#------------------------------------------------------------------------------
#$Date: 2024-05-18 04:51:34 +0300 (Sat, 18 May 2024) $
#$Revision: 291950 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023130.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_2023130
loop_
_publ_author_name
'Abad, Nadeem'
'Mague, Joel T.'
'Alsubari, Abdulsalam'
'Essassi, El Mokhtar'
'Alzahrani, Abdullah Yahya Abdullah'
'Ramli, Youssef'
_publ_section_title
;
Synthesis, crystal structure and Hirshfeld surface analysis of
1-[3-(2-oxo-3-phenyl-1,2-dihydroquinoxalin-1-yl)propyl]-3-phenyl-1,2-dihydroquinoxalin-2-one
;
_journal_coeditor_code VM2302
_journal_issue 6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024004377
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C31 H24 N4 O2'
_chemical_formula_moiety 'C31 H24 N4 O2'
_chemical_formula_sum 'C31 H24 N4 O2'
_chemical_formula_weight 484.54
_chemical_name_systematic
1-[3-(2-Oxo-3-phenyl-1,2-dihydroquinoxalin-1-yl)propyl]-3-phenyl-1,2-dihydroquinoxalin-2-one
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/1
_cell_angle_alpha 77.2670(10)
_cell_angle_beta 83.9910(10)
_cell_angle_gamma 72.7080(10)
_cell_formula_units_Z 2
_cell_length_a 9.0384(3)
_cell_length_b 9.4484(4)
_cell_length_c 14.9524(6)
_cell_measurement_reflns_used 7750
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 28.6245
_cell_measurement_theta_min 2.4449
_cell_volume 1188.16(8)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2019/1 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type 'Bruker SMART APEX CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0270
_diffrn_reflns_av_unetI/netI 0.0350
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 23105
_diffrn_reflns_theta_full 28.500
_diffrn_reflns_theta_max 29.160
_diffrn_reflns_theta_min 2.304
_diffrn_source 'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu 0.087
_exptl_absorpt_correction_T_max 0.99
_exptl_absorpt_correction_T_min 0.89
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS;Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.354
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'thick plate'
_exptl_crystal_F_000 508
_exptl_crystal_size_max 0.352
_exptl_crystal_size_mid 0.298
_exptl_crystal_size_min 0.103
_refine_diff_density_max 0.303
_refine_diff_density_min -0.162
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.081
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 334
_refine_ls_number_reflns 6318
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.081
_refine_ls_R_factor_all 0.0665
_refine_ls_R_factor_gt 0.0461
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0793P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1319
_refine_ls_wR_factor_ref 0.1397
_reflns_number_gt 4347
_reflns_number_total 6318
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vm2302.cif
_cod_data_source_block I
_cod_database_code 2023130
_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 0.970
_shelx_estimated_absorpt_t_max 0.991
_shelx_hkl_file
;
-1 0 0 1487.85 74.09
-1 0 0 1515.25 74.09
1 0 0 1472.25 74.09
-2 0 0 205.38 10.30
-2 0 0 207.88 10.30
-2 0 0 207.78 10.30
2 0 0 202.98 10.30
-3 0 0 27.00 1.50
-3 0 0 27.10 1.50
-3 0 0 28.40 1.50
3 0 0 26.10 1.30
3 0 0 25.90 1.50
3 0 0 25.40 1.30
-4 0 0 219.58 11.10
-4 0 0 223.88 11.00
-4 0 0 215.08 11.10
4 0 0 217.38 11.00
4 0 0 220.48 10.90
4 0 0 216.28 10.90
-5 0 0 587.94 28.70
-5 0 0 564.74 28.60
-5 0 0 579.64 28.70
5 0 0 578.34 28.70
5 0 0 572.64 28.50
5 0 0 557.54 28.50
-6 0 0 3.00 0.80
-6 0 0 2.00 0.60
6 0 0 2.50 0.70
6 0 0 2.30 0.40
6 0 0 1.80 0.40
6 0 0 1.50 0.70
-7 0 0 59.79 3.50
7 0 0 57.49 3.40
7 0 0 58.69 3.10
-8 0 0 63.39 4.10
8 0 0 76.99 4.10
8 0 0 70.19 3.70
-9 0 0 119.09 6.50
9 0 0 110.49 6.00
9 0 0 125.69 6.50
-10 0 0 4.40 1.80
10 0 0 4.80 0.80
11 0 0 3.30 0.90
11 -1 0 0.70 1.00
10 -1 0 -0.30 0.80
-10 1 0 1.10 1.80
9 -1 0 4.70 0.80
9 -1 0 3.90 1.50
-9 1 0 6.60 1.70
8 -1 0 25.50 2.10
8 -1 0 22.50 1.50
-8 1 0 21.90 2.20
7 -1 0 28.40 2.20
7 -1 0 33.10 1.80
-7 1 0 28.30 2.30
6 -1 0 4.80 0.90
6 -1 0 6.30 0.60
-6 1 0 8.70 1.10
5 -1 0 1.10 0.30
5 -1 0 1.40 0.70
