#------------------------------------------------------------------------------
#$Date: 2026-09-04 22:11:37 +0100 (Fri, 04 Sep 2026) $
#$Revision: 306865 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/35/2023562.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_2023562
loop_
_publ_author_name
'Murillo, Maria Isabel'
'Cuen\'u-Ibarg\"uen, Yahaira'
'Le Lagadec, Ronan'
'Cuen\'u-Cabezas, Fernando'
'G\'omez Casta\~no, Jovanny Arles'
_publ_section_title
;
Conformation and supramolecular assembly in an azo--azomethine--pyrazole
hybrid: crystal structure, Hirshfeld surface and QTAIM analyses
;
_journal_coeditor_code ZO3074
_journal_issue 10
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi 10.1107/S2053229626008533
_journal_volume 82
_journal_year 2026
_chemical_formula_iupac 'C27 H26 N6 O3'
_chemical_formula_moiety 'C27 H26 N6 O3'
_chemical_formula_sum 'C27 H26 N6 O3'
_chemical_formula_weight 482.54
_chemical_name_systematic
2-({[3-tert-Butyl-1-(4-nitrophenyl)-1H-pyrazol-5-yl]imino}methyl)-4-[(4-methylphenyl)diazenyl]phenol
_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
_audit_creation_method SHELXL-2014/7
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 13.2445(11)
_cell_length_b 16.5273(17)
_cell_length_c 22.826(3)
_cell_measurement_reflns_used 5510
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 25.73
_cell_measurement_theta_min 2.16
_cell_volume 4996.5(9)
_computing_cell_refinement
;
APEX2 (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
XP (Bruker, 1998)
;
_computing_publication_material
;
CIFTAB (Sheldrick, 2013)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2012 (Bruker, 2013)
;
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Bruker SMART APEX CCD'
_diffrn_measurement_method \w-scans
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0967
_diffrn_reflns_av_unetI/netI 0.1025
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 31
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_number 38434
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.126
_diffrn_reflns_theta_min 1.970
_diffrn_source 'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu 0.087
_exptl_absorpt_correction_T_max 0.9891
_exptl_absorpt_correction_T_min 0.9711
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.283
_exptl_crystal_description prism
_exptl_crystal_F_000 2032
_exptl_crystal_size_max 0.350
_exptl_crystal_size_mid 0.195
_exptl_crystal_size_min 0.158
_refine_diff_density_max 0.202
_refine_diff_density_min -0.257
_refine_ls_abs_structure_details 'Not determined.'
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.015
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 663
_refine_ls_number_reflns 13380
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.015
_refine_ls_R_factor_all 0.1378
_refine_ls_R_factor_gt 0.0629
_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^)+(0.0419P)^2^+0.2881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1102
_refine_ls_wR_factor_ref 0.1458
_reflns_number_gt 7186
_reflns_number_total 13380
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zo3074sup1.cif
_cod_data_source_block I
_cod_original_cell_volume 4996.4(9)
_cod_database_code 2023562
_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 0.986
_shelx_hkl_file
;
-1 0 0 0.00 0.10
-2 0 0 0.50 0.20
-3 0 0 -0.30 0.30
-4 0 0 9999.00 208.68
-5 0 0 -0.30 0.40
-6 0 0 74.49 3.20
-7 0 0 -0.20 0.50
-8 0 0 851.31 20.80
-9 0 0 -0.10 0.60
-10 0 0 69.79 4.00
-11 0 0 -0.50 0.70
-11 0 0 0.50 0.70
-12 0 0 111.09 5.50
-12 0 0 115.39 5.70
-13 0 0 0.60 0.90
-13 0 0 -0.60 0.50
-14 0 0 39.70 3.50
-14 0 0 43.30 3.60
-15 0 0 -0.90 1.00
-15 0 0 1.00 1.00
-16 0 0 2.00 1.20
-17 0 0 -1.90 0.60
-18 0 0 6.90 2.00
0 -1 0 0.00 0.10
0 1 0 0.00 0.10
0 1 0 0.00 0.10
-1 -1 0 435.66 8.80
-1 -1 0 365.76 8.60
2 1 0 666.33 14.60
-2 -1 0 679.13 14.60
-2 -1 0 673.53 14.60
-2 1 0 668.63 14.90
-3 1 0 168.18 4.70
3 1 0 165.28 4.30
-6 1 0 5.70 1.10
-7 -1 0 3.30 1.00
-7 1 0 3.60 1.10
-8 1 0 94.69 4.30
-8 -1 0 88.89 4.00
-9 1 0 47.40 3.10
-9 -1 0 42.20 2.80
-10 -1 0 3.50 1.20
-10 1 0 3.60 1.30
-10 1 0 1.10 0.60
-11 1 0 -0.20 0.70
-11 -1 0 -0.20 0.70
-11 1 0 0.50 0.80
-11 -1 0 0.00 0.60
-12 1 0 31.70 3.00
-12 -1 0 30.20 2.70
-12 1 0 23.20 2.60
-12 -1 0 29.40 2.80
-13 1 0 0.30 0.90
-13 -1 0 2.60 1.10
-13 -1 0 -0.50 0.80
-13 1 0 0.00 0.80
-14 1 0 0.70 0.90
-14 -1 0 -0.60 0.90
-14 1 0 1.70 1.10
-14 -1 0 0.80 0.90
-15 1 0 0.50 1.10
-15 -1 0 2.00 1.20
-15 1 0 1.80 1.20
-16 1 0 4.60 1.70
-16 -1 0 4.60 1.50
-17 1 0 -0.40 1.00
-17 -1 0 1.60 0.90
-18 1 0 1.60 1.10
0 2 0 9.60 0.50
0 -2 0 10.70 0.70
0 2 0 9.70 0.60
1 2 0 73.79 2.30
-1 2 0 73.79 2.20
-1 -2 0 73.69 2.50
1 2 0 74.79 1.80
2 2 0 13.00 0.90
-2 -2 0 14.20 0.70
-2 2 0 12.00 0.90
-3 -2 0 931.01 20.40
-3 2 0 964.80 21.10
3 2 0 923.01 20.70
-4 -2 0 41.60 1.80
-4 2 0 42.20 2.10
4 2 0 40.70 1.80
-5 2 0 1.80 0.70
-5 -2 0 2.10 0.60
5 2 0 1.40 0.50
-6 -2 0 43.50 2.20
-6 2 0 40.50 2.50
-7 2 0 20.70 1.90
-9 2 0 17.90 2.00
-10 2 0 20.80 2.00
-10 2 0 24.10 2.40
-11 -2 0 10.10 1.80
-11 2 0 9.40 1.90
-11 -2 0 4.10 1.20
-11 2 0 6.00 1.50
-12 -2 0 5.00 1.40
-12 2 0 7.60 1.90
-12 -2 0 8.10 1.90
-12 2 0 7.60 1.70
-13 2 0 0.30 1.00
-13 2 0 0.10 0.70
-13 -2 0 1.20 1.00
-13 -2 0 -1.00 0.50
-14 2 0 1.00 1.20
-14 2 0 5.80 1.70
-14 -2 0 4.20 1.60
-14 -2 0 3.20 1.30
-15 -2 0 2.60 1.30
-15 2 0 3.80 1.70
-15 2 0 2.40 1.40
-16 2 0 -0.30 1.10
-16 2 0 0.00 1.00
-16 -2 0 2.40 1.10
-17 2 0 2.70 1.40
-18 2 0 -0.20 1.00
0 3 0 -0.30 0.20
0 3 0 -0.10 0.20
