 1004.60 24.90
-1 -3 -9 995.00 24.90
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1 -3 -9 985.30 24.60
1 3 9 982.10 24.90
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1 3 9 985.60 24.80
1 -3 -9 985.70 24.70
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2 -3 9 612.74 15.80
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2 -3 9 600.04 15.80
-2 -3 -9 547.35 16.00
2 3 -9 608.94 15.80
2 3 9 588.24 15.80
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2 3 9 598.64 16.00
2 -3 -9 578.94 15.50
-2 -3 9 583.54 16.00
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-2 3 -9 585.24 15.90
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2 -3 -9 592.94 15.60
3 -3 9 168.18 6.40
-3 -3 -9 191.28 7.00
3 -3 9 168.38 6.30
3 -3 9 178.28 5.60
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3 3 -9 180.98 6.50
3 3 -9 176.78 6.30
-3 3 -9 172.48 6.70
-3 -3 9 187.28 6.80
-3 3 -9 176.78 6.80
3 -3 -9 177.48 6.10
-3 -3 9 173.78 6.90
3 3 9 194.48 6.80
-3 -3 9 189.88 6.80
3 -3 -9 174.78 6.10
3 3 9 188.28 6.60
-4 3 9 131.59 5.40
4 -3 9 135.89 5.10
4 3 -9 130.69 5.10
4 -3 9 129.59 5.10
-4 -3 -9 138.79 6.00
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4 3 -9 127.29 5.20
-4 -3 -9 132.09 5.70
4 -3 9 131.29 5.10
-4 -3 9 127.79 8.40
4 -3 -9 126.89 4.60
-4 3 -9 126.19 5.70
4 3 9 128.99 5.40
4 3 9 135.59 5.50
4 -3 -9 122.39 4.60
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-4 -3 9 134.59 6.20
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-5 3 9 210.38 7.10
-5 -3 -9 196.38 7.50
5 -3 9 201.08 7.30
5 -3 9 210.28 6.40
5 -3 9 190.48 6.30
5 3 -9 208.88 6.50
-5 -3 -9 204.28 7.70
5 3 -9 198.58 6.40
-5 -3 9 204.08 8.50
-5 3 -9 213.88 7.60
-5 -3 9 210.78 7.50
-5 -3 9 233.18 7.70
5 3 9 190.28 6.90
-5 3 -9 211.48 7.40
5 3 9 203.98 6.90
6 -3 9 32.60 3.40
-6 3 9 34.60 3.10
-6 3 9 32.90 3.00
-6 -3 -9 33.00 3.50
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6 3 9 28.70 2.90
-6 3 -9 27.70 3.00
6 3 9 29.50 2.90
-6 -3 9 24.20 2.80
-6 -3 9 24.80 3.80
-6 -3 9 31.20 3.20
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6 3 9 27.30 3.90
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-7 -3 -9 273.97 9.60
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-7 3 9 269.67 8.60
7 -3 9 281.37 10.10
-7 -3 9 270.97 9.20
7 3 9 266.87 11.40
-7 3 -9 266.97 9.10
-7 -3 9 294.17 11.50
-7 -3 9 281.77 9.30
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8 -3 9 96.99 6.50
-8 -3 -9 101.79 5.70
-8 -3 -9 119.69 6.10
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-8 3 9 107.59 5.00
8 3 9 97.79 7.60
-8 3 -9 103.39 5.40
-8 -3 9 98.99 5.30
-8 -3 9 92.69 8.60
-8 3 -9 106.69 5.60
-8 -3 9 98.79 5.40
-9 3 9 69.39 4.20
9 -3 9 76.79 6.30
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-9 -3 -9 65.19 5.20
-9 -3 -9 67.99 5.00
-9 -3 9 73.79 6.50
-9 -3 9 59.89 4.60
-9 3 -9 59.79 4.60
9 3 9 68.89 7.30
-10 3 9 24.10 2.80
-10 -3 -9 30.50 3.60
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10 -3 9 30.50 4.60
-10 -3 -9 31.20 3.80
-10 -3 9 30.00 3.50
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-10 3 -9 28.10 3.20
10 3 9 26.70 5.50
-10 -3 9 29.10 3.30
-11 -3 -9 17.90 3.40
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-11 -3 -9 9.90 3.10
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-11 3 -9 15.40 3.10
-11 -3 9 14.50 2.90
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-11 -3 9 16.50 3.10
11 3 9 9.30 4.40
-12 -3 -9 40.50 4.60
-12 -3 -9 39.00 4.20
12 3 9 39.70 6.60
-12 -3 9 24.00 3.40
-12 -3 9 40.80 4.10
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0 4 9 5.40 2.00
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0 -4 -9 2.80 2.20
0 4 -9 3.90 2.20
0 -4 -9 3.40 1.90
0 -4 9 3.80 2.00
1 -4 9 3838.22 88.59
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-1 -4 -9 3699.93 88.59
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1 4 -9 3823.02 88.69
1 4 -9 4048.50 90.09
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1 -4 -9 3829.22 88.49
-1 -4 9 3852.61 88.69
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1 4 9 3823.32 88.59
1 4 9 3853.31 88.69
1 -4 -9 3801.62 88.29
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2 -4 9 456.35 12.90
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2 -4 9 447.46 12.90
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2 4 9 466.95 13.10
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2 -4 -9 454.25 12.70
2 -4 -9 442.66 12.60
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2 4 9 446.56 13.00
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3 -4 9 24.70 2.70
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-3 -4 -9 28.70 3.20
3 -4 9 29.50 3.00
3 4 -9 29.20 2.90
3 4 -9 27.00 3.00
-3 -4 9 29.30 3.20
3 -4 -9 31.70 2.90
-3 -4 9 24.00 2.70
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3 4 9 33.70 3.20
-3 4 -9 23.10 3.10
3 4 9 30.80 3.60
-3 -4 9 26.70 3.10
3 -4 -9 27.30 2.70
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4 4 -9 252.27 8.10
-4 -4 -9 238.08 8.60
-4 -4 -9 234.38 8.60
4 -4 9 231.28 7.70
4 4 -9 242.68 7.90
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4 -4 9 237.38 7.20
4 -4 9 239.98 7.80
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-4 -4 9 244.18 8.50
4 4 9 227.38 8.10
4 -4 -9 248.58 7.50
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4 4 9 222.08 8.20
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4 -4 -9 242.78 7.40
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-5 -4 -9 14.70 2.80
5 4 -9 16.10 2.20
5 4 -9 16.20 2.40
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5 -4 9 15.80 2.30
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5 -4 9 16.50 2.10
5 -4 9 16.60 2.10
-5 -4 9 12.40 2.80
5 4 9 11.60 2.30
-5 4 -9 16.80 2.90
-5 4 -9 13.20 2.60
5 -4 -9 15.10 1.60
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5 -4 -9 15.80 1.80
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6 -4 9 20.90 2.90
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-6 -4 -9 21.70 3.10
-6 -4 -9 19.30 3.20
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6 4 9 28.00 2.90
-6 4 -9 28.50 3.30
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-6 -4 9 26.70 3.30