5 -1 0 1.60 0.40
-5 1 0 2.10 0.50
-5 1 0 3.00 0.70
4 -1 0 2.30 0.30
4 -1 0 1.20 0.50
4 -1 0 2.40 0.40
-4 1 0 3.10 0.40
-4 1 0 1.80 0.60
3 -1 0 0.10 0.40
3 -1 0 0.10 0.20
3 -1 0 -0.10 0.20
-3 1 0 0.20 0.30
-3 1 0 0.00 0.10
-3 1 0 0.10 0.40
-3 1 0 0.10 0.10
2 -1 0 258.87 13.90
2 -1 0 274.87 13.90
-2 1 0 280.97 13.90
-2 1 0 280.97 14.00
-2 1 0 289.67 13.90
-2 1 0 286.07 13.90
1 -1 0 142.49 7.10
1 -1 0 139.69 7.20
-1 1 0 144.29 7.20
-1 1 0 144.29 7.10
0 -1 0 130.89 6.50
0 -1 0 130.39 6.60
0 1 0 129.59 6.50
0 1 0 132.69 6.60
-1 -1 0 1228.98 59.89
-1 -1 0 1242.18 59.89
-1 -1 0 1209.08 59.89
1 1 0 1168.48 59.89
1 1 0 1221.88 59.89
1 1 0 1166.68 59.89
-2 -1 0 0.30 0.30
-2 -1 0 0.80 0.30
-2 -1 0 0.80 0.30
-3 -1 0 19.90 1.10
-3 -1 0 19.60 1.10
-3 -1 0 17.00 1.10
-4 -1 0 296.47 14.90
-4 -1 0 296.37 14.90
-4 -1 0 292.87 14.90
4 1 0 298.27 14.90
-5 -1 0 16.40 1.20
-5 -1 0 16.30 1.20
-5 -1 0 17.10 1.30
5 1 0 14.00 1.20
5 1 0 15.20 1.20
-6 -1 0 117.59 6.00
-6 -1 0 114.59 6.00
-6 -1 0 117.39 6.00
6 1 0 117.89 5.70
6 1 0 110.49 6.00
6 1 0 114.19 6.00
6 1 0 110.29 5.70
-7 -1 0 44.50 2.50
-7 -1 0 37.20 2.50
-7 -1 0 42.40 2.50
7 1 0 38.00 2.00
7 1 0 39.40 2.40
7 1 0 37.80 2.00
7 1 0 37.10 2.40
-8 -1 0 18.80 2.00
-8 -1 0 22.30 2.00
8 1 0 21.10 1.30
8 1 0 22.00 2.00
-9 -1 0 1.10 1.40
9 1 0 1.30 1.20
9 1 0 0.60 0.50
10 1 0 -0.10 0.60
10 1 0 0.70 1.60
11 1 0 1.30 0.80
12 1 0 -0.40 0.90
-11 2 0 -0.80 2.40
10 -2 0 42.00 2.80
-10 2 0 42.20 3.70
9 -2 0 79.39 4.40
-9 2 0 80.19 5.00
8 -2 0 10.60 1.70
8 -2 0 7.10 0.90
-8 2 0 8.70 1.60
7 -2 0 9.70 1.00
7 -2 0 11.80 1.50
-7 2 0 12.40 1.50
6 -2 0 -0.20 0.50
6 -2 0 0.60 0.90
-6 2 0 1.10 1.00
5 -2 0 1.20 0.70
5 -2 0 0.90 0.50
-5 2 0 1.60 0.80
4 -2 0 0.30 0.40
4 -2 0 0.10 0.30
4 -2 0 0.00 0.60
-4 2 0 0.40 0.30
-4 2 0 -0.20 0.60
-4 2 0 0.20 0.30
-4 2 0 0.10 0.20
3 -2 0 132.89 6.80
3 -2 0 123.99 6.70
-3 2 0 127.39 6.90
-3 2 0 141.29 6.70
-3 2 0 137.09 6.70
-3 2 0 132.69 6.70
2 -2 0 293.07 15.10
2 -2 0 288.67 15.00
-2 2 0 317.37 15.00
-2 2 0 301.37 15.00
1 -2 0 6691.33 332.27
1 -2 0 6640.04 332.07
1 -2 0 6844.81 332.27
-1 2 0 6643.14 332.27
-1 2 0 6932.21 332.17
-1 2 0 6370.26 332.27
0 -2 0 3930.41 194.78
0 -2 0 3864.31 194.78
0 -2 0 3914.41 194.88
0 2 0 3890.01 194.88
0 2 0 4038.00 194.88
0 2 0 3954.70 194.88
0 2 0 3855.91 194.98
-1 -2 0 584.14 28.60
-1 -2 0 569.94 28.70
-1 -2 0 581.44 28.70
1 2 0 579.64 28.70
1 2 0 548.25 28.60
1 2 0 588.44 28.60
-2 -2 0 177.18 8.90
-2 -2 0 190.98 8.90
-2 -2 0 170.38 9.00
2 2 0 178.98 9.00
2 2 0 178.98 8.90
2 2 0 174.08 8.90
-3 -2 0 949.40 46.80
-3 -2 0 955.60 46.80
-3 -2 0 919.91 46.80
3 2 0 930.61 46.70
3 2 0 926.91 46.70
3 2 0 949.40 46.80
3 2 0 949.31 46.80
-4 -2 0 45.30 2.40
-4 -2 0 44.80 2.50
-4 -2 0 46.60 2.50
4 2 0 43.10 2.50
4 2 0 44.70 2.40
-5 -2 0 63.69 3.50
-5 -2 0 66.59 3.50
-5 -2 0 65.59 3.50
5 2 0 61.69 3.50
-6 -2 0 9.20 1.00
-6 -2 0 6.70 0.90
-6 -2 0 6.60 0.90
6 2 0 5.10 0.90
-7 -2 0 23.80 1.70
-7 -2 0 22.60 1.70
-7 -2 0 22.60 1.70
7 2 0 19.30 1.70
7 2 0 20.40 1.60
-8 -2 0 252.07 12.60
-8 -2 0 241.38 12.60
-8 -2 0 260.27 12.60
8 2 0 234.88 12.60
8 2 0 254.87 12.60
8 2 0 250.77 12.20
8 2 0 227.38 12.30
-9 -2 0 60.49 3.90
9 2 0 62.09 3.30
9 2 0 68.39 3.90
10 2 0 0.50 0.50
10 2 0 2.00 1.50
11 2 0 13.70 2.40
11 2 0 15.30 1.30
12 2 0 0.50 0.90
10 -3 0 18.10 1.70
-10 3 0 13.70 2.40
9 -3 0 5.90 1.20
-9 3 0 5.00 1.80
8 -3 0 8.10 1.90
8 -3 0 7.40 1.00
-8 3 0 7.10 1.60
7 -3 0 25.30 2.20
7 -3 0 23.30 1.70
-7 3 0 23.10 2.30
6 -3 0 0.70 1.00
6 -3 0 0.50 0.60
-6 3 0 2.40 1.10
5 -3 0 37.70 2.70
5 -3 0 45.50 2.40
-5 3 0 44.60 2.30
-5 3 0 45.20 2.70
-5 3 0 42.00 2.30
4 -3 0 27.60 2.00
4 -3 0 33.50 1.90
-4 3 0 29.00 2.10
-4 3 0 33.10 1.80
-4 3 0 33.50 1.80
3 -3 0 485.55 24.60
3 -3 0 489.45 24.70
-3 3 0 501.85 24.80
-3 3 0 513.45 24.50
-3 3 0 490.15 24.60
-3 3 0 473.45 24.60
2 -3 0 154.98 7.80
2 -3 0 155.58 7.80
2 -3 0 159.38 7.90
-2 3 0 148.39 7.90
-2 3 0 156.28 7.70
-2 3 0 149.59 7.80
1 -3 0 860.41 42.70
1 -3 0 826.92 42.70
1 -3 0 848.72 42.80
-1 3 0 871.91 42.70
-1 3 0 878.01 42.70
-1 3 0 858.61 42.80
-1 3 0 861.71 42.70
0 -3 0 545.85 26.60
0 -3 0 519.75 26.60
0 -3 0 521.35 26.60
0 3 0 529.35 26.60