-1 3 0 32.70 1.50
1 3 0 32.90 1.10
1 3 0 33.70 1.60
-1 3 0 31.70 1.40
2 3 0 134.19 4.00
-2 3 0 138.69 4.00
-3 3 0 13.80 1.20
3 3 0 15.90 1.10
-3 -3 0 15.60 0.90
-4 3 0 69.49 2.90
4 3 0 65.19 2.60
-4 -3 0 67.59 2.30
-5 -3 0 2.20 0.60
-5 3 0 2.50 0.80
5 3 0 2.20 0.60
-6 3 0 32.10 2.20
-6 -3 0 31.40 1.80
6 3 0 29.30 1.80
-7 -3 0 0.30 0.50
-7 3 0 -0.40 0.60
-8 3 0 2.60 0.90
-8 -3 0 3.80 0.90
-9 3 0 1.70 1.00
-9 -3 0 6.40 1.30
-10 3 0 2.70 0.90
-10 -3 0 3.20 1.00
-10 3 0 3.60 1.30
-11 -3 0 12.10 2.00
-11 3 0 9.00 2.00
-11 3 0 11.30 2.00
-11 -3 0 11.50 2.00
-12 3 0 1.30 0.90
-12 -3 0 0.40 0.70
-12 -3 0 0.90 0.80
-12 3 0 0.80 0.80
-13 -3 0 -0.60 0.70
-13 3 0 -1.50 0.60
-13 -3 0 -0.40 0.50
-13 3 0 0.50 0.80
-14 -3 0 0.50 0.60
-14 3 0 4.30 1.50
-14 3 0 2.80 1.20
-15 3 0 -0.90 0.80
-15 3 0 0.20 1.00
-15 -3 0 -0.10 0.70
-16 3 0 2.70 1.20
-16 3 0 -1.00 1.20
-17 3 0 0.30 1.00
-17 3 0 -1.70 1.30
0 4 0 271.67 7.10
0 4 0 271.77 6.50
-1 4 0 29.30 1.60
1 4 0 29.00 1.20
1 4 0 32.50 1.70
-1 4 0 32.00 1.50
2 4 0 107.29 3.70
2 4 0 112.59 2.90
-2 4 0 115.39 3.70
-3 4 0 10.80 1.10
3 4 0 10.80 1.10
-3 -4 0 10.10 0.70
-4 -4 0 0.60 0.30
4 4 0 0.70 0.50
-4 4 0 0.10 0.40
-5 -4 0 1.00 0.40
5 4 0 0.40 0.50
-5 4 0 0.70 0.60
6 4 0 66.29 3.00
-6 -4 0 65.99 2.70
-6 4 0 64.89 3.40
7 4 0 2.20 0.80
-7 4 0 1.90 1.00
-7 -4 0 1.70 0.70
-8 4 0 8.90 1.80
-8 -4 0 8.30 1.40
-9 4 0 3.20 1.00
-9 4 0 3.50 1.30
-9 -4 0 3.80 1.00
-10 -4 0 7.90 1.40
-10 4 0 5.40 1.60
-10 4 0 8.40 1.80
-11 -4 0 1.20 0.70
-11 -4 0 3.20 1.10
-11 4 0 0.40 0.70
-11 4 0 1.50 1.00
-12 -4 0 0.70 0.80
-12 4 0 2.50 1.20
-12 -4 0 0.80 0.70
-12 4 0 -0.60 0.80
-13 4 0 2.50 1.30
-13 -4 0 2.50 1.10
-13 -4 0 0.60 0.60
-13 4 0 0.00 1.00
-14 -4 0 8.50 1.90
-14 4 0 8.20 2.20
-14 4 0 6.30 2.10
-15 4 0 2.40 1.30
-15 4 0 1.30 0.90
-16 4 0 -1.40 0.80
-16 4 0 1.00 1.30
-17 4 0 -0.10 1.00
-17 4 0 1.10 1.30
0 5 0 -0.10 0.30
0 5 0 0.00 0.40
-1 5 0 2.00 0.60
1 5 0 2.40 0.50
1 5 0 2.70 0.70
-1 5 0 1.70 0.60
2 5 0 3.30 0.40
-2 5 0 4.90 0.90
-2 5 0 4.90 0.90
2 5 0 3.30 0.80
3 5 0 0.70 0.60
-3 5 0 1.20 0.50
-3 5 0 0.10 0.20
4 5 0 0.40 0.50
-4 -5 0 0.40 0.30
-4 5 0 0.50 0.50
-4 5 0 -0.20 0.30
-5 -5 0 0.10 0.20
5 5 0 0.40 0.50
-5 5 0 -0.10 0.50
-6 5 0 2.50 0.90
6 5 0 3.70 0.90
-6 -5 0 3.90 0.70
-7 5 0 1.60 0.90
-7 -5 0 1.80 0.60
7 5 0 2.60 0.90
8 5 0 5.90 1.30
-8 5 0 6.70 1.60
-8 -5 0 7.20 1.20
-8 5 0 8.90 2.00
-9 5 0 0.30 0.70
-9 5 0 0.00 0.50
-9 -5 0 -0.30 0.40
-10 5 0 1.50 1.10
-10 -5 0 2.30 0.80
-10 5 0 2.20 1.10
-11 -5 0 8.30 1.60
-11 5 0 5.60 1.60
-11 5 0 4.60 1.60
-11 -5 0 8.40 1.60
-12 5 0 5.80 1.60
-12 5 0 6.50 2.00
-12 -5 0 8.60 1.70
-12 -5 0 5.20 1.30
-13 5 0 3.80 1.40
-13 -5 0 4.90 1.30
-13 5 0 2.90 1.30
-14 5 0 0.20 0.90
-14 5 0 -0.40 1.20
-15 5 0 0.50 1.20
-15 5 0 -1.40 0.90
-16 5 0 4.20 1.70
-16 5 0 6.10 1.90
-17 5 0 2.90 1.40
-17 5 0 3.40 1.70
0 6 0 97.19 3.80
0 6 0 100.39 3.20
-1 6 0 121.59 4.40
1 6 0 123.49 4.50
1 6 0 123.79 3.50
-1 6 0 124.09 4.00
-2 6 0 29.70 1.80
2 6 0 33.70 1.40
-2 6 0 31.60 2.00
2 6 0 31.40 2.10
-3 6 0 228.48 6.80
-3 6 0 218.18 6.70
3 6 0 231.18 7.00
3 6 0 226.58 5.60
-4 -6 0 57.19 2.00
-4 6 0 54.29 2.90
4 6 0 52.89 2.90
-5 -6 0 34.30 1.60
-5 6 0 34.20 2.10
5 6 0 34.80 2.30
-5 6 0 33.30 2.30
-6 6 0 59.19 3.40
-6 6 0 63.69 3.00
-6 -6 0 63.59 2.50
6 6 0 62.39 3.20
7 6 0 34.40 2.40
-7 -6 0 33.50 1.90
-7 6 0 31.10 2.50
-8 6 0 -1.10 0.30
8 6 0 -0.10 0.50
-8 -6 0 0.80 0.40
-8 6 0 -0.10 0.60
-9 -6 0 1.00 0.60
9 6 0 1.40 0.80
-9 6 0 2.70 1.10
-9 6 0 0.70 0.80
-10 6 0 20.00 2.30
-10 -6 0 19.90 1.80
-10 -6 0 19.30 1.70
-10 6 0 18.50 2.30
-11 -6 0 7.70 1.50
-11 6 0 4.70 1.70
-11 -6 0 5.70 1.30
-11 6 0 6.00 1.80
-12 6 0 0.50 0.90
-12 -6 0 0.90 0.80
-12 6 0 1.10 1.20
-13 6 0 0.00 0.90
-13 6 0 -0.80 0.60
-14 6 0 5.30 1.80
-14 6 0 6.10 1.80
-15 6 0 5.80 1.90
-15 6 0 2.60 1.30
-16 6 0 -0.80 0.90
-16 6 0 0.40 1.20
-17 6 0 -1.90 0.90
-17 6 0 0.60 1.30
0 7 0 -0.40 0.30
0 7 0 0.40 0.50
-1 7 0 -0.60 0.30
1 7 0 0.40 0.60
1 7 0 0.40 0.30
-1 7 0 -0.10 0.50
2 7 0 45.80 2.70
-2 7 0 50.79 2.60
2 7 0 52.69 1.90
-2 7 0 46.80 2.60
-3 7 0 15.40 1.60
3 7 0 16.00 1.60
3 7 0 15.20 0.90
-3 7 0 20.40 1.70
-4 7 0 28.80 2.00
-4 7 0 37.70 2.40
4 7 0 33.60 2.40
-5 -7 0 0.30 0.30
-5 7 0 0.00 0.30
-5 7 0 0.00 0.60
5 7 0 1.90 0.80
-6 7 0 7.30 1.60
6 7 0 8.70 1.60
-6 7 0 7.30 1.40
-6 -7 0 7.20 0.80
-7 7 0 8.50 1.60
-7 7 0 9.50 1.30
-7 7 0 9.80 1.80
-7 -7 0 9.70 0.90
7 7 0 7.80 1.50
8 7 0 4.60 1.20
-8 7 0 3.90 1.30
-8 7 0 1.10 1.00
-8 -7 0 3.50 0.80
-8 7 0 3.00 1.00
9 7 0 -0.30 0.60
-9 7 0 0.50 0.80
-9 7 0 1.60 0.70
-9 -7 0 -0.20 0.40
-9 7 0 -0.60 0.60
-10 7 0 1.30 1.10
10 7 0 -0.10 0.50
-10 7 0 -0.10 0.80
-10 -7 0 0.50 0.50
-10 7 0 -0.40 0.60
-10 -7 0 -0.10 0.50
-11 7 0 1.20 1.10
-11 7 0 1.60 1.10
-11 -7 0 1.50 0.80
-12 7 0 -0.70 0.70
-12 7 0 0.10 0.80
-13 7 0 2.00 1.30
-13 7 0 2.40 1.40
-14 7 0 -0.40 0.70
-14 7 0 0.40 1.00
-15 7 0 0.50 1.30
-15 7 0 2.60 1.40
-16 7 0 0.60 1.30
-16 7 0 0.70 1.10
-17 7 0 0.40 1.50
-17 7 0 2.10 1.20
0 8 0 58.99 3.20
0 8 0 58.99 2.50
-1 8 0 2.90 0.80
1 8 0 3.60 0.70
-1 8 0 2.80 0.90
1 8 0 2.70 1.00
2 8 0 2.10 0.90
2 8 0 2.50 0.50
-2 8 0 3.10 0.90
-2 8 0 3.50 0.90
3 8 0 15.20 1.80
-3 8 0 17.70 1.70
-3 8 0 16.30 1.70
3 8 0 17.40 1.00
-4 8 0 2.80 1.00
4 8 0 0.80 0.80
-4 8 0 4.00 1.10
-5 8 0 -0.30 0.20
5 8 0 2.20 0.90
-5 8 0 1.00 0.80
-5 -8 0 1.10 0.40
6 8 0 -0.10 0.50
-6 8 0 -0.50 0.60
-6 8 0 0.50 0.50
-6 -8 0 0.30 0.30
-6 8 0 0.50 0.60
-7 8 0 23.60 2.30
7 8 0 20.80 2.20
-7 -8 0 23.30 1.50
-7 8 0 25.80 2.10
-7 8 0 25.20 2.40
8 8 0 -0.30 0.60