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-7 -4 -9 139.79 6.80
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-7 -4 -9 132.79 6.60
7 -4 9 149.69 6.80
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7 4 9 146.59 8.50
-7 -4 9 146.39 6.80
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8 -4 9 9.00 2.90
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-10 -4 -9 7.10 3.70
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-10 -4 -9 10.10 3.30
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10 4 9 9.10 4.20
-11 -4 -9 27.60 3.80
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-11 -4 -9 22.20 3.80
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11 4 9 17.90 5.20
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0 -5 -9 46.80 4.00
0 -5 9 46.70 4.00
0 -5 -9 54.89 4.30
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1 -5 9 383.66 12.00
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1 5 -9 393.66 12.10
1 5 -9 391.36 12.10
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1 -5 9 406.86 12.10
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1 -5 -9 394.86 13.10
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1 -5 -9 392.86 11.90
1 5 9 389.76 12.10
2 -5 9 238.08 8.60
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2 -5 9 251.17 8.60
2 -5 -9 233.68 8.30
2 -5 -9 226.18 8.30
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2 5 9 241.08 8.70
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3 5 -9 592.74 16.60
3 -5 9 610.84 16.50
3 -5 9 644.94 17.20
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3 -5 -9 585.94 16.20
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3 5 9 576.94 16.70
3 5 9 569.34 16.70
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3 -5 -9 576.44 16.10
4 -5 9 132.09 5.60
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4 5 -9 128.79 6.20
4 -5 9 125.89 5.60
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4 5 9 132.29 6.10
4 -5 -9 128.09 5.20
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4 5 9 122.79 5.90
4 -5 -9 134.59 5.40
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-4 5 -9 125.89 6.10
5 -5 9 26.70 2.80
-5 -5 -9 23.30 3.40
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5 5 -9 18.40 2.80
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-5 -5 -9 21.10 3.40
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5 -5 9 25.30 2.70
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5 -5 -9 23.60 2.30
-5 5 -9 23.60 3.50
5 5 9 26.70 3.30
-5 -5 9 21.50 3.30
5 -5 -9 24.70 2.30
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-5 5 -9 25.70 3.30
-5 -5 9 23.10 3.60
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-6 -5 -9 2.60 2.60
-6 -5 -9 4.60 2.60
6 -5 9 7.00 1.70
6 -5 9 3.90 1.60
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7 5 -9 44.80 5.10
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-7 -5 9 50.29 4.70
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-8 -5 9 11.30 4.00
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0 -6 -9 48.60 4.40
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0 -6 9 44.80 4.40
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0 -6 -9 42.90 4.30
0 6 -9 49.90 4.30
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1 -6 9 780.42 20.60
1 6 -9 725.93 20.40
1 -6 9 745.93 20.40
1 6 -9 731.13 20.60
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1 6 9 756.92 20.60
1 6 9 732.13 20.50
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1 -6 -9 740.03 20.30
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1 -6 -9 743.83 20.40
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2 -6 9 287.87 9.70
2 -6 9 258.17 9.50
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2 -6 -9 284.37 9.50
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2 -6 -9 279.67 9.50
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3 -6 9 428.26 12.70
3 -6 9 410.16 12.60
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3 -6 -9 403.66 12.30
3 -6 -9 401.16 12.40
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4 -6 9 266.77 9.20
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4 -6 9 283.57 9.40
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4 -6 -9 269.77 8.90
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5 -6 9 31.90 3.20
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5 -6 9 36.80 3.30
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5 -6 -9 33.90 3.20
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-5 -6 9 28.50 3.90
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-3 3 -28 10.80 4.90
3 -3 -28 18.40 4.30
0 -4 28 4.20 4.10
0 -4 28 -1.20 2.30
0 -4 -28 4.10 3.90
0 4 28 5.00 4.00
0 4 -28 -1.00 3.70
1 -4 28 12.80 4.40
-1 -4 -28 8.20 4.30
-1 4 28 12.80 4.40
1 4 -28 27.50 5.90
1 4 28 11.60 4.30
-1 4 -28 11.00 4.60
-1 -4 28 13.60 4.70
1 -4 -28 12.30 4.40
-1 -4 28 10.60 3.10
2 -4 28 9.20 4.00
-2 4 28 4.70 4.10
-2 -4 -28 6.30 3.90
2 4 -28 0.40 3.50
2 4 28 6.80 4.10
-2 4 -28 -5.20 3.90
2 -4 -28 3.80 3.70
-2 -4 28 -0.30 3.00
-2 -4 28 -3.70 3.80
0 0 29 1.30 3.70
0 0 -29 -1.40 3.60
-1 0 29 9.00 4.20
1 0 -29 4.20 3.90
1 0 29 -1.50 3.80
-1 0 -29 5.60 4.20
-2 0 29 2.10 3.90
-2 0 -29 2.40 3.80
2 0 -29 1.10 3.50
2 0 29 -3.40 3.40
0 -1 -29 65.79 7.10
0 -1 29 89.79 8.00
0 1 29 83.19 7.80
0 1 -29 68.59 7.30
1 -1 29 3.90 4.10
1 1 -29 4.60 3.80
-1 -1 -29 1.70 4.00
-1 1 29 5.40 4.10
1 -1 -29 -0.50 3.60
-1 -1 29 6.20 4.20
1 1 29 5.70 3.80
-1 1 -29 8.60 4.50
-2 -1 -29 4.10 3.90
-2 1 29 5.40 4.00
2 -1 29 3.50 3.90
2 1 -29 6.00 4.00
2 1 29 10.20 4.30
2 -1 -29 3.20 3.70
-2 1 -29 8.20 4.20
-2 -1 29 3.00 4.00
0 -2 29 3.80 4.10
0 2 -29 8.60 4.30
0 -2 -29 14.30 4.70
0 2 29 7.30 3.80
-1 2 29 54.49 6.70
-1 -2 -29 55.89 6.60
1 2 -29 55.49 6.70
1 -2 29 52.79 6.70
1 -2 -29 59.39 6.70
1 2 29 56.29 6.90
-1 2 -29 64.39 7.20
-1 -2 29 59.59 6.90
2 2 -29 25.50 5.20
-2 -2 -29 20.70 4.90
2 -2 -29 28.20 5.20
-2 2 -29 27.50 5.30
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_radiation_probe x-ray
_diffrn_radiation_wavelength 0.71073
_diffrn_standards_number 0
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_decay_% ?