0 3 0 542.55 26.60
0 3 0 540.95 26.60
0 3 0 532.85 26.60
-1 -3 0 430.26 20.60
-1 -3 0 416.96 20.60
1 3 0 404.86 20.60
1 3 0 408.66 20.60
1 3 0 402.66 20.60
-2 -3 0 14.10 1.00
-2 -3 0 15.20 1.00
-2 -3 0 15.10 0.90
2 3 0 15.20 1.00
2 3 0 13.90 1.00
2 3 0 16.90 0.90
-3 -3 0 28.90 1.70
-3 -3 0 28.80 1.50
-3 -3 0 30.20 1.50
-3 -3 0 29.20 1.70
3 3 0 25.40 1.50
3 3 0 31.10 1.50
3 3 0 27.60 1.60
3 3 0 25.10 1.70
-4 -3 0 223.68 11.50
-4 -3 0 235.68 11.60
4 3 0 230.98 11.60
4 3 0 230.98 11.40
4 3 0 224.58 11.50
4 3 0 222.28 11.40
-5 -3 0 10.00 0.90
-5 -3 0 8.10 0.90
-5 -3 0 8.00 0.90
5 3 0 7.20 0.90
5 3 0 7.30 0.50
5 3 0 7.90 0.80
5 3 0 7.40 0.50
-6 -3 0 7.30 1.00
-6 -3 0 8.80 1.00
-6 -3 0 10.50 1.00
6 3 0 7.20 0.50
6 3 0 7.90 1.00
6 3 0 7.50 0.90
6 3 0 7.20 0.50
-7 -3 0 13.80 1.40
-7 -3 0 14.10 1.30
-7 -3 0 13.90 1.40
7 3 0 11.20 0.70
7 3 0 13.10 1.30
7 3 0 11.00 0.70
7 3 0 11.90 1.30
-8 -3 0 -0.10 1.00
-8 -3 0 -0.30 1.00
-8 -3 0 -0.20 1.00
8 3 0 0.30 1.00
8 3 0 -0.50 1.00
8 3 0 0.10 0.30
8 3 0 -0.50 1.20
8 3 0 0.10 0.30
-9 -3 0 -0.30 1.30
-9 -3 0 -0.40 1.30
9 3 0 0.40 1.30
9 3 0 0.40 0.40
9 3 0 -0.70 1.10
-10 -3 0 7.80 1.80
10 3 0 9.00 0.80
10 3 0 7.90 1.80
-11 -3 0 -0.10 1.60
11 3 0 1.60 1.70
11 3 0 0.50 0.60
12 3 0 0.50 0.80
-10 4 0 7.20 2.40
9 -4 0 0.60 1.10
-9 4 0 0.30 1.90
8 -4 0 0.50 0.90
-8 4 0 0.20 1.60
7 -4 0 0.90 1.40
7 -4 0 0.00 0.80
-7 4 0 0.80 1.30
6 -4 0 2.60 0.80
6 -4 0 0.50 1.20
-6 4 0 2.90 0.50
-6 4 0 4.00 1.20
5 -4 0 27.00 1.90
5 -4 0 26.70 2.10
-5 4 0 30.20 2.20
4 -4 0 45.00 2.80
4 -4 0 48.20 2.70
-4 4 0 43.70 2.50
-4 4 0 51.49 2.90
3 -4 0 53.59 3.20
3 -4 0 60.69 3.10
-3 4 0 56.99 3.00
-3 4 0 54.89 3.30
2 -4 0 3.30 0.60
2 -4 0 2.50 0.70
2 -4 0 1.60 0.60
-2 4 0 2.50 0.60
-2 4 0 2.90 0.60
-2 4 0 4.90 0.50
-2 4 0 3.70 0.80
1 -4 0 476.95 24.00
1 -4 0 474.85 24.00
1 -4 0 486.65 24.00
-1 4 0 488.05 24.00
-1 4 0 480.85 23.90
-1 4 0 482.35 24.00
-1 4 0 464.85 24.10
0 -4 0 -0.30 0.40
0 -4 0 0.10 0.30
0 -4 0 0.20 0.40
0 4 0 -0.10 0.40
0 4 0 -0.20 0.50
0 4 0 0.70 0.40
0 4 0 -0.10 0.40
-1 -4 0 203.48 10.70
-1 -4 0 209.68 10.70
-1 -4 0 212.88 10.60
1 4 0 221.78 10.70
1 4 0 210.68 10.70
1 4 0 207.18 10.70
1 4 0 215.38 10.70
-2 -4 0 0.10 0.40
-2 -4 0 0.10 0.30
2 4 0 -0.20 0.30
2 4 0 0.10 0.40
2 4 0 -0.20 0.40
2 4 0 0.40 0.60
-3 -4 0 539.55 26.40
-3 -4 0 527.65 26.30
-3 -4 0 552.64 26.30
-3 -4 0 500.05 26.40
3 4 0 527.95 26.30
3 4 0 538.25 26.40
3 4 0 506.25 26.40
-4 -4 0 10.60 1.00
-4 -4 0 9.90 1.00
4 4 0 8.90 1.00
4 4 0 8.10 0.90
4 4 0 8.40 0.70
4 4 0 9.20 0.70
-5 -4 0 40.10 2.40
-5 -4 0 36.40 2.40
5 4 0 40.40 2.10
5 4 0 36.50 2.20
5 4 0 38.10 2.00
5 4 0 38.40 2.40
-6 -4 0 22.30 1.60
-6 -4 0 19.90 1.70
6 4 0 19.40 1.50
6 4 0 18.60 1.10
6 4 0 17.30 1.60
6 4 0 19.80 1.20
-7 -4 0 232.28 11.30
-7 -4 0 221.38 11.30
7 4 0 217.28 11.20
7 4 0 210.08 11.30
7 4 0 216.08 11.00
-8 -4 0 11.40 1.60
-8 -4 0 12.70 1.60
8 4 0 13.90 1.60
8 4 0 11.60 0.80
-9 -4 0 -1.00 1.30
9 4 0 -0.70 1.10
9 4 0 0.00 0.40
-10 -4 0 1.20 1.60
10 4 0 3.90 1.60
10 4 0 3.50 0.50
-11 -4 0 0.60 1.90
11 4 0 0.50 1.90
11 4 0 0.10 0.60
-12 -4 0 2.50 2.40
12 4 0 0.50 0.80
12 4 0 0.60 2.40
9 -5 0 6.50 1.50
-9 5 0 3.70 2.20
8 -5 0 -0.90 1.00
-8 5 0 0.00 1.80
7 -5 0 4.30 1.00
-7 5 0 4.20 1.50
6 -5 0 5.60 1.00
6 -5 0 6.20 1.50
-6 5 0 5.10 0.70
-6 5 0 4.50 1.50
5 -5 0 0.20 1.20
5 -5 0 0.30 0.70
-5 5 0 0.50 0.60
-5 5 0 1.50 1.10
4 -5 0 8.40 1.00
4 -5 0 7.90 1.30
-4 5 0 8.40 1.30
-4 5 0 8.90 0.90
3 -5 0 54.09 2.80
3 -5 0 47.80 2.90
-3 5 0 44.70 2.70
-3 5 0 46.50 3.00
2 -5 0 320.47 15.70
2 -5 0 300.67 15.70
2 -5 0 309.67 15.60
-2 5 0 295.87 15.80
-2 5 0 322.37 15.50
-2 5 0 304.97 15.60
1 -5 0 935.71 46.20
1 -5 0 918.91 46.20
1 -5 0 972.30 46.20
-1 5 0 901.51 46.20
-1 5 0 910.61 46.30
-1 5 0 911.11 46.20
-1 5 0 931.51 46.10
0 -5 0 1.80 0.60
0 -5 0 1.50 0.60
0 -5 0 2.00 0.60
0 5 0 1.50 0.60
0 5 0 2.40 0.60
0 5 0 1.70 0.70
0 5 0 3.20 0.60
-1 -5 0 11.30 1.00
-1 -5 0 10.90 1.20
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;
TITL JTM1034_0m_a.res in P-1
jtm1034.res
created by SHELXL-2019/1 at 11:25:23 on 01-May-2024
REM Old TITL JTM1034_0m in P-1
REM SHELXT solution in P-1