-8 8 0 0.90 0.90
-8 -8 0 -0.10 0.30
-8 8 0 -0.50 0.40
-8 8 0 0.20 0.70
-9 8 0 0.60 0.90
-9 8 0 0.90 0.80
-9 -8 0 0.20 0.40
-9 8 0 0.70 0.90
9 8 0 -0.40 0.70
-10 -8 0 4.50 1.20
-10 8 0 1.60 1.10
-10 8 0 2.90 1.30
-10 8 0 5.50 1.30
10 8 0 1.70 1.10
-11 8 0 6.30 1.80
-11 8 0 8.30 2.10
-11 -8 0 9.10 1.60
11 8 0 7.70 1.80
-12 8 0 0.80 0.90
-12 8 0 0.70 1.10
-13 8 0 3.80 1.60
-13 8 0 1.30 1.30
-14 8 0 0.10 1.10
-14 8 0 -1.20 0.80
-15 8 0 1.60 1.40
-15 8 0 3.00 1.70
-16 8 0 0.30 1.20
-16 8 0 3.70 1.80
0 9 0 -0.20 0.40
0 9 0 -0.50 0.50
1 9 0 107.49 3.70
1 9 0 105.69 4.80
-1 9 0 109.69 4.10
-1 9 0 117.59 4.90
-2 9 0 0.50 0.70
2 9 0 0.30 0.60
2 9 0 0.20 0.30
-2 9 0 1.00 0.60
3 9 0 22.20 2.20
3 9 0 23.60 1.30
-3 9 0 21.50 1.90
-3 9 0 20.70 2.00
-4 9 0 11.30 1.50
4 9 0 12.10 1.60
-4 9 0 8.20 1.60
4 9 0 10.30 0.80
5 9 0 155.78 6.40
-5 9 0 155.38 6.00
-5 9 0 152.28 6.10
-5 -9 0 153.78 4.40
-5 9 0 163.48 6.40
-6 -9 0 13.50 1.00
6 9 0 16.60 2.00
-6 9 0 15.40 2.40
-6 9 0 10.50 1.80
-7 -9 0 6.20 0.70
-7 9 0 6.70 1.70
7 9 0 8.20 1.80
-7 9 0 5.40 1.50
-7 9 0 10.00 1.70
-8 9 0 4.00 1.40
8 9 0 2.10 1.10
-8 9 0 3.70 1.50
-8 9 0 7.20 1.50
-8 -9 0 4.70 1.10
9 9 0 59.99 4.00
-9 9 0 63.79 4.40
-9 9 0 58.99 4.10
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1 21 8 -0.40 0.80
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1 1 9 22.30 1.70
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1 2 9 4.10 0.90
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5 -2 -9 19.50 1.00
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-11 -2 -9 5.60 1.70
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-11 -2 9 5.70 1.30
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1 3 9 59.89 3.00
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-2 -3 9 23.50 1.40
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3 3 9 64.39 3.30
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-8 -3 9 10.10 1.50
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-10 -3 -9 2.80 1.30
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-10 -3 9 4.80 1.10
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-11 -3 -9 -0.10 0.60
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1 4 9 732.03 17.80
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2 4 9 104.69 4.30
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3 4 9 238.78 7.70
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4 4 9 30.90 2.40
-4 4 -9 30.20 2.30
-4 -4 9 31.80 1.60
5 4 -9 193.78 5.80
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1 5 -9 21.80 1.40
1 5 9 18.70 1.70
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1 5 9 19.20 1.80
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2 5 9 9.10 1.50
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3 5 9 60.49 3.20
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4 5 9 88.09 4.10
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5 5 9 2.70 1.00
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2 6 9 183.98 6.40
3 6 -9 5.40 1.20
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3 6 9 2.90 1.00
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3 6 9 6.80 1.50
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4 6 -9 2.80 0.90
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0 7 9 2.90 1.00
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1 7 -9 73.99 2.70
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-1 7 -9 74.09 3.10
1 7 9 77.89 3.90
1 7 9 71.79 3.60
2 7 -9 18.40 1.10
2 7 -9 18.80 1.90
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2 7 9 21.80 2.00
-2 7 -9 18.20 1.60
2 7 9 16.20 1.80
3 7 -9 18.90 1.80
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3 7 -9 19.10 0.90
3 7 9 17.70 2.00
3 7 9 20.70 1.90
-3 7 -9 19.70 1.70
4 7 -9 3.80 0.30
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4 7 -9 2.40 1.00
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4 7 9 4.00 1.30
-4 7 -9 3.80 1.10
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-2 3 -30 -0.90 1.60
2 3 30 0.80 0.90
-3 3 30 0.80 0.80
-3 3 -30 -2.50 1.20
-4 3 30 2.30 1.20
-4 -3 30 0.50 1.20
-4 3 -30 0.90 1.70
0 4 30 -0.30 1.00
0 4 -30 2.00 2.30
-1 4 30 1.20 1.10
1 4 30 0.80 1.20
-1 4 -30 1.00 1.50
-2 4 30 -1.10 0.80
-2 4 -30 0.10 1.50
2 4 30 0.60 0.90
-3 4 30 -1.50 0.90
3 4 30 1.00 1.20
-3 4 -30 3.60 2.10
0 5 30 1.00 0.80
-1 5 30 0.10 0.90
1 5 30 -0.30 0.90
-2 5 30 0.10 1.00
-2 5 -30 -1.70 1.10
2 5 30 -1.70 1.00
-3 5 30 0.10 1.30
3 5 30 -1.10 0.80
-3 5 -30 -1.70 0.90
0 6 30 4.00 1.60
-1 6 30 0.70 0.90
1 6 30 0.20 0.70
0 0 31 -1.60 0.80
-1 0 31 0.40 0.80
-2 0 31 1.30 1.00
0 1 31 1.60 1.10
-1 1 31 1.60 1.00
-1 -1 31 -1.20 1.00
-2 1 -31 1.80 1.90
0 2 31 0.20 1.00
-1 2 31 -0.10 1.00
-1 2 -31 0.10 1.90
1 2 31 1.90 1.00
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 57390
_shelx_res_file
;
517LLR16.res created by SHELXL-2014/7
TITL 517LLR16_0m_a.res in P2(1)2(1)2(1)
CELL 0.71073 13.2445 16.5273 22.8256 90.000 90.000 90.000
ZERR 8.00 0.0011 0.0017 0.0025 0.000 0.000 0.000
LATT -1
SYMM x+1/2, -y+1/2, -z
SYMM -x, y+1/2, -z+1/2
SYMM -x+1/2, -y, z+1/2
SFAC C H N O
UNIT 216 208 48 24
OMIT 0 1 1
OMIT 0 0 2
OMIT 1 0 2
OMIT 1 0 1
OMIT 2 0 0
OMIT 0 3 9
OMIT 2 2 14
OMIT 4 0 0
OMIT 4 0 2
LIST 4
TEMP -123.000
SIZE 0.158 0.195 0.350
ACTA
L.S. 20
FMAP 2
PLAN 5
SADI 0.01 O1 H1 O21 H21
HTAB O1 N1
EQIV $1 -x+1/2, -y+1, z+1/2
HTAB C3 O23_$1
HTAB C7 O23_$1
HTAB C16 O21
HTAB O21 N21
HTAB C33 O22_$1
HTAB C37 O3_$1
HTAB C46 N3
BOND $H
CONF
WGHT 0.041900 0.288100