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_theta_min 2.942
_diffrn_reflns_theta_max 27.521
_diffrn_reflns_av_unetI/netI 0.067916
_diffrn_reflns_number 33137
_diffrn_reflns_number_extinctions 0
_diffrn_reflns_number_accepted 33137
_diffrn_reflns_number_rejected 0
_diffrn_ambient_temperature 297(2)
_computing_data_collection ?
_computing_cell_refinement ?
_computing_data_reduction ?
_exptl_crystal_description ?
_exptl_crystal_colour ?
_exptl_crystal_size_max 0.33
_exptl_crystal_size_mid 0.225
_exptl_crystal_size_min 0.114
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F000 1016
_cell_length_a 9.9759(2)
_cell_length_b 10.6052(2)
_cell_length_c 22.8535(4)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2417.82(8)
_cell_measurement_temperature 297(2)
_cell_measurement_wavelength 0.71073
_cell_measurement_reflns_used 0
_cell_measurement_theta_max 0
_cell_measurement_theta_min 0
_exptl_absorpt_coefficient_mu 0.099
_exptl_absorpt_correction_type ?
loop_
_atom_type_symbol
_atom_type_number_in_cell
C 100
H 104
N 8
O 32
_cell_formula_units_Z 4
_chemical_formula_moiety 'C25 H26 N2 O8'
_chemical_formula_sum 'C25 H26 N2 O8'
_chemical_compound_source ?
_space_group_crystal_system orthorhombic
_space_group_name_H-M_alt P212121
_space_group_name_Hall 'P 2ac 2ab'
_space_group_IT_number 19
_computing_structure_solution ?
_computing_structure_refinement 'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics 'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material
'WinGX publication routines (Farrugia, 2012)'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_refine_ls_number_constraints 0
_refine_ls_number_restraints 0
;
_shelx_hkl_checksum 88912
_shelx_res_file
;
TITL 2_0m_a.res in P2(1)2(1)2(1)
shelx.res
created by SHELXL-2018/3 at 18:23:59 on 13-Apr-2020
CELL 0.71073 9.9759 10.6052 22.8535 90.000 90.000 90.000
ZERR 4.00 0.0002 0.0002 0.0004 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 96 128 8 36
MERG 2
OMIT -3.00 50.00
DFIX 0.82 0.02 O1 H1'
DFIX 0.82 0.02 O3 H3'
DFIX 0.82 0.02 O9 H9A
DFIX 0.82 0.02 O9 H9B
MPLA C1 C2 C3 C4 C5 C6
MPLA C9 C10 C11 C12 C13 C14
EQIV $1 x+1/2, -y+1/2, -z+1
HTAB N1 O6_$1
EQIV $2 -x+1, y-1/2, -z+1/2
HTAB N1 O4_$2
HTAB N1 O9_$2
HTAB O2 O6
EQIV $3 -x, y-1/2, -z+3/2
HTAB N2 O8_$3
EQIV $4 -x+1/2, -y+1, z+1/2
HTAB N2 O5_$4
HTAB N2 O7
HTAB O4 O9
HTAB C6 O6
EQIV $5 -x, y+1/2, -z+1/2
HTAB C12 O2_$5
HTAB O1 O8
HTAB O3 O2_$5
EQIV $6 x+1/2, -y+3/2, -z+1
HTAB O9 O7_$6
FMAP 2
PLAN 20
SIZE 0.114 0.225 0.330
ACTA
HTAB 2.00000
BOND $H
CONF
LIST 4
L.S. 20
TEMP 24.00
WGHT 0.060300 1.019200
FVAR 0.91720
O1 4 0.131545 0.615927 0.615816 11.00000 0.07269 0.05443 =
0.03055 0.00106 0.00301 0.01380
N1 3 0.775143 0.318237 0.470971 11.00000 0.03326 0.05294 =
0.04813 0.00356 0.00184 0.00655
AFIX 23
H1A 2 0.821241 0.251273 0.483057 11.00000 -1.20000
H1B 2 0.765150 0.313168 0.432344 11.00000 -1.20000
AFIX 0
C1 1 0.116467 0.644219 0.558209 11.00000 0.04736 0.03578 =
0.03089 -0.00308 -0.00012 -0.00279
O2 4 0.266116 0.541511 0.420475 11.00000 0.04753 0.05716 =
0.03220 -0.00393 -0.00418 0.01758
AFIX 148
H2' 2 0.323082 0.489499 0.440547 11.00000 -1.50000
AFIX 0
N2 3 -0.078174 0.492602 0.794010 11.00000 0.05134 0.02737 =
0.03115 -0.00076 0.00407 -0.00060
AFIX 23
H2A 2 -0.032399 0.421409 0.799100 11.00000 -1.20000
H2B 2 -0.055795 0.546139 0.822364 11.00000 -1.20000
AFIX 0
C2 1 0.026129 0.733528 0.538672 11.00000 0.05320 0.04585 =
0.03877 -0.00220 0.00719 0.01284
AFIX 43
H2 2 -0.026401 0.778272 0.565113 11.00000 -1.20000
AFIX 0
O3 4 -0.266616 0.993310 0.198999 11.00000 0.05263 0.07674 =
0.04077 0.01869 -0.00149 0.00609
C3 1 0.015014 0.755320 0.479468 11.00000 0.05380 0.04730 =
0.04395 0.00529 0.00142 0.01716
AFIX 43
H3 2 -0.047640 0.814001 0.466565 11.00000 -1.20000
AFIX 0
O4 4 0.096918 0.738649 0.139454 11.00000 0.12623 0.09750 =
0.05464 0.00310 0.03858 0.03864
AFIX 148