REM R1 0.146, Rweak 0.004, Alpha 0.024, Orientation as input
REM Formula found by SHELXT: C31 N4 O2
CELL 0.71073 9.0384 9.4484 14.9524 77.267 83.991 72.708
ZERR 2.000 0.0003 0.0004 0.0006 0.001 0.001 0.001
LATT 1
SFAC C H N O
UNIT 62 48 8 4
TEMP 25
SIZE 0.103 0.298 0.352
L.S. 5
BOND $H
LIST 4
FMAP 2
PLAN 5
MPLA C9 > C14
MPLA N1 N2 C1 > C8
MPLA N3 N4 C15 > C22
MPLA C23 > C28
CONF
ACTA 57
htab
WGHT 0.079300
FVAR 0.70383
O1 4 0.396201 0.886738 0.069180 11.00000 0.06469 0.03854 =
0.05021 -0.00475 -0.01958 -0.02161
O2 4 0.214754 0.716196 0.391022 11.00000 0.06848 0.11130 =
0.04077 -0.00018 -0.01425 -0.05178
N1 3 0.446989 0.632905 0.113546 11.00000 0.04085 0.03623 =
0.03048 -0.00642 -0.00332 -0.01351
N2 3 0.214975 0.640956 0.003355 11.00000 0.04722 0.04177 =
0.03436 -0.00681 -0.00236 -0.01987
N3 3 0.439898 0.779809 0.382191 11.00000 0.04412 0.04315 =
0.03036 -0.00423 -0.00465 -0.01219
N4 3 0.423413 0.740890 0.573235 11.00000 0.03991 0.04689 =
0.03500 -0.00601 -0.00461 -0.01211
C1 1 0.289389 0.507868 0.060155 11.00000 0.04691 0.03790 =
0.03172 -0.00810 0.00481 -0.01762
C2 1 0.249512 0.376026 0.058809 11.00000 0.06172 0.04674 =
0.04617 -0.01291 0.00514 -0.02886
AFIX 43
H2 2 0.169960 0.381198 0.022410 11.00000 -1.20000
AFIX 0
C3 1 0.325745 0.239901 0.110176 11.00000 0.07320 0.04074 =
0.05583 -0.01460 0.01549 -0.02741
AFIX 43
H3 2 0.299792 0.152567 0.108083 11.00000 -1.20000
AFIX 0
C4 1 0.442154 0.233830 0.165379 11.00000 0.06753 0.03405 =
0.05493 -0.00375 0.00886 -0.01188
AFIX 43
H4 2 0.493638 0.141281 0.200596 11.00000 -1.20000
AFIX 0
C5 1 0.483930 0.361092 0.169628 11.00000 0.05387 0.03892 =
0.04514 -0.00429 -0.00129 -0.00962
AFIX 43
H5 2 0.561308 0.354575 0.207998 11.00000 -1.20000
AFIX 0
C6 1 0.408761 0.499946 0.115669 11.00000 0.04312 0.03569 =
0.03072 -0.00844 0.00537 -0.01372
C7 1 0.367291 0.770862 0.063126 11.00000 0.04181 0.03618 =
0.02932 -0.00706 -0.00129 -0.01480
C8 1 0.249340 0.764853 0.002425 11.00000 0.03766 0.03884 =
0.02785 -0.00832 0.00081 -0.01478
C9 1 0.167774 0.902210 -0.063287 11.00000 0.03860 0.04148 =
0.02849 -0.00722 0.00007 -0.01303
C10 1 0.202058 1.039964 -0.081652 11.00000 0.05618 0.05098 =
0.04826 0.00325 -0.01600 -0.02738
AFIX 43
H10 2 0.280946 1.051677 -0.051211 11.00000 -1.20000
AFIX 0
C11 1 0.119137 1.159824 -0.145127 11.00000 0.06345 0.04969 =
0.05711 0.00820 -0.01384 -0.02784
AFIX 43
H11 2 0.142651 1.251697 -0.156303 11.00000 -1.20000
AFIX 0
C12 1 0.002919 1.146114 -0.191971 11.00000 0.04688 0.05094 =
0.04270 0.00284 -0.00646 -0.01064
AFIX 43
H12 2 -0.051781 1.227421 -0.234579 11.00000 -1.20000
AFIX 0
C13 1 -0.030837 1.010386 -0.174712 11.00000 0.05784 0.05688 =
0.06094 -0.00422 -0.02579 -0.01659
AFIX 43
H13 2 -0.108010 0.998776 -0.206648 11.00000 -1.20000
AFIX 0
C14 1 0.048595 0.890789 -0.110400 11.00000 0.05841 0.04394 =
0.06022 -0.00521 -0.02192 -0.01758
AFIX 43
H14 2 0.021810 0.800486 -0.098289 11.00000 -1.20000
AFIX 0
C15 1 0.541979 0.789756 0.521691 11.00000 0.03659 0.04047 =
0.03782 -0.00674 -0.00458 -0.00738
C16 1 0.654039 0.817622 0.567740 11.00000 0.04514 0.05715 =
0.04161 -0.00963 -0.00852 -0.01235
AFIX 43
H16 2 0.645671 0.805913 0.631306 11.00000 -1.20000
AFIX 0
C17 1 0.776084 0.862007 0.520211 11.00000 0.04082 0.05644 =
0.06188 -0.01225 -0.01045 -0.01454
AFIX 43
H17 2 0.850311 0.880335 0.551234 11.00000 -1.20000
AFIX 0
C18 1 0.787934 0.879351 0.425454 11.00000 0.04326 0.04879 =
0.06127 -0.00946 0.00350 -0.01538
AFIX 43
H18 2 0.871213 0.908817 0.393312 11.00000 -1.20000
AFIX 0
C19 1 0.679119 0.853891 0.378024 11.00000 0.04900 0.04509 =
0.04282 -0.00673 0.00254 -0.01261
AFIX 43
H19 2 0.688651 0.866859 0.314411 11.00000 -1.20000
AFIX 0
C20 1 0.554020 0.808421 0.425732 11.00000 0.03641 0.03398 =
0.03870 -0.00650 -0.00379 -0.00651
C21 1 0.316367 0.736188 0.430568 11.00000 0.04479 0.05083 =
0.03597 -0.00149 -0.00801 -0.01630
C22 1 0.317969 0.715373 0.531670 11.00000 0.04073 0.03906 =
0.03418 -0.00443 -0.00481 -0.00926
C23 1 0.193745 0.661972 0.589061 11.00000 0.03746 0.03910 =
0.03447 -0.00049 -0.00635 -0.00822
C24 1 0.137894 0.718255 0.668406 11.00000 0.05182 0.04745 =
0.04530 -0.01178 0.00136 -0.01735