FVAR 0.15543
O1 4 0.340958 0.231183 0.277251 11.00000 0.05557 0.03333 =
0.03018 0.00113 -0.00270 -0.00228
H1 2 0.359609 0.283664 0.281707 11.00000 -1.50000
O2 4 0.291153 0.321006 0.036611 11.00000 0.08786 0.06235 =
0.04287 -0.01276 -0.01555 -0.00794
O3 4 0.416256 0.394487 0.009193 11.00000 0.08274 0.09841 =
0.02907 -0.00296 0.00660 -0.00519
N1 3 0.382458 0.368284 0.328268 11.00000 0.02970 0.03027 =
0.02833 0.00444 -0.00030 -0.00107
N2 3 0.399044 0.491952 0.275484 11.00000 0.03478 0.02842 =
0.02674 0.00215 -0.00474 -0.00636
N3 3 0.421765 0.572500 0.283450 11.00000 0.03913 0.03128 =
0.03221 0.00236 -0.00437 -0.00752
N4 3 0.375027 0.088328 0.497395 11.00000 0.03480 0.03453 =
0.03740 0.00837 0.00196 0.00249
N5 3 0.364887 0.012570 0.497797 11.00000 0.04580 0.03498 =
0.03982 0.00959 -0.00136 0.00092
N6 3 0.357637 0.370374 0.046371 11.00000 0.06270 0.04904 =
0.02801 -0.00179 -0.00586 0.00790
C1 1 0.348385 0.197891 0.330931 11.00000 0.03388 0.03699 =
0.02738 0.00274 0.00142 0.00438
C2 1 0.373957 0.243534 0.380514 11.00000 0.02643 0.03336 =
0.02472 0.00102 0.00044 -0.00028
C3 1 0.381890 0.203835 0.434685 11.00000 0.03525 0.03133 =
0.03260 0.00198 -0.00126 -0.00029
AFIX 43
H3 2 0.400103 0.234125 0.468441 11.00000 -1.20000
AFIX 0
C4 1 0.363940 0.122066 0.440156 11.00000 0.03132 0.03806 =
0.03054 0.00875 0.00155 0.00287
C5 1 0.335433 0.078047 0.390195 11.00000 0.04153 0.03530 =
0.04488 0.00512 0.00061 0.00015
AFIX 43
H5 2 0.321364 0.021872 0.393537 11.00000 -1.20000
AFIX 0
C6 1 0.327628 0.115256 0.336483 11.00000 0.04792 0.03250 =
0.04210 -0.00403 -0.00586 -0.00113
AFIX 43
H6 2 0.308093 0.084760 0.303074 11.00000 -1.20000
AFIX 0
C7 1 0.390886 0.330063 0.377300 11.00000 0.03222 0.03483 =
0.02675 -0.00040 -0.00186 -0.00248
AFIX 43
H7 2 0.408431 0.359028 0.411778 11.00000 -1.20000
AFIX 0
C8 1 0.430194 0.581827 0.341114 11.00000 0.03521 0.03099 =
0.03171 0.00032 -0.00426 -0.00257
C9 1 0.415083 0.508105 0.371017 11.00000 0.03494 0.03595 =
0.02640 -0.00076 -0.00378 -0.00104
AFIX 43
H9 2 0.417078 0.499353 0.412136 11.00000 -1.20000
AFIX 0
C10 1 0.396944 0.451858 0.328285 11.00000 0.02939 0.03153 =
0.02619 0.00344 -0.00349 -0.00032
C11 1 0.459375 0.662760 0.367763 11.00000 0.04630 0.03539 =
0.03582 -0.00057 -0.00800 -0.00470
C12 1 0.435825 0.731422 0.325290 11.00000 0.06746 0.03275 =
0.05607 0.00347 -0.01202 -0.00455
AFIX 137
H12A 2 0.455612 0.783121 0.342904 11.00000 -1.50000
H12B 2 0.363275 0.732060 0.316865 11.00000 -1.50000
H12C 2 0.473453 0.723216 0.288802 11.00000 -1.50000
AFIX 0
C13 1 0.401409 0.676381 0.424616 11.00000 0.08492 0.04430 =
0.04756 -0.01357 0.00251 -0.00502
AFIX 137
H13A 2 0.419246 0.729353 0.440898 11.00000 -1.50000
H13B 2 0.419001 0.633929 0.452800 11.00000 -1.50000
H13C 2 0.328719 0.674617 0.416698 11.00000 -1.50000
AFIX 0
C14 1 0.573490 0.660662 0.380148 11.00000 0.05004 0.04331 =
0.08369 -0.00948 -0.01891 -0.00625
AFIX 137
H14A 2 0.594555 0.712363 0.397253 11.00000 -1.50000
H14B 2 0.610159 0.651561 0.343443 11.00000 -1.50000
H14C 2 0.588470 0.616726 0.407638 11.00000 -1.50000
AFIX 0
C15 1 0.388066 0.461031 0.217919 11.00000 0.03397 0.03205 =
0.02621 0.00213 -0.00195 0.00102
C16 1 0.317379 0.401197 0.206266 11.00000 0.03489 0.02871 =
0.02945 0.00182 -0.00313 0.00056
AFIX 43
H16 2 0.275624 0.381008 0.236787 11.00000 -1.20000
AFIX 0
C17 1 0.307960 0.370917 0.149654 11.00000 0.03635 0.02938 =
0.03610 0.00346 -0.01019 0.00177
AFIX 43
H17 2 0.260867 0.329174 0.141167 11.00000 -1.20000
AFIX 0
C18 1 0.368162 0.402585 0.106179 11.00000 0.04350 0.03610 =
0.02788 -0.00264 -0.00659 0.00851
C19 1 0.437332 0.462944 0.116401 11.00000 0.05059 0.04979 =
0.02988 0.01123 0.00055 -0.00178
AFIX 43
H19 2 0.477710 0.483737 0.085472 11.00000 -1.20000
AFIX 0
C20 1 0.446892 0.493052 0.173419 11.00000 0.04727 0.04653 =
0.02996 0.00551 -0.00272 -0.01177
AFIX 43
H20 2 0.493510 0.535259 0.181577 11.00000 -1.20000
AFIX 0
C21 1 0.371964 -0.022893 0.554972 11.00000 0.03436 0.03786 =
0.04213 0.01430 0.00083 0.00224
C22 1 0.386218 0.019236 0.606643 11.00000 0.03806 0.04091 =
0.04580 0.00817 -0.00130 -0.00076
AFIX 43
H22 2 0.393260 0.076433 0.606003 11.00000 -1.20000
AFIX 0
C23 1 0.390196 -0.022124 0.659270 11.00000 0.04209 0.05979 =
0.03928 0.01185 0.00031 -0.00020
AFIX 43
H23 2 0.400285 0.007073 0.694639 11.00000 -1.20000
AFIX 0
C24 1 0.379613 -0.106124 0.661202 11.00000 0.03412 0.06037 =
0.04783 0.02606 0.00620 0.00634
C25 1 0.364397 -0.146844 0.609028 11.00000 0.05360 0.04244 =
0.06516 0.02154 0.01124 0.00189
AFIX 43
H25 2 0.356575 -0.203977 0.609537 11.00000 -1.20000
AFIX 0
C26 1 0.360326 -0.106282 0.556218 11.00000 0.05433 0.04311 =
0.04959 0.00941 -0.00215 0.00416
AFIX 43
H26 2 0.349595 -0.135366 0.520863 11.00000 -1.20000
AFIX 0
C27 1 0.385264 -0.151219 0.718944 11.00000 0.05185 0.08470 =
0.06240 0.03834 0.01033 0.00690
AFIX 137
H27A 2 0.429054 -0.198629 0.714551 11.00000 -1.50000
H27B 2 0.317427 -0.168772 0.730454 11.00000 -1.50000
H27C 2 0.412962 -0.115409 0.749156 11.00000 -1.50000
AFIX 0
O21 4 0.117283 0.453200 0.273515 11.00000 0.05326 0.04621 =
0.02979 -0.00633 0.00000 0.00001
H21 2 0.120580 0.507457 0.278859 11.00000 -1.50000
O22 4 0.192813 0.525525 0.041753 11.00000 0.07018 0.04457 =
0.03737 -0.00421 0.01104 0.00289
O23 4 0.090545 0.618966 0.013590 11.00000 0.07908 0.08683 =
0.02857 -0.00043 -0.01260 0.01838
N21 3 0.139235 0.591773 0.327027 11.00000 0.03383 0.03664 =
0.02601 0.00187 -0.00028 0.00029
N22 3 0.143261 0.720142 0.276931 11.00000 0.03542 0.03604 =
0.02551 0.00264 0.00050 0.00255