H4' 2 0.189590 0.722648 0.152562 11.00000 -1.50000
AFIX 0
C4 1 0.094161 0.692803 0.437694 11.00000 0.03684 0.03791 =
0.03586 -0.00057 -0.00061 0.00315
O5 4 0.577846 0.421199 0.411137 11.00000 0.05569 0.06757 =
0.03264 0.01276 0.00332 0.00659
C5 1 0.185838 0.604079 0.459102 11.00000 0.03104 0.03429 =
0.03157 -0.00518 -0.00223 -0.00298
O6 4 0.417955 0.374340 0.475242 11.00000 0.03127 0.05893 =
0.05650 0.01413 0.00129 0.00632
C6 1 0.195670 0.579240 0.518872 11.00000 0.03510 0.03713 =
0.03391 0.00034 -0.00544 0.00138
AFIX 43
H6 2 0.255747 0.518732 0.532283 11.00000 -1.20000
AFIX 0
O7 4 -0.044175 0.742524 0.787186 11.00000 0.19061 0.03380 =
0.04300 -0.01069 0.03053 -0.00755
C7 1 0.081882 0.718126 0.374847 11.00000 0.04845 0.04353 =
0.03577 0.00166 0.00337 0.00782
AFIX 43
H7 2 0.147494 0.684006 0.350660 11.00000 -1.20000
AFIX 0
O8 4 -0.001354 0.745661 0.692761 11.00000 0.09897 0.03034 =
0.03944 0.00204 0.01177 -0.00384
C8 1 -0.013344 0.784689 0.349325 11.00000 0.04360 0.05552 =
0.03596 0.00329 0.00186 0.00847
AFIX 43
H8 2 -0.078062 0.818540 0.374046 11.00000 -1.20000
AFIX 0
O9 4 0.331212 0.640690 0.126593 11.00000 0.10865 0.07242 =
0.11518 -0.02189 -0.05584 0.01561
C9 1 -0.029863 0.811987 0.286703 11.00000 0.04176 0.04141 =
0.03405 0.00454 0.00148 -0.00074
C10 1 -0.135325 0.890150 0.270124 11.00000 0.04335 0.04793 =
0.03412 0.00573 0.00576 0.00068
AFIX 43
H10 2 -0.190263 0.925334 0.298660 11.00000 -1.20000
AFIX 0
C11 1 -0.159464 0.916158 0.211796 11.00000 0.04561 0.04579 =
0.03625 0.00739 -0.00012 -0.00695
C12 1 -0.079151 0.865592 0.169096 11.00000 0.07228 0.05215 =
0.03126 0.00649 0.00200 -0.00277
AFIX 43
H12 2 -0.094718 0.884207 0.129914 11.00000 -1.20000
AFIX 0
C13 1 0.024207 0.787417 0.184683 11.00000 0.07422 0.04910 =
0.04109 0.00019 0.02060 0.00251
C14 1 0.051665 0.759310 0.243177 11.00000 0.05391 0.04287 =
0.04486 0.00583 0.00504 0.00432
AFIX 43
H14 2 0.122696 0.706643 0.253042 11.00000 -1.20000
AFIX 0
C15 1 0.537642 0.377013 0.457387 11.00000 0.03478 0.03828 =
0.03404 0.00050 -0.00104 0.00340
C16 1 0.641220 0.322325 0.500270 11.00000 0.03181 0.04574 =
0.03572 0.00890 0.00127 0.00066
AFIX 13
H16 2 0.614353 0.237957 0.513251 11.00000 -1.20000
AFIX 0
C17 1 0.665513 0.408575 0.552622 11.00000 0.05659 0.09462 =
0.03564 -0.00537 -0.00517 0.00009
AFIX 23
H17A 2 0.583267 0.450158 0.564463 11.00000 -1.20000
H17B 2 0.700761 0.361392 0.585567 11.00000 -1.20000
AFIX 0
C18 1 0.765318 0.501677 0.531074 11.00000 0.09225 0.09444 =
0.08848 -0.03335 0.00398 -0.02782
AFIX 23
H18A 2 0.720375 0.573782 0.513840 11.00000 -1.20000
H18B 2 0.821256 0.530953 0.563023 11.00000 -1.20000
AFIX 0
C19 1 0.847226 0.436196 0.486782 11.00000 0.05254 0.05820 =
0.13541 0.00020 0.01764 -0.01235
AFIX 23
H19A 2 0.935075 0.416595 0.502539 11.00000 -1.20000
H19B 2 0.858597 0.489086 0.452511 11.00000 -1.20000
AFIX 0
C20 1 -0.046780 0.548516 0.735471 11.00000 0.04609 0.02738 =
0.02585 -0.00161 0.00208 0.00056
AFIX 13
H20 2 0.035826 0.510986 0.720132 11.00000 -1.20000
AFIX 0
C21 1 -0.164546 0.511549 0.696553 11.00000 0.07867 0.06540 =
0.05105 0.00287 -0.02347 -0.01785
AFIX 23
H21A 2 -0.210407 0.586187 0.682371 11.00000 -1.20000
H21B 2 -0.133480 0.463214 0.663169 11.00000 -1.20000
AFIX 0
C22 1 -0.258028 0.432663 0.733984 11.00000 0.06202 0.07678 =
0.09641 0.00379 -0.01786 -0.02225
AFIX 23
H22A 2 -0.350908 0.452288 0.725335 11.00000 -1.20000
H22B 2 -0.243179 0.343458 0.727209 11.00000 -1.20000
AFIX 0
C23 1 -0.224527 0.466934 0.795601 11.00000 0.05295 0.06881 =
0.07494 0.00740 0.01548 -0.00541
AFIX 23
H23A 2 -0.273919 0.541110 0.807923 11.00000 -1.20000
H23B 2 -0.244741 0.397964 0.822045 11.00000 -1.20000
AFIX 0
C24 1 -0.030066 0.691268 0.739931 11.00000 0.07348 0.02896 =
0.03406 -0.00392 0.00584 0.00164
H1' 2 0.079673 0.660034 0.636088 11.00000 -1.50000
H3' 2 -0.269514 1.004196 0.162296 11.00000 -1.50000
H9A 2 0.375541 0.669896 0.157634 11.00000 -1.20000