AFIX 43
H24 2 0.175355 0.791637 0.683015 11.00000 -1.20000
AFIX 0
C25 1 0.027108 0.665681 0.725566 11.00000 0.06255 0.06298 =
0.04712 -0.01716 0.01446 -0.02180
AFIX 43
H25 2 -0.010397 0.704779 0.778051 11.00000 -1.20000
AFIX 0
C26 1 -0.027993 0.556166 0.705446 11.00000 0.05371 0.05514 =
0.05299 -0.00176 0.00490 -0.02263
AFIX 43
H26 2 -0.102757 0.521512 0.744151 11.00000 -1.20000
AFIX 0
C27 1 0.027272 0.497806 0.628188 11.00000 0.05150 0.04320 =
0.05088 0.00107 -0.01076 -0.01832
AFIX 43
H27 2 -0.008983 0.422527 0.615101 11.00000 -1.20000
AFIX 0
C28 1 0.136901 0.550789 0.569690 11.00000 0.04744 0.04408 =
0.03687 -0.00446 -0.00914 -0.01108
AFIX 43
H28 2 0.172843 0.511759 0.517023 11.00000 -1.20000
AFIX 0
C29 1 0.582577 0.629655 0.161490 11.00000 0.03938 0.04342 =
0.03821 -0.00689 -0.00603 -0.01258
AFIX 23
H29A 2 0.619669 0.715413 0.131354 11.00000 -1.20000
H29B 2 0.664531 0.538571 0.155101 11.00000 -1.20000
AFIX 0
C30 1 0.553170 0.633869 0.262710 11.00000 0.05163 0.04048 =
0.03375 -0.00195 -0.01168 -0.01179
AFIX 23
H30A 2 0.652121 0.610476 0.290478 11.00000 -1.20000
H30B 2 0.504683 0.555402 0.291637 11.00000 -1.20000
AFIX 0
C31 1 0.451418 0.784051 0.282793 11.00000 0.05010 0.04290 =
0.03029 -0.00207 -0.00571 -0.01188
AFIX 23
H31A 2 0.495241 0.864656 0.251294 11.00000 -1.20000
H31B 2 0.348760 0.804628 0.260318 11.00000 -1.20000
AFIX 0
HKLF 4
REM JTM1034_0m_a.res in P-1
REM wR2 = 0.1397, GooF = S = 1.081, Restrained GooF = 1.081 for all data
REM R1 = 0.0461 for 4347 Fo > 4sig(Fo) and 0.0665 for all 6318 data
REM 334 parameters refined using 0 restraints
END
WGHT 0.0793 0.0000
REM No hydrogen bonds found for HTAB generation
REM Highest difference peak 0.303, deepest hole -0.162, 1-sigma level 0.041
Q1 1 0.3190 0.7661 0.0255 11.00000 0.05 0.30
Q2 1 0.5421 0.8182 0.4721 11.00000 0.05 0.26
Q3 1 0.3720 0.4984 0.0739 11.00000 0.05 0.26
Q4 1 0.2613 0.6851 0.5601 11.00000 0.05 0.23
Q5 1 0.1026 0.9050 -0.0735 11.00000 0.05 0.23
;
_shelx_res_checksum 3119
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.39620(10) 0.88674(9) 0.06918(6) 0.0490(2) Uani d 1 . .
O O2 0.21475(12) 0.71620(14) 0.39102(6) 0.0692(3) Uani d 1 . .
N N1 0.44699(10) 0.63291(10) 0.11355(6) 0.0352(2) Uani d 1 . .
N N2 0.21498(11) 0.64096(11) 0.00336(6) 0.0396(2) Uani d 1 . .
N N3 0.43990(11) 0.77981(11) 0.38219(6) 0.0395(2) Uani d 1 . .
N N4 0.42341(11) 0.74089(11) 0.57324(7) 0.0408(2) Uani d 1 . .
C C1 0.28939(13) 0.50787(13) 0.06015(8) 0.0379(3) Uani d 1 . .
C C2 0.24951(16) 0.37603(15) 0.05881(9) 0.0485(3) Uani d 1 . .
H H2 0.169960 0.381198 0.022410 0.058 Uiso calc 1 . .
C C3 0.32574(17) 0.23990(15) 0.11018(10) 0.0546(4) Uani d 1 . .
H H3 0.299792 0.152567 0.108083 0.066 Uiso calc 1 . .
C C4 0.44215(17) 0.23383(15) 0.16538(10) 0.0544(3) Uani d 1 . .
H H4 0.493638 0.141281 0.200596 0.065 Uiso calc 1 . .
C C5 0.48393(15) 0.36109(14) 0.16963(9) 0.0475(3) Uani d 1 . .
H H5 0.561308 0.354575 0.207998 0.057 Uiso calc 1 . .
C C6 0.40876(13) 0.49995(12) 0.11567(7) 0.0362(3) Uani d 1 . .
C C7 0.36729(13) 0.77086(13) 0.06313(7) 0.0349(2) Uani d 1 . .
C C8 0.24934(12) 0.76485(13) 0.00243(7) 0.0338(2) Uani d 1 . .
C C9 0.16777(12) 0.90221(13) -0.06329(7) 0.0359(3) Uani d 1 . .
C C10 0.20206(15) 1.03996(15) -0.08165(9) 0.0502(3) Uani d 1 . .
H H10 0.280946 1.051677 -0.051211 0.060 Uiso calc 1 . .
C C11 0.11914(16) 1.15982(16) -0.14513(10) 0.0563(4) Uani d 1 . .
H H11 0.142651 1.251697 -0.156303 0.068 Uiso calc 1 . .
C C12 0.00292(14) 1.14611(16) -0.19197(9) 0.0492(3) Uani d 1 . .
H H12 -0.051781 1.227421 -0.234579 0.059 Uiso calc 1 . .
C C13 -0.03084(16) 1.01039(16) -0.17471(10) 0.0579(4) Uani d 1 . .
H H13 -0.108010 0.998776 -0.206648 0.070 Uiso calc 1 . .
C C14 0.04859(16) 0.89079(15) -0.11040(10) 0.0529(3) Uani d 1 . .
H H14 0.021810 0.800486 -0.098289 0.063 Uiso calc 1 . .
C C15 0.54198(13) 0.78976(13) 0.52169(8) 0.0390(3) Uani d 1 . .
C C16 0.65404(14) 0.81762(15) 0.56774(9) 0.0480(3) Uani d 1 . .
H H16 0.645671 0.805913 0.631306 0.058 Uiso calc 1 . .
C C17 0.77608(14) 0.86201(16) 0.52021(10) 0.0522(3) Uani d 1 . .
H H17 0.850311 0.880335 0.551234 0.063 Uiso calc 1 . .