N23 3 0.127120 0.800874 0.287148 11.00000 0.03990 0.03368 =
0.03430 0.00095 0.00183 0.00373
N24 3 0.150368 0.310565 0.493701 11.00000 0.03751 0.03513 =
0.04638 0.00573 -0.00055 -0.00371
N25 3 0.134875 0.235367 0.495623 11.00000 0.03429 0.03640 =
0.05043 0.00460 0.00388 -0.00274
N26 3 0.144617 0.587762 0.050777 11.00000 0.04806 0.04847 =
0.02804 0.00267 0.00584 -0.00369
C31 1 0.128568 0.419101 0.327088 11.00000 0.02656 0.04319 =
0.03157 -0.00146 0.00445 -0.00262
C32 1 0.143639 0.466020 0.377755 11.00000 0.02945 0.03478 =
0.03195 -0.00132 -0.00069 -0.00043
C33 1 0.151308 0.426146 0.431552 11.00000 0.03606 0.03869 =
0.03334 -0.00113 -0.00381 0.00101
AFIX 43
H33 2 0.161272 0.457063 0.466159 11.00000 -1.20000
AFIX 0
C34 1 0.144776 0.342974 0.435708 11.00000 0.03215 0.03808 =
0.03793 0.00386 0.00067 -0.00055
C35 1 0.132617 0.297278 0.384553 11.00000 0.03258 0.03378 =
0.04894 0.00053 0.00170 0.00013
AFIX 43
H35 2 0.129436 0.239939 0.386808 11.00000 -1.20000
AFIX 0
C36 1 0.125205 0.335350 0.330655 11.00000 0.03462 0.03892 =
0.04060 -0.01519 0.00594 -0.00484
AFIX 43
H36 2 0.117798 0.304011 0.296031 11.00000 -1.20000
AFIX 0
C37 1 0.148945 0.553110 0.375521 11.00000 0.03679 0.03928 =
0.02781 -0.00118 -0.00150 -0.00007
AFIX 43
H37 2 0.159865 0.582553 0.410700 11.00000 -1.20000
AFIX 0
C38 1 0.111333 0.806314 0.344837 11.00000 0.03420 0.04151 =
0.02952 -0.00287 0.00192 0.00185
C39 1 0.117317 0.730497 0.372725 11.00000 0.03882 0.04138 =
0.02713 -0.00179 -0.00217 -0.00220
AFIX 43
H39 2 0.109777 0.719411 0.413328 11.00000 -1.20000
AFIX 0
C40 1 0.136377 0.676012 0.328704 11.00000 0.03340 0.03834 =
0.02881 0.00297 -0.00058 -0.00241
C41 1 0.087942 0.886003 0.374310 11.00000 0.05529 0.03511 =
0.03851 -0.00496 0.00905 -0.00200
C42 1 0.105317 0.957054 0.332433 11.00000 0.07608 0.03578 =
0.04963 -0.00151 0.00196 0.00134
AFIX 137
H42A 2 0.090187 1.007939 0.352652 11.00000 -1.50000
H42B 2 0.060983 0.951424 0.298302 11.00000 -1.50000
H42C 2 0.175900 0.957264 0.319550 11.00000 -1.50000
AFIX 0
C43 1 -0.023008 0.885141 0.392651 11.00000 0.08534 0.05145 =
0.11979 -0.01833 0.05506 0.00076
AFIX 137
H43A 2 -0.040551 0.937244 0.410441 11.00000 -1.50000
H43B 2 -0.034142 0.841686 0.421139 11.00000 -1.50000
H43C 2 -0.065490 0.875941 0.358135 11.00000 -1.50000
AFIX 0
C44 1 0.154806 0.895246 0.428548 11.00000 0.13458 0.04396 =
0.04719 -0.00667 -0.01692 -0.01290
AFIX 137
H44A 2 0.140717 0.947289 0.447431 11.00000 -1.50000
H44B 2 0.225968 0.893171 0.416881 11.00000 -1.50000
H44C 2 0.140566 0.851198 0.456078 11.00000 -1.50000
AFIX 0
C45 1 0.150991 0.690133 0.219271 11.00000 0.03235 0.03593 =
0.02769 0.00174 0.00096 0.00191
C46 1 0.206293 0.621349 0.207163 11.00000 0.03631 0.03922 =
0.02695 0.00234 -0.00159 0.00747
AFIX 43
H46 2 0.245477 0.596816 0.237159 11.00000 -1.20000
AFIX 0
C47 1 0.204988 0.587920 0.151589 11.00000 0.04413 0.03457 =
0.03181 0.00440 0.00183 0.00924
AFIX 43
H47 2 0.240968 0.539487 0.143430 11.00000 -1.20000
AFIX 0
C48 1 0.150470 0.626267 0.108315 11.00000 0.03586 0.04083 =
0.02237 0.00380 -0.00070 -0.00001
C49 1 0.100579 0.698311 0.118377 11.00000 0.04145 0.05277 =
0.02653 0.00996 -0.00111 0.01422
AFIX 43
H49 2 0.066135 0.725192 0.087491 11.00000 -1.20000
AFIX 0
C50 1 0.101714 0.730506 0.174154 11.00000 0.03753 0.04377 =
0.03347 0.00494 0.00212 0.01356
AFIX 43
H50 2 0.068694 0.780446 0.181742 11.00000 -1.20000
AFIX 0
C51 1 0.138209 0.203380 0.553154 11.00000 0.03033 0.04222 =
0.04518 0.00471 0.00040 -0.00507
C52 1 0.134846 0.249011 0.604619 11.00000 0.03478 0.04288 =
0.05140 0.00907 -0.00460 -0.00826
AFIX 43
H52 2 0.130800 0.306329 0.602550 11.00000 -1.20000
AFIX 0
C53 1 0.137398 0.210850 0.658823 11.00000 0.03856 0.05385 =
0.05048 0.00513 -0.00419 -0.00912
AFIX 43
H53 2 0.133812 0.242324 0.693587 11.00000 -1.20000
AFIX 0
C54 1 0.145163 0.126865 0.662807 11.00000 0.02875 0.05730 =
0.05648 0.01531 -0.00459 -0.00998
C55 1 0.147397 0.082413 0.611594 11.00000 0.03176 0.04235 =
0.06339 0.01516 0.00229 -0.00169
AFIX 43
H55 2 0.152038 0.025125 0.613686 11.00000 -1.20000
AFIX 0
C56 1 0.143016 0.119560 0.557187 11.00000 0.03622 0.03627 =
0.05949 0.00308 0.00234 -0.00371
AFIX 43
H56 2 0.143300 0.087635 0.522577 11.00000 -1.20000
AFIX 0
C57 1 0.149895 0.086824 0.722061 11.00000 0.05039 0.07933 =
0.06398 0.03000 -0.01096 -0.01381
AFIX 137
H57A 2 0.140658 0.028326 0.717531 11.00000 -1.50000
H57B 2 0.096346 0.108582 0.747155 11.00000 -1.50000
H57C 2 0.215756 0.097527 0.740028 11.00000 -1.50000
AFIX 0
HKLF 4 1 1 0 0 0 1 0 0 0 1
REM 517LLR16_0m_a.res in P2(1)2(1)2(1)
REM R1 = 0.0629 for 7186 Fo > 4sig(Fo) and 0.1378 for all 13380 data
REM 663 parameters refined using 1 restraints
END
WGHT 0.0419 0.2881
REM Highest difference peak 0.202, deepest hole -0.257, 1-sigma level 0.048
Q1 1 0.3846 0.8349 0.3389 11.00000 0.05 0.20
Q2 1 0.0347 1.0184 0.3620 11.00000 0.05 0.19
Q3 1 0.1374 0.5678 0.2929 11.00000 0.05 0.18
Q4 1 0.0760 0.1109 0.4791 11.00000 0.05 0.18
Q5 1 0.1379 0.1416 0.7699 11.00000 0.05 0.17
;
_shelx_res_checksum 42089
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 0.3410(2) 0.23118(17) 0.27725(13) 0.0397(7) Uani d 1 . .
H H1 0.360(4) 0.284(2) 0.282(2) 0.060 Uiso d 1 . .
O O2 0.2912(3) 0.3210(2) 0.03661(15) 0.0644(10) Uani d 1 . .
O O3 0.4163(3) 0.3945(2) 0.00919(16) 0.0701(11) Uani d 1 . .
N N1 0.3825(2) 0.36828(17) 0.32827(15) 0.0294(7) Uani d 1 . .
N N2 0.3990(2) 0.49195(18) 0.27548(14) 0.0300(7) Uani d 1 . .
N N3 0.4218(3) 0.57250(18) 0.28345(16) 0.0342(8) Uani d 1 . .