H9B 2 0.419143 0.643875 0.103051 11.00000 -1.20000
HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00
REM 2_0m_a.res in P2(1)2(1)2(1)
REM wR2 = 0.1167, GooF = S = 1.049, Restrained GooF = 1.064 for all data
REM R1 = 0.0439 for 4046 Fo > 4sig(Fo) and 0.0459 for all 4237 data
REM 332 parameters refined using 4 restraints
END
WGHT 0.0603 1.0183
REM Instructions for potential hydrogen bonds
HTAB N1 O6_$1
HTAB N1 O4_$2
HTAB N1 O9_$2
HTAB O2 O6
HTAB N2 O8_$3
HTAB N2 O5_$4
HTAB N2 O7
HTAB O4 O9
HTAB C6 O6
HTAB C12 O2_$5
HTAB O1 O8
HTAB O3 O2_$5
HTAB O9 O7_$6
REM Highest difference peak 0.349, deepest hole -0.312, 1-sigma level 0.039
Q1 1 0.1815 0.7606 0.1601 11.00000 0.05 0.35
Q2 1 0.8231 0.4322 0.5473 11.00000 0.05 0.22
Q3 1 -0.1220 0.7224 0.7940 11.00000 0.05 0.19
Q4 1 -0.0415 0.9034 0.2832 11.00000 0.05 0.15
Q5 1 0.0839 0.8007 0.2060 11.00000 0.05 0.15
Q6 1 0.0121 0.8160 0.6914 11.00000 0.05 0.14
Q7 1 0.3579 0.5432 0.1343 11.00000 0.05 0.14
Q8 1 -0.0011 0.7007 0.3534 11.00000 0.05 0.13
Q9 1 0.6378 0.3466 0.5345 11.00000 0.05 0.12
Q10 1 -0.0633 0.6201 0.7357 11.00000 0.05 0.12
Q11 1 0.0387 0.6485 0.5442 11.00000 0.05 0.12
Q12 1 0.9098 0.3937 0.5622 11.00000 0.05 0.12
Q13 1 0.1018 0.6227 0.4475 11.00000 0.05 0.12
Q14 1 0.1219 0.7356 0.5549 11.00000 0.05 0.12
Q15 1 -0.0085 0.7212 0.7973 11.00000 0.05 0.12
Q16 1 0.0970 0.7460 0.4571 11.00000 0.05 0.12
Q17 1 0.0420 0.6966 0.4515 11.00000 0.05 0.11
Q18 1 -0.1030 0.7620 0.3742 11.00000 0.05 0.11
Q19 1 -0.2388 0.6033 0.8059 11.00000 0.05 0.11
Q20 1 0.7956 0.5694 0.5586 11.00000 0.05 0.11
;
_shelx_res_checksum 3740
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 0.1315(3) 0.6159(2) 0.61582(10) 0.0526(7) Uani d 1 . .
N N1 0.7751(3) 0.3182(3) 0.47097(13) 0.0448(7) Uani d 1 . .
H H1A 0.821241 0.251273 0.483057 0.054 Uiso calc 1 . .
H H1B 0.765150 0.313168 0.432344 0.054 Uiso calc 1 . .
C C1 0.1165(3) 0.6442(3) 0.55821(13) 0.0380(7) Uani d 1 . .
O O2 0.2661(2) 0.5415(2) 0.42047(10) 0.0456(6) Uani d 1 . .
H H2' 0.323(4) 0.489(4) 0.4405(11) 0.068 Uiso calc 1 . .
N N2 -0.0782(3) 0.4926(2) 0.79401(11) 0.0366(6) Uani d 1 . .
H H2A -0.032399 0.421409 0.799100 0.044 Uiso calc 1 . .
H H2B -0.055795 0.546139 0.822364 0.044 Uiso calc 1 . .
C C2 0.0261(4) 0.7335(3) 0.53867(14) 0.0459(8) Uani d 1 . .
H H2 -0.026401 0.778272 0.565113 0.055 Uiso calc 1 . .
O O3 -0.2666(3) 0.9933(3) 0.19900(11) 0.0567(7) Uani d 1 . .
C C3 0.0150(4) 0.7553(3) 0.47947(14) 0.0484(8) Uani d 1 . .
H H3 -0.047640 0.814001 0.466565 0.058 Uiso calc 1 . .
O O4 0.0969(5) 0.7386(4) 0.13945(13) 0.0928(13) Uani d 1 . .
H H4' 0.190(8) 0.723(8) 0.1526(16) 0.139 Uiso calc 1 . .
C C4 0.0942(3) 0.6928(3) 0.43769(13) 0.0369(7) Uani d 1 . .
O O5 0.5778(3) 0.4212(3) 0.41114(10) 0.0520(6) Uani d 1 . .
C C5 0.1858(3) 0.6041(3) 0.45910(12) 0.0323(6) Uani d 1 . .
O O6 0.4180(2) 0.3743(2) 0.47524(11) 0.0489(6) Uani d 1 . .
C C6 0.1957(3) 0.5792(3) 0.51887(13) 0.0354(6) Uani d 1 . .
H H6 0.255747 0.518732 0.532283 0.042 Uiso calc 1 . .
O O7 -0.0442(5) 0.7425(2) 0.78719(12) 0.0891(13) Uani d 1 . .
C C7 0.0819(4) 0.7181(3) 0.37485(14) 0.0426(7) Uani d 1 . .
H H7 0.147494 0.684006 0.350660 0.051 Uiso calc 1 . .
O O8 -0.0014(3) 0.7457(2) 0.69276(10) 0.0562(7) Uani d 1 . .
C C8 -0.0133(4) 0.7847(4) 0.34932(14) 0.0450(8) Uani d 1 . .
H H8 -0.078062 0.818540 0.374046 0.054 Uiso calc 1 . .
O O9 0.3312(5) 0.6407(4) 0.1266(2) 0.0987(14) Uani d 1 . .
C C9 -0.0299(3) 0.8120(3) 0.28670(14) 0.0391(7) Uani d 1 . .
C C10 -0.1353(3) 0.8902(3) 0.27012(14) 0.0418(7) Uani d 1 . .
H H10 -0.190263 0.925334 0.298660 0.050 Uiso calc 1 . .
C C11 -0.1595(3) 0.9162(3) 0.21180(14) 0.0426(7) Uani d 1 . .
C C12 -0.0792(4) 0.8656(4) 0.16910(15) 0.0519(9) Uani d 1 . .
H H12 -0.094718 0.884207 0.129914 0.062 Uiso calc 1 . .
C C13 0.0242(4) 0.7874(4) 0.18468(15) 0.0548(9) Uani d 1 . .
C C14 0.0517(4) 0.7593(3) 0.24318(15) 0.0472(8) Uani d 1 . .