C C18 0.78793(15) 0.87935(15) 0.42545(10) 0.0513(3) Uani d 1 . .
H H18 0.871213 0.908817 0.393312 0.062 Uiso calc 1 . .
C C19 0.67912(14) 0.85389(14) 0.37802(9) 0.0465(3) Uani d 1 . .
H H19 0.688651 0.866859 0.314411 0.056 Uiso calc 1 . .
C C20 0.55402(13) 0.80842(12) 0.42573(8) 0.0371(3) Uani d 1 . .
C C21 0.31637(14) 0.73619(15) 0.43057(8) 0.0439(3) Uani d 1 . .
C C22 0.31797(13) 0.71537(13) 0.53167(8) 0.0387(3) Uani d 1 . .
C C23 0.19375(13) 0.66197(13) 0.58906(8) 0.0383(3) Uani d 1 . .
C C24 0.13789(15) 0.71825(15) 0.66841(9) 0.0473(3) Uani d 1 . .
H H24 0.175355 0.791637 0.683015 0.057 Uiso calc 1 . .
C C25 0.02711(16) 0.66568(17) 0.72557(10) 0.0569(4) Uani d 1 . .
H H25 -0.010397 0.704779 0.778051 0.068 Uiso calc 1 . .
C C26 -0.02799(16) 0.55617(16) 0.70545(10) 0.0543(3) Uani d 1 . .
H H26 -0.102757 0.521512 0.744151 0.065 Uiso calc 1 . .
C C27 0.02727(15) 0.49781(14) 0.62819(9) 0.0485(3) Uani d 1 . .
H H27 -0.008983 0.422527 0.615101 0.058 Uiso calc 1 . .
C C28 0.13690(14) 0.55079(14) 0.56969(8) 0.0432(3) Uani d 1 . .
H H28 0.172843 0.511759 0.517023 0.052 Uiso calc 1 . .
C C29 0.58258(13) 0.62965(14) 0.16149(8) 0.0400(3) Uani d 1 . .
H H29A 0.619669 0.715413 0.131354 0.048 Uiso calc 1 . .
H H29B 0.664531 0.538571 0.155101 0.048 Uiso calc 1 . .
C C30 0.55317(14) 0.63387(13) 0.26271(8) 0.0424(3) Uani d 1 . .
H H30A 0.652121 0.610476 0.290478 0.051 Uiso calc 1 . .
H H30B 0.504683 0.555402 0.291637 0.051 Uiso calc 1 . .
C C31 0.45142(14) 0.78405(14) 0.28279(8) 0.0419(3) Uani d 1 . .
H H31A 0.495241 0.864656 0.251294 0.050 Uiso calc 1 . .
H H31B 0.348760 0.804628 0.260318 0.050 Uiso calc 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 0.0647(6) 0.0385(5) 0.0502(5) -0.0216(4) -0.0196(4) -0.0048(4)
O2 0.0685(6) 0.1113(9) 0.0408(5) -0.0518(6) -0.0143(4) -0.0002(5)
N1 0.0409(5) 0.0362(5) 0.0305(5) -0.0135(4) -0.0033(4) -0.0064(4)
N2 0.0472(6) 0.0418(6) 0.0344(5) -0.0199(4) -0.0024(4) -0.0068(4)
N3 0.0441(5) 0.0432(6) 0.0304(5) -0.0122(4) -0.0047(4) -0.0042(4)
N4 0.0399(5) 0.0469(6) 0.0350(5) -0.0121(4) -0.0046(4) -0.0060(4)
C1 0.0469(6) 0.0379(6) 0.0317(6) -0.0176(5) 0.0048(5) -0.0081(5)
C2 0.0617(8) 0.0467(7) 0.0462(7) -0.0289(6) 0.0051(6) -0.0129(6)
C3 0.0732(9) 0.0407(7) 0.0558(8) -0.0274(7) 0.0155(7) -0.0146(6)
C4 0.0675(9) 0.0340(7) 0.0549(9) -0.0119(6) 0.0089(7) -0.0037(6)
C5 0.0539(7) 0.0389(7) 0.0451(7) -0.0096(6) -0.0013(6) -0.0043(6)
C6 0.0431(6) 0.0357(6) 0.0307(6) -0.0137(5) 0.0054(4) -0.0084(5)
C7 0.0418(6) 0.0362(6) 0.0293(6) -0.0148(5) -0.0013(4) -0.0071(4)
C8 0.0377(6) 0.0388(6) 0.0278(5) -0.0148(5) 0.0008(4) -0.0083(5)
C9 0.0386(6) 0.0415(6) 0.0285(6) -0.0130(5) 0.0001(4) -0.0072(5)
C10 0.0562(8) 0.0510(8) 0.0483(7) -0.0274(6) -0.0160(6) 0.0032(6)
C11 0.0634(9) 0.0497(8) 0.0571(9) -0.0278(7) -0.0138(7) 0.0082(6)
C12 0.0469(7) 0.0509(8) 0.0427(7) -0.0106(6) -0.0065(5) 0.0028(6)
C13 0.0578(8) 0.0569(9) 0.0609(9) -0.0166(7) -0.0258(7) -0.0042(7)
C14 0.0584(8) 0.0439(7) 0.0602(9) -0.0176(6) -0.0219(7) -0.0052(6)
C15 0.0366(6) 0.0405(6) 0.0378(6) -0.0074(5) -0.0046(5) -0.0067(5)
C16 0.0451(7) 0.0571(8) 0.0416(7) -0.0124(6) -0.0085(5) -0.0096(6)
C17 0.0408(7) 0.0564(8) 0.0619(9) -0.0145(6) -0.0105(6) -0.0122(7)
C18 0.0433(7) 0.0488(8) 0.0613(9) -0.0154(6) 0.0035(6) -0.0095(6)
C19 0.0490(7) 0.0451(7) 0.0428(7) -0.0126(6) 0.0025(5) -0.0067(6)
C20 0.0364(6) 0.0340(6) 0.0387(6) -0.0065(5) -0.0038(5) -0.0065(5)
C21 0.0448(7) 0.0508(7) 0.0360(6) -0.0163(6) -0.0080(5) -0.0015(5)
C22 0.0407(6) 0.0391(6) 0.0342(6) -0.0093(5) -0.0048(5) -0.0044(5)
C23 0.0375(6) 0.0391(6) 0.0345(6) -0.0082(5) -0.0063(4) -0.0005(5)
C24 0.0518(7) 0.0475(7) 0.0453(7) -0.0173(6) 0.0014(5) -0.0118(6)
C25 0.0626(9) 0.0630(9) 0.0471(8) -0.0218(7) 0.0145(6) -0.0172(7)
C26 0.0537(8) 0.0551(8) 0.0530(8) -0.0226(6) 0.0049(6) -0.0018(7)
C27 0.0515(7) 0.0432(7) 0.0509(8) -0.0183(6) -0.0108(6) 0.0011(6)
C28 0.0474(7) 0.0441(7) 0.0369(6) -0.0111(5) -0.0091(5) -0.0045(5)
C29 0.0394(6) 0.0434(7) 0.0382(6) -0.0126(5) -0.0060(5) -0.0069(5)
C30 0.0516(7) 0.0405(7) 0.0337(6) -0.0118(5) -0.0117(5) -0.0019(5)
C31 0.0501(7) 0.0429(7) 0.0303(6) -0.0119(5) -0.0057(5) -0.0021(5)
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
C7 N1 C6 . . 122.56(9) ?