N N4 0.3750(3) 0.08833(19) 0.49739(16) 0.0356(8) Uani d 1 . .
N N5 0.3649(3) 0.0126(2) 0.49780(16) 0.0402(9) Uani d 1 . .
N N6 0.3576(3) 0.3704(2) 0.04637(17) 0.0466(10) Uani d 1 . .
C C1 0.3484(3) 0.1979(2) 0.33093(18) 0.0328(9) Uani d 1 . .
C C2 0.3740(3) 0.2435(2) 0.38051(17) 0.0282(9) Uani d 1 . .
C C3 0.3819(3) 0.2038(2) 0.43468(19) 0.0331(9) Uani d 1 . .
H H3 0.4001 0.2341 0.4684 0.040 Uiso calc 1 . .
C C4 0.3639(3) 0.1221(2) 0.44016(19) 0.0333(9) Uani d 1 . .
C C5 0.3354(3) 0.0780(3) 0.3902(2) 0.0406(11) Uani d 1 . .
H H5 0.3214 0.0219 0.3935 0.049 Uiso calc 1 . .
C C6 0.3276(3) 0.1153(2) 0.3365(2) 0.0408(11) Uani d 1 . .
H H6 0.3081 0.0848 0.3031 0.049 Uiso calc 1 . .
C C7 0.3909(3) 0.3301(2) 0.37730(18) 0.0313(9) Uani d 1 . .
H H7 0.4084 0.3590 0.4118 0.038 Uiso calc 1 . .
C C8 0.4302(3) 0.5818(2) 0.34111(19) 0.0326(9) Uani d 1 . .
C C9 0.4151(3) 0.5081(2) 0.37102(19) 0.0324(9) Uani d 1 . .
H H9 0.4171 0.4994 0.4121 0.039 Uiso calc 1 . .
C C10 0.3969(3) 0.4519(2) 0.32828(18) 0.0290(9) Uani d 1 . .
C C11 0.4594(3) 0.6628(2) 0.3678(2) 0.0392(10) Uani d 1 . .
C C12 0.4358(4) 0.7314(2) 0.3253(2) 0.0521(13) Uani d 1 . .
H H12A 0.4556 0.7831 0.3429 0.078 Uiso calc 1 . .
H H12B 0.3633 0.7321 0.3169 0.078 Uiso calc 1 . .
H H12C 0.4735 0.7232 0.2888 0.078 Uiso calc 1 . .
C C13 0.4014(4) 0.6764(3) 0.4246(2) 0.0589(15) Uani d 1 . .
H H13A 0.4192 0.7294 0.4409 0.088 Uiso calc 1 . .
H H13B 0.4190 0.6339 0.4528 0.088 Uiso calc 1 . .
H H13C 0.3287 0.6746 0.4167 0.088 Uiso calc 1 . .
C C14 0.5735(4) 0.6607(3) 0.3801(3) 0.0590(15) Uani d 1 . .
H H14A 0.5946 0.7124 0.3973 0.089 Uiso calc 1 . .
H H14B 0.6102 0.6516 0.3434 0.089 Uiso calc 1 . .
H H14C 0.5885 0.6167 0.4076 0.089 Uiso calc 1 . .
C C15 0.3881(3) 0.4610(2) 0.21792(18) 0.0307(9) Uani d 1 . .
C C16 0.3174(3) 0.4012(2) 0.20627(18) 0.0310(9) Uani d 1 . .
H H16 0.2756 0.3810 0.2368 0.037 Uiso calc 1 . .
C C17 0.3080(3) 0.3709(2) 0.14965(19) 0.0339(10) Uani d 1 . .
H H17 0.2609 0.3292 0.1412 0.041 Uiso calc 1 . .
C C18 0.3682(3) 0.4026(2) 0.10618(19) 0.0358(10) Uani d 1 . .
C C19 0.4373(4) 0.4629(3) 0.1164(2) 0.0434(11) Uani d 1 . .
H H19 0.4777 0.4837 0.0855 0.052 Uiso calc 1 . .
C C20 0.4469(3) 0.4931(3) 0.17342(19) 0.0413(11) Uani d 1 . .
H H20 0.4935 0.5353 0.1816 0.050 Uiso calc 1 . .
C C21 0.3720(3) -0.0229(2) 0.5550(2) 0.0381(10) Uani d 1 . .
C C22 0.3862(3) 0.0192(3) 0.6066(2) 0.0416(11) Uani d 1 . .
H H22 0.3933 0.0764 0.6060 0.050 Uiso calc 1 . .
C C23 0.3902(3) -0.0221(3) 0.6593(2) 0.0471(12) Uani d 1 . .
H H23 0.4003 0.0071 0.6946 0.056 Uiso calc 1 . .
C C24 0.3796(3) -0.1061(3) 0.6612(2) 0.0474(12) Uani d 1 . .
C C25 0.3644(4) -0.1468(3) 0.6090(2) 0.0537(14) Uani d 1 . .
H H25 0.3566 -0.2040 0.6095 0.064 Uiso calc 1 . .
C C26 0.3603(4) -0.1063(3) 0.5562(2) 0.0490(12) Uani d 1 . .
H H26 0.3496 -0.1354 0.5209 0.059 Uiso calc 1 . .
C C27 0.3853(4) -0.1512(3) 0.7189(3) 0.0663(16) Uani d 1 . .
H H27A 0.4291 -0.1986 0.7146 0.099 Uiso calc 1 . .
H H27B 0.3174 -0.1688 0.7305 0.099 Uiso calc 1 . .
H H27C 0.4130 -0.1154 0.7492 0.099 Uiso calc 1 . .
O O21 0.1173(2) 0.45320(18) 0.27352(14) 0.0431(8) Uani d 1 . .
H H21 0.121(4) 0.507(2) 0.279(2) 0.065 Uiso d 1 . .
O O22 0.1928(3) 0.52552(19) 0.04175(14) 0.0507(9) Uani d 1 . .
O O23 0.0905(3) 0.6190(2) 0.01359(15) 0.0648(10) Uani d 1 . .
N N21 0.1392(2) 0.59177(18) 0.32703(15) 0.0322(8) Uani d 1 . .
N N22 0.1433(2) 0.72014(19) 0.27693(15) 0.0323(8) Uani d 1 . .
N N23 0.1271(3) 0.80087(19) 0.28715(16) 0.0360(8) Uani d 1 . .
N N24 0.1504(3) 0.3106(2) 0.49370(17) 0.0397(9) Uani d 1 . .
N N25 0.1349(3) 0.2354(2) 0.49562(17) 0.0404(9) Uani d 1 . .
N N26 0.1446(3) 0.5878(2) 0.05078(16) 0.0415(9) Uani d 1 . .
C C31 0.1286(3) 0.4191(2) 0.32709(19) 0.0338(9) Uani d 1 . .
C C32 0.1436(3) 0.4660(2) 0.37775(19) 0.0321(9) Uani d 1 . .
C C33 0.1513(3) 0.4261(2) 0.4316(2) 0.0360(10) Uani d 1 . .
H H33 0.1613 0.4571 0.4662 0.043 Uiso calc 1 . .
C C34 0.1448(3) 0.3430(2) 0.4357(2) 0.0361(10) Uani d 1 . .
C C35 0.1326(3) 0.2973(2) 0.3846(2) 0.0384(10) Uani d 1 . .
H H35 0.1294 0.2399 0.3868 0.046 Uiso calc 1 . .
C C36 0.1252(3) 0.3354(2) 0.3307(2) 0.0380(10) Uani d 1 . .
H H36 0.1178 0.3040 0.2960 0.046 Uiso calc 1 . .
C C37 0.1489(3) 0.5531(2) 0.37552(19) 0.0346(10) Uani d 1 . .
H H37 0.1599 0.5826 0.4107 0.042 Uiso calc 1 . .
C C38 0.1113(3) 0.8063(2) 0.34484(19) 0.0351(10) Uani d 1 . .
C C39 0.1173(3) 0.7305(2) 0.37272(19) 0.0358(10) Uani d 1 . .
H H39 0.1098 0.7194 0.4133 0.043 Uiso calc 1 . .
C C40 0.1364(3) 0.6760(2) 0.32870(18) 0.0335(9) Uani d 1 . .
C C41 0.0879(4) 0.8860(2) 0.3743(2) 0.0430(11) Uani d 1 . .
C C42 0.1053(4) 0.9571(3) 0.3324(2) 0.0538(14) Uani d 1 . .
H H42A 0.0902 1.0079 0.3527 0.081 Uiso calc 1 . .
H H42B 0.0610 0.9514 0.2983 0.081 Uiso calc 1 . .
H H42C 0.1759 0.9573 0.3196 0.081 Uiso calc 1 . .