H H14 0.122696 0.706643 0.253042 0.057 Uiso calc 1 . .
C C15 0.5376(3) 0.3770(3) 0.45739(13) 0.0357(7) Uani d 1 . .
C C16 0.6412(3) 0.3223(3) 0.50027(14) 0.0378(7) Uani d 1 . .
H H16 0.614353 0.237957 0.513251 0.045 Uiso calc 1 . .
C C17 0.6655(4) 0.4086(5) 0.55262(16) 0.0623(11) Uani d 1 . .
H H17A 0.583267 0.450158 0.564463 0.075 Uiso calc 1 . .
H H17B 0.700761 0.361392 0.585567 0.075 Uiso calc 1 . .
C C18 0.7653(6) 0.5017(6) 0.5311(3) 0.0917(17) Uani d 1 . .
H H18A 0.720375 0.573782 0.513840 0.110 Uiso calc 1 . .
H H18B 0.821256 0.530953 0.563023 0.110 Uiso calc 1 . .
C C19 0.8472(5) 0.4362(5) 0.4868(3) 0.0820(15) Uani d 1 . .
H H19A 0.935075 0.416595 0.502539 0.098 Uiso calc 1 . .
H H19B 0.858597 0.489086 0.452511 0.098 Uiso calc 1 . .
C C20 -0.0468(3) 0.5485(3) 0.73547(12) 0.0331(6) Uani d 1 . .
H H20 0.035826 0.510986 0.720132 0.040 Uiso calc 1 . .
C C21 -0.1645(5) 0.5115(4) 0.69655(18) 0.0650(11) Uani d 1 . .
H H21A -0.210407 0.586187 0.682371 0.078 Uiso calc 1 . .
H H21B -0.133480 0.463214 0.663169 0.078 Uiso calc 1 . .
C C22 -0.2580(5) 0.4327(5) 0.7340(2) 0.0784(14) Uani d 1 . .
H H22A -0.350908 0.452288 0.725335 0.094 Uiso calc 1 . .
H H22B -0.243179 0.343458 0.727209 0.094 Uiso calc 1 . .
C C23 -0.2245(4) 0.4669(4) 0.7956(2) 0.0656(11) Uani d 1 . .
H H23A -0.273919 0.541110 0.807923 0.079 Uiso calc 1 . .
H H23B -0.244741 0.397964 0.822045 0.079 Uiso calc 1 . .
C C24 -0.0301(4) 0.6913(3) 0.73993(14) 0.0455(8) Uani d 1 . .
H H1' 0.080(4) 0.660(4) 0.6361(18) 0.068 Uiso d 1 . .
H H3' -0.270(5) 1.004(5) 0.1623(11) 0.068 Uiso d 1 . .
H H9A 0.376(4) 0.670(4) 0.1576(14) 0.055 Uiso d 1 . .
H H9B 0.419(3) 0.644(4) 0.1031(16) 0.055 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 0.0727(17) 0.0544(15) 0.0305(11) 0.0138(13) 0.0030(11) 0.0011(11)
N1 0.0333(14) 0.0529(17) 0.0481(16) 0.0065(12) 0.0018(12) 0.0036(13)
C1 0.0474(18) 0.0358(16) 0.0309(15) -0.0028(14) -0.0001(13) -0.0031(12)
O2 0.0475(13) 0.0572(14) 0.0322(12) 0.0176(11) -0.0042(10) -0.0039(10)
N2 0.0513(16) 0.0274(12) 0.0311(13) -0.0006(11) 0.0041(11) -0.0008(10)
C2 0.0532(19) 0.0458(18) 0.0388(17) 0.0128(16) 0.0072(15) -0.0022(14)
O3 0.0526(15) 0.0767(18) 0.0408(14) 0.0061(14) -0.0015(11) 0.0187(14)
C3 0.054(2) 0.0473(19) 0.0439(18) 0.0172(16) 0.0014(16) 0.0053(15)
O4 0.126(3) 0.097(3) 0.0546(17) 0.039(2) 0.0386(19) 0.0031(18)
C4 0.0368(16) 0.0379(16) 0.0359(16) 0.0031(13) -0.0006(13) -0.0006(13)
O5 0.0557(14) 0.0676(16) 0.0326(11) 0.0066(12) 0.0033(11) 0.0128(11)
C5 0.0310(14) 0.0343(15) 0.0316(14) -0.0030(12) -0.0022(11) -0.0052(12)
O6 0.0313(12) 0.0589(15) 0.0565(14) 0.0063(11) 0.0013(10) 0.0141(12)
C6 0.0351(15) 0.0371(15) 0.0339(15) 0.0014(12) -0.0054(12) 0.0003(13)
O7 0.191(4) 0.0338(13) 0.0430(14) -0.0075(19) 0.031(2) -0.0107(12)
C7 0.0484(18) 0.0435(18) 0.0358(16) 0.0078(15) 0.0034(14) 0.0017(14)
O8 0.099(2) 0.0303(11) 0.0394(12) -0.0038(13) 0.0118(13) 0.0020(10)
C8 0.0436(18) 0.056(2) 0.0360(17) 0.0085(16) 0.0019(14) 0.0033(15)
O9 0.109(3) 0.072(2) 0.115(3) 0.016(2) -0.056(3) -0.022(2)
C9 0.0418(16) 0.0414(17) 0.0341(15) -0.0007(14) 0.0015(14) 0.0045(13)
C10 0.0434(17) 0.0479(18) 0.0341(16) 0.0007(15) 0.0058(13) 0.0057(14)
C11 0.0456(18) 0.0458(18) 0.0363(16) -0.0069(15) -0.0001(14) 0.0074(14)
C12 0.072(2) 0.052(2) 0.0313(16) -0.0028(19) 0.0020(16) 0.0065(15)
C13 0.074(2) 0.0491(19) 0.0411(19) 0.0025(19) 0.0206(18) 0.0002(16)
C14 0.054(2) 0.0429(18) 0.0449(18) 0.0043(15) 0.0050(16) 0.0058(15)
C15 0.0348(16) 0.0383(16) 0.0340(16) 0.0034(13) -0.0010(12) 0.0005(13)
C16 0.0318(15) 0.0457(18) 0.0357(15) 0.0007(13) 0.0013(13) 0.0089(13)
C17 0.057(2) 0.095(3) 0.0356(18) 0.000(2) -0.0052(16) -0.005(2)
C18 0.092(4) 0.094(4) 0.088(4) -0.028(3) 0.004(3) -0.033(3)
C19 0.053(2) 0.058(3) 0.135(5) -0.012(2) 0.018(3) 0.000(3)
C20 0.0461(17) 0.0274(13) 0.0259(13) 0.0006(12) 0.0021(12) -0.0016(11)
C21 0.079(3) 0.065(3) 0.051(2) -0.018(2) -0.023(2) 0.003(2)
C22 0.062(3) 0.077(3) 0.096(4) -0.022(2) -0.018(2) 0.004(3)
C23 0.053(2) 0.069(3) 0.075(3) -0.005(2) 0.015(2) 0.007(2)
C24 0.073(2) 0.0290(15) 0.0341(16) 0.0016(15) 0.0058(16) -0.0039(13)
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' . . 110(3) ?