C7 N1 C29 . . 116.94(9) ?
C6 N1 C29 . . 120.40(9) ?
C8 N2 C1 . . 120.56(10) ?
C21 N3 C20 . . 122.01(10) ?
C21 N3 C31 . . 116.59(9) ?
C20 N3 C31 . . 121.26(10) ?
C22 N4 C15 . . 119.21(10) ?
N2 C1 C2 . . 118.84(11) ?
N2 C1 C6 . . 121.69(10) ?
C2 C1 C6 . . 119.39(11) ?
C3 C2 C1 . . 120.99(13) ?
C3 C2 H2 . . 119.5 ?
C1 C2 H2 . . 119.5 ?
C2 C3 C4 . . 119.07(12) ?
C2 C3 H3 . . 120.5 ?
C4 C3 H3 . . 120.5 ?
C5 C4 C3 . . 121.87(13) ?
C5 C4 H4 . . 119.1 ?
C3 C4 H4 . . 119.1 ?
C4 C5 C6 . . 119.28(13) ?
C4 C5 H5 . . 120.4 ?
C6 C5 H5 . . 120.4 ?
N1 C6 C5 . . 123.06(11) ?
N1 C6 C1 . . 117.58(10) ?
C5 C6 C1 . . 119.37(11) ?
O1 C7 N1 . . 120.38(10) ?
O1 C7 C8 . . 124.38(10) ?
N1 C7 C8 . . 115.24(9) ?
N2 C8 C9 . . 117.15(9) ?
N2 C8 C7 . . 122.00(10) ?
C9 C8 C7 . . 120.84(9) ?
C14 C9 C10 . . 117.63(11) ?
C14 C9 C8 . . 117.09(11) ?
C10 C9 C8 . . 125.28(10) ?
C11 C10 C9 . . 120.18(11) ?
C11 C10 H10 . . 119.9 ?
C9 C10 H10 . . 119.9 ?
C12 C11 C10 . . 121.47(12) ?
C12 C11 H11 . . 119.3 ?
C10 C11 H11 . . 119.3 ?
C13 C12 C11 . . 118.69(12) ?
C13 C12 H12 . . 120.7 ?
C11 C12 H12 . . 120.7 ?
C12 C13 C14 . . 120.56(12) ?
C12 C13 H13 . . 119.7 ?
C14 C13 H13 . . 119.7 ?
C13 C14 C9 . . 121.44(12) ?
C13 C14 H14 . . 119.3 ?
C9 C14 H14 . . 119.3 ?
N4 C15 C16 . . 118.36(11) ?
N4 C15 C20 . . 121.96(10) ?
C16 C15 C20 . . 119.66(11) ?
C17 C16 C15 . . 120.69(12) ?
C17 C16 H16 . . 119.7 ?
C15 C16 H16 . . 119.7 ?
C16 C17 C18 . . 119.41(12) ?
C16 C17 H17 . . 120.3 ?
C18 C17 H17 . . 120.3 ?
C19 C18 C17 . . 121.36(12) ?
C19 C18 H18 . . 119.3 ?
C17 C18 H18 . . 119.3 ?
C18 C19 C20 . . 119.80(12) ?
C18 C19 H19 . . 120.1 ?
C20 C19 H19 . . 120.1 ?
N3 C20 C19 . . 122.91(11) ?
N3 C20 C15 . . 118.01(10) ?
C19 C20 C15 . . 119.08(11) ?
O2 C21 N3 . . 121.12(11) ?
O2 C21 C22 . . 123.53(11) ?
N3 C21 C22 . . 115.35(10) ?
N4 C22 C23 . . 117.70(10) ?
N4 C22 C21 . . 123.37(11) ?
C23 C22 C21 . . 118.92(10) ?
C28 C23 C24 . . 118.47(11) ?
C28 C23 C22 . . 122.47(11) ?
C24 C23 C22 . . 118.95(10) ?
C25 C24 C23 . . 120.36(12) ?
C25 C24 H24 . . 119.8 ?
C23 C24 H24 . . 119.8 ?
C26 C25 C24 . . 120.48(13) ?
C26 C25 H25 . . 119.8 ?
C24 C25 H25 . . 119.8 ?
C25 C26 C27 . . 119.99(12) ?
C25 C26 H26 . . 120.0 ?
C27 C26 H26 . . 120.0 ?
C26 C27 C28 . . 120.14(12) ?
C26 C27 H27 . . 119.9 ?
C28 C27 H27 . . 119.9 ?
C27 C28 C23 . . 120.55(12) ?
C27 C28 H28 . . 119.7 ?
C23 C28 H28 . . 119.7 ?
N1 C29 C30 . . 115.05(9) ?
N1 C29 H29A . . 108.5 ?
C30 C29 H29A . . 108.5 ?
N1 C29 H29B . . 108.5 ?
C30 C29 H29B . . 108.5 ?
H29A C29 H29B . . 107.5 ?
C29 C30 C31 . . 114.50(10) ?
C29 C30 H30A . . 108.6 ?
C31 C30 H30A . . 108.6 ?
C29 C30 H30B . . 108.6 ?
C31 C30 H30B . . 108.6 ?
H30A C30 H30B . . 107.6 ?
N3 C31 C30 . . 110.11(9) ?
N3 C31 H31A . . 109.6 ?
C30 C31 H31A . . 109.6 ?
N3 C31 H31B . . 109.6 ?
C30 C31 H31B . . 109.6 ?
H31A C31 H31B . . 108.2 ?
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 C7 . 1.2222(13) ?
O2 C21 . 1.2227(13) ?
N1 C7 . 1.3815(14) ?
N1 C6 . 1.3917(13) ?
N1 C29 . 1.4726(13) ?
N2 C8 . 1.2943(14) ?
N2 C1 . 1.3787(15) ?
N3 C21 . 1.3830(15) ?
N3 C20 . 1.3946(14) ?
N3 C31 . 1.4714(14) ?
N4 C22 . 1.2959(14) ?
N4 C15 . 1.3856(15) ?
C1 C2 . 1.4006(15) ?
C1 C6 . 1.4039(16) ?
C2 C3 . 1.367(2) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.384(2) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.3788(18) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.3971(17) ?
C5 H5 . 0.9300 ?
C7 C8 . 1.4916(14) ?
C8 C9 . 1.4879(16) ?
C9 C14 . 1.3891(16) ?
C9 C10 . 1.3892(16) ?
C10 C11 . 1.3840(18) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.3732(17) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.3691(19) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.3785(18) ?
C13 H13 . 0.9300 ?
C14 H14 . 0.9300 ?