C C43 -0.0230(5) 0.8851(3) 0.3927(3) 0.086(2) Uani d 1 . .
H H43A -0.0406 0.9372 0.4104 0.128 Uiso calc 1 . .
H H43B -0.0341 0.8417 0.4211 0.128 Uiso calc 1 . .
H H43C -0.0655 0.8759 0.3581 0.128 Uiso calc 1 . .
C C44 0.1548(5) 0.8952(3) 0.4285(2) 0.0752(19) Uani d 1 . .
H H44A 0.1407 0.9473 0.4474 0.113 Uiso calc 1 . .
H H44B 0.2260 0.8932 0.4169 0.113 Uiso calc 1 . .
H H44C 0.1406 0.8512 0.4561 0.113 Uiso calc 1 . .
C C45 0.1510(3) 0.6901(2) 0.21927(18) 0.0320(9) Uani d 1 . .
C C46 0.2063(3) 0.6213(2) 0.20716(18) 0.0342(9) Uani d 1 . .
H H46 0.2455 0.5968 0.2372 0.041 Uiso calc 1 . .
C C47 0.2050(3) 0.5879(2) 0.15159(19) 0.0368(10) Uani d 1 . .
H H47 0.2410 0.5395 0.1434 0.044 Uiso calc 1 . .
C C48 0.1505(3) 0.6263(2) 0.10831(18) 0.0330(9) Uani d 1 . .
C C49 0.1006(3) 0.6983(3) 0.11838(19) 0.0402(11) Uani d 1 . .
H H49 0.0661 0.7252 0.0875 0.048 Uiso calc 1 . .
C C50 0.1017(3) 0.7305(3) 0.17415(19) 0.0383(10) Uani d 1 . .
H H50 0.0687 0.7804 0.1817 0.046 Uiso calc 1 . .
C C51 0.1382(3) 0.2034(3) 0.5532(2) 0.0392(10) Uani d 1 . .
C C52 0.1348(3) 0.2490(3) 0.6046(2) 0.0430(11) Uani d 1 . .
H H52 0.1308 0.3063 0.6025 0.052 Uiso calc 1 . .
C C53 0.1374(3) 0.2108(3) 0.6588(2) 0.0476(12) Uani d 1 . .
H H53 0.1338 0.2423 0.6936 0.057 Uiso calc 1 . .
C C54 0.1452(3) 0.1269(3) 0.6628(2) 0.0475(12) Uani d 1 . .
C C55 0.1474(3) 0.0824(3) 0.6116(2) 0.0458(12) Uani d 1 . .
H H55 0.1520 0.0251 0.6137 0.055 Uiso calc 1 . .
C C56 0.1430(3) 0.1196(3) 0.5572(2) 0.0440(11) Uani d 1 . .
H H56 0.1433 0.0876 0.5226 0.053 Uiso calc 1 . .
C C57 0.1499(4) 0.0868(3) 0.7221(2) 0.0646(16) Uani d 1 . .
H H57A 0.1407 0.0283 0.7175 0.097 Uiso calc 1 . .
H H57B 0.0963 0.1086 0.7472 0.097 Uiso calc 1 . .
H H57C 0.2158 0.0975 0.7400 0.097 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 0.056(2) 0.0333(15) 0.0302(17) -0.0023(14) -0.0027(15) 0.0011(14)
O2 0.088(3) 0.062(2) 0.043(2) -0.008(2) -0.016(2) -0.0128(18)
O3 0.083(3) 0.098(3) 0.029(2) -0.005(2) 0.007(2) -0.003(2)
N1 0.0297(18) 0.0303(16) 0.0283(19) -0.0011(14) -0.0003(15) 0.0044(14)
N2 0.0348(19) 0.0284(16) 0.0267(19) -0.0064(14) -0.0047(15) 0.0021(14)
N3 0.039(2) 0.0313(17) 0.032(2) -0.0075(15) -0.0044(16) 0.0024(15)
N4 0.035(2) 0.0345(18) 0.037(2) 0.0025(16) 0.0020(17) 0.0084(16)
N5 0.046(2) 0.0350(19) 0.040(2) 0.0009(17) -0.0014(19) 0.0096(17)
N6 0.063(3) 0.049(2) 0.028(2) 0.008(2) -0.006(2) -0.0018(18)
C1 0.034(2) 0.037(2) 0.027(2) 0.0044(18) 0.0014(19) 0.0027(19)
C2 0.026(2) 0.033(2) 0.025(2) -0.0003(16) 0.0004(17) 0.0010(16)
C3 0.035(2) 0.031(2) 0.033(2) -0.0003(18) -0.0013(19) 0.0020(18)
C4 0.031(2) 0.038(2) 0.031(2) 0.0029(19) 0.0015(18) 0.0088(19)
C5 0.042(3) 0.035(2) 0.045(3) 0.0001(19) 0.001(2) 0.005(2)
C6 0.048(3) 0.032(2) 0.042(3) -0.0011(19) -0.006(2) -0.004(2)
C7 0.032(2) 0.035(2) 0.027(2) -0.0025(17) -0.0019(18) -0.0004(18)
C8 0.035(2) 0.031(2) 0.032(2) -0.0026(17) -0.0043(18) 0.0003(18)
C9 0.035(2) 0.036(2) 0.026(2) -0.0010(18) -0.0038(18) -0.0008(18)
C10 0.029(2) 0.0315(19) 0.026(2) -0.0003(16) -0.0035(18) 0.0034(17)
C11 0.046(3) 0.035(2) 0.036(3) -0.0047(19) -0.008(2) -0.001(2)
C12 0.067(3) 0.033(2) 0.056(3) -0.005(2) -0.012(3) 0.003(2)
C13 0.085(4) 0.044(3) 0.048(3) -0.005(3) 0.003(3) -0.014(2)
C14 0.050(3) 0.043(3) 0.084(4) -0.006(2) -0.019(3) -0.009(3)
C15 0.034(2) 0.0320(19) 0.026(2) 0.0010(17) -0.0019(18) 0.0021(17)
C16 0.035(2) 0.029(2) 0.029(2) 0.0006(17) -0.0031(18) 0.0018(17)
C17 0.036(2) 0.029(2) 0.036(2) 0.0018(18) -0.0102(19) 0.0035(18)
C18 0.043(3) 0.036(2) 0.028(2) 0.009(2) -0.007(2) -0.0026(18)
C19 0.051(3) 0.050(3) 0.030(3) -0.002(2) 0.001(2) 0.011(2)
C20 0.047(3) 0.047(2) 0.030(2) -0.012(2) -0.003(2) 0.006(2)
C21 0.034(2) 0.038(2) 0.042(3) 0.0022(19) 0.001(2) 0.014(2)
C22 0.038(3) 0.041(2) 0.046(3) -0.001(2) -0.001(2) 0.008(2)
C23 0.042(3) 0.060(3) 0.039(3) 0.000(2) 0.000(2) 0.012(2)
C24 0.034(3) 0.060(3) 0.048(3) 0.006(2) 0.006(2) 0.026(3)
C25 0.054(3) 0.042(3) 0.065(4) 0.002(2) 0.011(3) 0.022(3)
C26 0.054(3) 0.043(3) 0.050(3) 0.004(2) -0.002(3) 0.009(2)
C27 0.052(3) 0.085(4) 0.062(4) 0.007(3) 0.010(3) 0.038(3)
O21 0.053(2) 0.0462(17) 0.0298(17) 0.0000(16) 0.0000(15) -0.0063(15)
O22 0.070(2) 0.0446(18) 0.037(2) 0.0029(17) 0.0110(17) -0.0042(15)
O23 0.079(3) 0.087(3) 0.0286(19) 0.018(2) -0.0126(19) -0.0004(19)
N21 0.0338(19) 0.0366(18) 0.0260(18) 0.0003(15) -0.0003(16) 0.0019(15)
N22 0.0354(19) 0.0360(18) 0.0255(19) 0.0026(15) 0.0005(16) 0.0026(15)
N23 0.040(2) 0.0337(18) 0.034(2) 0.0037(16) 0.0018(17) 0.0009(15)
N24 0.038(2) 0.0351(19) 0.046(2) -0.0037(16) -0.0006(18) 0.0057(17)
N25 0.034(2) 0.0364(19) 0.050(3) -0.0027(16) 0.0039(19) 0.0046(18)
N26 0.048(2) 0.048(2) 0.028(2) -0.0037(19) 0.0058(18) 0.0027(18)
C31 0.027(2) 0.043(2) 0.032(2) -0.0026(18) 0.0044(19) -0.0015(19)
C32 0.029(2) 0.035(2) 0.032(2) -0.0004(17) -0.0007(19) -0.0013(18)
C33 0.036(2) 0.039(2) 0.033(2) 0.0010(19) -0.004(2) -0.001(2)