C19 N1 C16 . . 107.4(3) ?
C19 N1 H1A . . 110.2 ?
C16 N1 H1A . . 110.2 ?
C19 N1 H1B . . 110.2 ?
C16 N1 H1B . . 110.2 ?
H1A N1 H1B . . 108.5 ?
O1 C1 C6 . . 117.2(3) ?
O1 C1 C2 . . 122.5(3) ?
C6 C1 C2 . . 120.3(3) ?
C5 O2 H2' . . 109.5 ?
C23 N2 C20 . . 107.5(3) ?
C23 N2 H2A . . 110.2 ?
C20 N2 H2A . . 110.2 ?
C23 N2 H2B . . 110.2 ?
C20 N2 H2B . . 110.2 ?
H2A N2 H2B . . 108.5 ?
C3 C2 C1 . . 119.0(3) ?
C3 C2 H2 . . 120.5 ?
C1 C2 H2 . . 120.5 ?
C11 O3 H3' . . 109(3) ?
C2 C3 C4 . . 122.9(3) ?
C2 C3 H3 . . 118.6 ?
C4 C3 H3 . . 118.6 ?
C13 O4 H4' . . 109.5 ?
C5 C4 C3 . . 116.5(3) ?
C5 C4 C7 . . 121.3(3) ?
C3 C4 C7 . . 122.2(3) ?
O2 C5 C6 . . 120.0(3) ?
O2 C5 C4 . . 119.0(3) ?
C6 C5 C4 . . 121.0(3) ?
C1 C6 C5 . . 120.2(3) ?
C1 C6 H6 . . 119.9 ?
C5 C6 H6 . . 119.9 ?
C8 C7 C4 . . 126.2(3) ?
C8 C7 H7 . . 116.9 ?
C4 C7 H7 . . 116.9 ?
C7 C8 C9 . . 128.1(3) ?
C7 C8 H8 . . 116.0 ?
C9 C8 H8 . . 116.0 ?
H9A O9 H9B . . 89(3) ?
C10 C9 C14 . . 118.9(3) ?
C10 C9 C8 . . 117.9(3) ?
C14 C9 C8 . . 123.2(3) ?
C11 C10 C9 . . 120.9(3) ?
C11 C10 H10 . . 119.6 ?
C9 C10 H10 . . 119.6 ?
C12 C11 O3 . . 122.3(3) ?
C12 C11 C10 . . 120.4(3) ?
O3 C11 C10 . . 117.3(3) ?
C13 C12 C11 . . 119.4(3) ?
C13 C12 H12 . . 120.3 ?
C11 C12 H12 . . 120.3 ?
O4 C13 C12 . . 115.6(3) ?
O4 C13 C14 . . 122.7(4) ?
C12 C13 C14 . . 121.7(3) ?
C13 C14 C9 . . 118.7(3) ?
C13 C14 H14 . . 120.6 ?
C9 C14 H14 . . 120.6 ?
O5 C15 O6 . . 126.7(3) ?
O5 C15 C16 . . 118.3(3) ?
O6 C15 C16 . . 114.9(3) ?
N1 C16 C17 . . 103.1(3) ?
N1 C16 C15 . . 109.0(2) ?
C17 C16 C15 . . 112.4(3) ?
N1 C16 H16 . . 110.7 ?
C17 C16 H16 . . 110.7 ?
C15 C16 H16 . . 110.7 ?
C18 C17 C16 . . 104.2(3) ?
C18 C17 H17A . . 110.9 ?
C16 C17 H17A . . 110.9 ?
C18 C17 H17B . . 110.9 ?
C16 C17 H17B . . 110.9 ?
H17A C17 H17B . . 108.9 ?
C19 C18 C17 . . 106.6(4) ?
C19 C18 H18A . . 110.4 ?
C17 C18 H18A . . 110.4 ?
C19 C18 H18B . . 110.4 ?
C17 C18 H18B . . 110.4 ?
H18A C18 H18B . . 108.6 ?
C18 C19 N1 . . 107.2(4) ?
C18 C19 H19A . . 110.3 ?
N1 C19 H19A . . 110.3 ?
C18 C19 H19B . . 110.3 ?
N1 C19 H19B . . 110.3 ?
H19A C19 H19B . . 108.5 ?
N2 C20 C21 . . 105.0(3) ?
N2 C20 C24 . . 110.9(2) ?
C21 C20 C24 . . 112.2(3) ?
N2 C20 H20 . . 109.6 ?
C21 C20 H20 . . 109.6 ?
C24 C20 H20 . . 109.6 ?
C22 C21 C20 . . 106.6(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 . . 105.1(3) ?
C23 C22 H22A . . 110.7 ?
C21 C22 H22A . . 110.7 ?
C23 C22 H22B . . 110.7 ?
C21 C22 H22B . . 110.7 ?
H22A C22 H22B . . 108.8 ?
N2 C23 C22 . . 104.0(3) ?
N2 C23 H23A . . 111.0 ?
C22 C23 H23A . . 111.0 ?
N2 C23 H23B . . 111.0 ?
C22 C23 H23B . . 111.0 ?
H23A C23 H23B . . 109.0 ?
O7 C24 O8 . . 125.7(3) ?
O7 C24 C20 . . 119.3(3) ?
O8 C24 C20 . . 115.0(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 . 1.359(4) ?
O1 H1' . 0.84(2) ?
N1 C19 . 1.487(6) n
N1 C16 . 1.495(4) n
N1 H1A . 0.8900 ?
N1 H1B . 0.8900 ?
C1 C6 . 1.381(5) ?
C1 C2 . 1.382(5) ?
O2 C5 . 1.364(4) ?
O2 H2' . 0.92(5) ?