C15 C16 . 1.3978(15) ?
C15 C20 . 1.4031(16) ?
C16 C17 . 1.3701(18) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.3864(19) ?
C17 H17 . 0.9300 ?
C18 C19 . 1.3748(17) ?
C18 H18 . 0.9300 ?
C19 C20 . 1.3988(16) ?
C19 H19 . 0.9300 ?
C21 C22 . 1.4819(16) ?
C22 C23 . 1.4818(16) ?
C23 C28 . 1.3920(16) ?
C23 C24 . 1.3922(17) ?
C24 C25 . 1.3818(17) ?
C24 H24 . 0.9300 ?
C25 C26 . 1.3727(19) ?
C25 H25 . 0.9300 ?
C26 C27 . 1.373(2) ?
C26 H26 . 0.9300 ?
C27 C28 . 1.3849(17) ?
C27 H27 . 0.9300 ?
C28 H28 . 0.9300 ?
C29 C30 . 1.5162(16) ?
C29 H29A . 0.9700 ?
C29 H29B . 0.9700 ?
C30 C31 . 1.5178(17) ?
C30 H30A . 0.9700 ?
C30 H30B . 0.9700 ?
C31 H31A . 0.9700 ?
C31 H31B . 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
C3 H3 O1 1_545 0.93 2.58 3.3871(16) 146 yes
C10 H10 O1 . 0.93 2.22 2.8531(16) 124 y
C27 H27 O2 2_566 0.93 2.59 3.4603(18) 155 yes
C30 H30A Cg6 2_666 0.97 2.75 3.6013(14) 147 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
C8 N2 C1 C2 . . . . -179.66(10) ?
C8 N2 C1 C6 . . . . -2.80(17) ?
N2 C1 C2 C3 . . . . 176.47(11) ?
C6 C1 C2 C3 . . . . -0.46(18) ?
C1 C2 C3 C4 . . . . 1.1(2) ?
C2 C3 C4 C5 . . . . -0.4(2) ?
C3 C4 C5 C6 . . . . -1.1(2) ?
C7 N1 C6 C5 . . . . -177.01(10) ?
C29 N1 C6 C5 . . . . 6.80(16) ?
C7 N1 C6 C1 . . . . 3.35(15) ?
C29 N1 C6 C1 . . . . -172.84(10) ?
C4 C5 C6 N1 . . . . -177.90(10) ?
C4 C5 C6 C1 . . . . 1.74(18) ?
N2 C1 C6 N1 . . . . 1.83(16) ?
C2 C1 C6 N1 . . . . 178.67(10) ?
N2 C1 C6 C5 . . . . -177.83(10) ?
C2 C1 C6 C5 . . . . -0.99(17) ?
C6 N1 C7 O1 . . . . 173.86(10) ?
C29 N1 C7 O1 . . . . -9.82(16) ?
C6 N1 C7 C8 . . . . -6.86(15) ?
C29 N1 C7 C8 . . . . 169.45(9) ?
C1 N2 C8 C9 . . . . 177.83(9) ?
C1 N2 C8 C7 . . . . -1.19(16) ?
O1 C7 C8 N2 . . . . -174.88(11) ?
N1 C7 C8 N2 . . . . 5.88(16) ?
O1 C7 C8 C9 . . . . 6.14(17) ?
N1 C7 C8 C9 . . . . -173.10(9) ?
N2 C8 C9 C14 . . . . 7.41(16) ?
C7 C8 C9 C14 . . . . -173.56(11) ?
N2 C8 C9 C10 . . . . -172.08(11) ?
C7 C8 C9 C10 . . . . 6.96(18) ?
C14 C9 C10 C11 . . . . -0.2(2) ?
C8 C9 C10 C11 . . . . 179.29(12) ?
C9 C10 C11 C12 . . . . -0.6(2) ?
C10 C11 C12 C13 . . . . 0.2(2) ?
C11 C12 C13 C14 . . . . 1.1(2) ?
C12 C13 C14 C9 . . . . -2.0(2) ?
C10 C9 C14 C13 . . . . 1.5(2) ?
C8 C9 C14 C13 . . . . -178.05(13) ?
C22 N4 C15 C16 . . . . 179.59(11) ?
C22 N4 C15 C20 . . . . -1.86(17) ?
N4 C15 C16 C17 . . . . 178.15(12) ?
C20 C15 C16 C17 . . . . -0.43(19) ?
C15 C16 C17 C18 . . . . 0.0(2) ?
C16 C17 C18 C19 . . . . 0.4(2) ?
C17 C18 C19 C20 . . . . -0.5(2) ?
C21 N3 C20 C19 . . . . -179.43(11) ?
C31 N3 C20 C19 . . . . 5.04(17) ?
C21 N3 C20 C15 . . . . 0.85(17) ?
C31 N3 C20 C15 . . . . -174.67(10) ?
C18 C19 C20 N3 . . . . -179.64(11) ?
C18 C19 C20 C15 . . . . 0.07(18) ?
N4 C15 C20 N3 . . . . 1.57(17) ?
C16 C15 C20 N3 . . . . -179.89(11) ?
N4 C15 C20 C19 . . . . -178.15(10) ?
C16 C15 C20 C19 . . . . 0.38(18) ?
C20 N3 C21 O2 . . . . 177.67(12) ?
C31 N3 C21 O2 . . . . -6.61(18) ?
C20 N3 C21 C22 . . . . -2.68(17) ?
C31 N3 C21 C22 . . . . 173.04(10) ?
C15 N4 C22 C23 . . . . 179.48(10) ?
C15 N4 C22 C21 . . . . -0.21(18) ?
O2 C21 C22 N4 . . . . -177.92(12) ?
N3 C21 C22 N4 . . . . 2.43(18) ?
O2 C21 C22 C23 . . . . 2.39(19) ?
N3 C21 C22 C23 . . . . -177.26(10) ?
N4 C22 C23 C28 . . . . -139.78(12) ?
C21 C22 C23 C28 . . . . 39.93(16) ?
N4 C22 C23 C24 . . . . 36.31(16) ?
C21 C22 C23 C24 . . . . -143.98(12) ?
C28 C23 C24 C25 . . . . -0.83(19) ?
C22 C23 C24 C25 . . . . -177.07(11) ?
C23 C24 C25 C26 . . . . 0.7(2) ?
C24 C25 C26 C27 . . . . 0.2(2) ?
C25 C26 C27 C28 . . . . -1.0(2) ?
C26 C27 C28 C23 . . . . 0.87(19) ?
C24 C23 C28 C27 . . . . 0.03(17) ?
C22 C23 C28 C27 . . . . 176.13(11) ?
C7 N1 C29 C30 . . . . 99.27(12) ?
C6 N1 C29 C30 . . . . -84.34(12) ?
N1 C29 C30 C31 . . . . -69.98(13) ?
C21 N3 C31 C30 . . . . -92.34(13) ?
C20 N3 C31 C30 . . . . 83.41(13) ?
C29 C30 C31 N3 . . . . -175.74(9) ?