N2 C23 . 1.486(5) n
N2 C20 . 1.496(4) n
N2 H2A . 0.8900 ?
N2 H2B . 0.8900 ?
C2 C3 . 1.377(5) ?
C2 H2 . 0.9300 ?
O3 C11 . 1.378(4) ?
O3 H3' . 0.85(2) ?
C3 C4 . 1.405(5) ?
C3 H3 . 0.9300 ?
O4 C13 . 1.365(4) ?
O4 H4' . 0.99(8) ?
C4 C5 . 1.400(4) ?
C4 C7 . 1.466(4) ?
O5 C15 . 1.224(4) n
C5 C6 . 1.395(4) ?
O6 C15 . 1.262(4) n
C6 H6 . 0.9300 ?
O7 C24 . 1.217(4) n
C7 C8 . 1.319(5) ?
C7 H7 . 0.9300 ?
O8 C24 . 1.256(4) n
C8 C9 . 1.469(4) ?
C8 H8 . 0.9300 ?
O9 H9A . 0.89(2) ?
O9 H9B . 1.03(2) ?
C9 C10 . 1.392(5) ?
C9 C14 . 1.401(5) ?
C10 C11 . 1.382(4) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.372(5) ?
C12 C13 . 1.370(6) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.397(5) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.538(4) ?
C16 C17 . 1.525(5) ?
C16 H16 . 0.9800 ?
C17 C18 . 1.486(7) ?
C17 H17A . 0.9700 ?
C17 H17B . 0.9700 ?
C18 C19 . 1.475(8) ?
C18 H18A . 0.9700 ?
C18 H18B . 0.9700 ?
C19 H19A . 0.9700 ?
C19 H19B . 0.9700 ?
C20 C21 . 1.525(5) ?
C20 C24 . 1.526(4) ?
C20 H20 . 0.9800 ?
C21 C22 . 1.517(6) ?
C21 H21A . 0.9700 ?
C21 H21B . 0.9700 ?
C22 C23 . 1.492(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 . 0.84(2) 1.78(3) 2.597(3) 166(5) yes
O2 H2' O6 . 0.92 1.74 2.647(3) 172 yes
O3 H3' O2 3 0.85(2) 1.93(3) 2.778(3) 175(5) yes
O4 H4' O9 . 0.99 1.76 2.575(6) 137 yes
O9 H9A O7 2_566 0.89(2) 1.76(3) 2.639(5) 168(4) yes
N1 H1A O6 2_556 0.89 1.90 2.777(4) 168 yes
N1 H1B O4 3_645 0.89 2.28 2.951(4) 132 yes
N1 H1B O9 3_645 0.89 2.47 3.105(5) 129 yes
N2 H2A O8 3_546 0.89 1.90 2.753(3) 159 yes
N2 H2B O5 4_565 0.89 2.07 2.829(3) 143 yes
N2 H2B O7 . 0.89 2.24 2.677(4) 110 yes
C6 H6 O6 . 0.93 2.58 3.261(4) 130 yes
C12 H12 O2 3 0.93 2.65 3.339(5) 131 no
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 . . . . -178.9(3) ?
C6 C1 C2 C3 . . . . 0.9(5) ?
C1 C2 C3 C4 . . . . -1.6(6) ?
C2 C3 C4 C5 . . . . 0.8(5) ?
C2 C3 C4 C7 . . . . -179.4(4) ?
C3 C4 C5 O2 . . . . -179.4(3) ?
C7 C4 C5 O2 . . . . 0.8(5) ?
C3 C4 C5 C6 . . . . 0.7(5) ?
C7 C4 C5 C6 . . . . -179.1(3) ?
O1 C1 C6 C5 . . . . -179.7(3) ?
C2 C1 C6 C5 . . . . 0.5(5) ?
O2 C5 C6 C1 . . . . 178.7(3) ?
C4 C5 C6 C1 . . . . -1.4(5) ?
C5 C4 C7 C8 . . . . 169.2(4) ?
C3 C4 C7 C8 . . . . -10.6(6) ?
C4 C7 C8 C9 . . . . -179.7(3) ?
C7 C8 C9 C10 . . . . -176.9(4) ?
C7 C8 C9 C14 . . . . 5.8(6) ?
C14 C9 C10 C11 . . . . -0.3(5) ?
C8 C9 C10 C11 . . . . -177.7(3) ?
C9 C10 C11 C12 . . . . -0.3(5) ?
C9 C10 C11 O3 . . . . 179.3(3) ?
O3 C11 C12 C13 . . . . -178.7(3) ?
C10 C11 C12 C13 . . . . 1.0(5) ?
C11 C12 C13 O4 . . . . 178.4(4) ?
C11 C12 C13 C14 . . . . -1.1(6) ?
O4 C13 C14 C9 . . . . -178.9(4) ?
C12 C13 C14 C9 . . . . 0.6(6) ?
C10 C9 C14 C13 . . . . 0.1(5) ?
C8 C9 C14 C13 . . . . 177.5(4) ?
C19 N1 C16 C17 . . . . -25.4(4) ?
C19 N1 C16 C15 . . . . 94.1(4) ?
O5 C15 C16 N1 . . . . -8.3(4) ?
O6 C15 C16 N1 . . . . 173.7(3) ?
O5 C15 C16 C17 . . . . 105.3(4) ?
O6 C15 C16 C17 . . . . -72.7(4) ?
N1 C16 C17 C18 . . . . 33.9(4) ?
C15 C16 C17 C18 . . . . -83.3(4) ?
C16 C17 C18 C19 . . . . -30.2(6) ?
C17 C18 C19 N1 . . . . 14.5(6) ?
C16 N1 C19 C18 . . . . 7.3(6) ?
C23 N2 C20 C21 . . . . -19.7(4) ?
C23 N2 C20 C24 . . . . 101.7(3) ?
N2 C20 C21 C22 . . . . -1.4(4) ?
C24 C20 C21 C22 . . . . -121.9(4) ?
C20 C21 C22 C23 . . . . 21.6(5) ?
C20 N2 C23 C22 . . . . 33.4(4) ?
C21 C22 C23 N2 . . . . -33.4(5) ?
N2 C20 C24 O7 . . . . -0.7(5) ?
C21 C20 C24 O7 . . . . 116.3(4) ?
N2 C20 C24 O8 . . . . 178.9(3) ?
C21 C20 C24 O8 . . . . -64.1(5) ?
_cod_database_fobs_code 2243567