C34 0.032(2) 0.038(2) 0.038(3) -0.0005(18) 0.001(2) 0.004(2)
C35 0.033(2) 0.034(2) 0.049(3) 0.0001(18) 0.002(2) 0.001(2)
C36 0.035(2) 0.039(2) 0.041(3) -0.0048(19) 0.006(2) -0.015(2)
C37 0.037(2) 0.039(2) 0.028(2) -0.0001(18) -0.0015(19) -0.0012(19)
C38 0.034(2) 0.042(2) 0.030(2) 0.0018(19) 0.0019(19) -0.0029(19)
C39 0.039(2) 0.041(2) 0.027(2) -0.0022(19) -0.0022(19) -0.0018(19)
C40 0.033(2) 0.038(2) 0.029(2) -0.0024(18) -0.0006(19) 0.0030(19)
C41 0.055(3) 0.035(2) 0.039(3) -0.002(2) 0.009(2) -0.005(2)
C42 0.076(4) 0.036(2) 0.050(3) 0.001(2) 0.002(3) -0.002(2)
C43 0.085(4) 0.051(3) 0.120(6) 0.001(3) 0.055(4) -0.018(4)
C44 0.135(6) 0.044(3) 0.047(3) -0.013(3) -0.017(4) -0.007(3)
C45 0.032(2) 0.036(2) 0.028(2) 0.0019(17) 0.0010(18) 0.0017(19)
C46 0.036(2) 0.039(2) 0.027(2) 0.0075(18) -0.0016(18) 0.0023(19)
C47 0.044(3) 0.035(2) 0.032(2) 0.0092(19) 0.002(2) 0.0044(19)
C48 0.036(2) 0.041(2) 0.022(2) 0.0000(19) -0.0007(18) 0.0038(18)
C49 0.041(3) 0.053(3) 0.027(2) 0.014(2) -0.001(2) 0.010(2)
C50 0.038(2) 0.044(2) 0.033(3) 0.0136(19) 0.002(2) 0.005(2)
C51 0.030(2) 0.042(2) 0.045(3) -0.0051(19) 0.000(2) 0.005(2)
C52 0.035(2) 0.043(2) 0.051(3) -0.008(2) -0.005(2) 0.009(2)
C53 0.039(3) 0.054(3) 0.050(3) -0.009(2) -0.004(2) 0.005(2)
C54 0.029(2) 0.057(3) 0.056(3) -0.010(2) -0.005(2) 0.015(3)
C55 0.032(2) 0.042(2) 0.063(4) -0.002(2) 0.002(2) 0.015(3)
C56 0.036(2) 0.036(2) 0.059(3) -0.004(2) 0.002(2) 0.003(2)
C57 0.050(3) 0.079(4) 0.064(4) -0.014(3) -0.011(3) 0.030(3)
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 . . 106(3) ?
C7 N1 C10 . . 118.2(3) ?
C10 N2 N3 . . 110.8(3) ?
C10 N2 C15 . . 129.5(3) ?
N3 N2 C15 . . 119.6(3) ?
C8 N3 N2 . . 105.1(3) ?
N5 N4 C4 . . 112.6(4) ?
N4 N5 C21 . . 114.0(4) ?
O3 N6 O2 . . 123.5(4) ?
O3 N6 C18 . . 117.9(4) ?
O2 N6 C18 . . 118.6(4) ?
O1 C1 C6 . . 117.8(4) ?
O1 C1 C2 . . 122.2(4) ?
C6 C1 C2 . . 120.0(4) ?
C1 C2 C3 . . 118.5(3) ?
C1 C2 C7 . . 121.8(4) ?
C3 C2 C7 . . 119.6(4) ?
C4 C3 C2 . . 121.7(4) ?
C4 C3 H3 . . 119.2 ?
C2 C3 H3 . . 119.2 ?
C3 C4 C5 . . 118.7(4) ?
C3 C4 N4 . . 116.6(4) ?
C5 C4 N4 . . 124.6(4) ?
C6 C5 C4 . . 120.8(4) ?
C6 C5 H5 . . 119.6 ?
C4 C5 H5 . . 119.6 ?
C5 C6 C1 . . 120.2(4) ?
C5 C6 H6 . . 119.9 ?
C1 C6 H6 . . 119.9 ?
N1 C7 C2 . . 120.9(4) ?
N1 C7 H7 . . 119.5 ?
C2 C7 H7 . . 119.5 ?
N3 C8 C9 . . 111.5(3) ?
N3 C8 C11 . . 121.3(4) ?
C9 C8 C11 . . 127.1(4) ?
C10 C9 C8 . . 105.5(4) ?
C10 C9 H9 . . 127.3 ?
C8 C9 H9 . . 127.3 ?
C9 C10 N2 . . 107.1(3) ?
C9 C10 N1 . . 134.2(4) ?
N2 C10 N1 . . 118.7(3) ?
C8 C11 C13 . . 110.0(4) ?
C8 C11 C12 . . 110.4(4) ?
C13 C11 C12 . . 109.2(4) ?
C8 C11 C14 . . 107.7(4) ?
C13 C11 C14 . . 110.0(4) ?
C12 C11 C14 . . 109.6(4) ?
C11 C12 H12A . . 109.5 ?
C11 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C11 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C11 C13 H13A . . 109.5 ?
C11 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C11 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C11 C14 H14A . . 109.5 ?
C11 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C11 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
C20 C15 C16 . . 120.7(4) ?
C20 C15 N2 . . 119.0(4) ?
C16 C15 N2 . . 120.3(4) ?
C15 C16 C17 . . 119.7(4) ?
C15 C16 H16 . . 120.2 ?
C17 C16 H16 . . 120.2 ?
C18 C17 C16 . . 118.7(4) ?
C18 C17 H17 . . 120.6 ?
C16 C17 H17 . . 120.6 ?
C19 C18 C17 . . 122.7(4) ?
C19 C18 N6 . . 118.9(4) ?
C17 C18 N6 . . 118.4(4) ?
C18 C19 C20 . . 118.5(4) ?
C18 C19 H19 . . 120.8 ?
C20 C19 H19 . . 120.8 ?
C15 C20 C19 . . 119.7(4) ?
C15 C20 H20 . . 120.2 ?
C19 C20 H20 . . 120.2 ?
C22 C21 C26 . . 119.9(4) ?
C22 C21 N5 . . 125.4(4) ?
C26 C21 N5 . . 114.7(4) ?
C21 C22 C23 . . 119.8(4) ?
C21 C22 H22 . . 120.1 ?
C23 C22 H22 . . 120.1 ?
C22 C23 C24 . . 121.0(5) ?
C22 C23 H23 . . 119.5 ?
C24 C23 H23 . . 119.5 ?
C25 C24 C23 . . 118.1(4) ?
C25 C24 C27 . . 121.1(5) ?
C23 C24 C27 . . 120.8(5) ?
C26 C25 C24 . . 121.4(4) ?
C26 C25 H25 . . 119.3 ?
C24 C25 H25 . . 119.3 ?
C25 C26 C21 . . 119.7(5) ?
C25 C26 H26 . . 120.1 ?
C21 C26 H26 . . 120.1 ?
C24 C27 H27A . . 109.5 ?
C24 C27 H27B . . 109.5 ?
H27A C27 H27B . . 109.5 ?
C24 C27 H27C . . 109.5 ?
H27A C27 H27C . . 109.5 ?
H27B C27 H27C . . 109.5 ?
C31 O21 H21 . . 107(3) ?
C37 N21 C40 . . 118.4(4) ?
N23 N22 C40 . . 110.8(3) ?
N23 N22 C45 . . 120.8(3) ?
C40 N22 C45 . . 127.8(3) ?
C38 N23 N22 . . 104.9(3) ?
N25 N24 C34 . . 113.1(4) ?
N24 N25 C51 . . 113.3(4) ?
O23 N26 O22 . . 122.7(4) ?
O23 N26 C48 . . 118.1(4) ?
O22 N26 C48 . . 119.2(4) ?
O21 C31 C36 . . 117.7(4) ?
O21 C31 C32 . . 121.9(4) ?
C36 C31 C32 . . 120.4(4) ?
C33 C32 C31 . . 118.2(4) ?
C33 C32 C37 . . 119.9(4) ?
C31 C32 C37 . . 121.9(4) ?
C34 C33 C32 . . 121.7(4) ?
C34 C33 H33 . . 119.2 ?
C32 C33 H33 . . 119.2 ?
C33 C34 C35 . . 119.1(4) ?
C33 C34 N24 . . 115.7(4) ?
C35 C34 N24 . . 125.2(4) ?
C36 C35 C34 . . 120.3(4) ?
C36 C35 H35 . . 119.9 ?
C34 C35 H35 . . 119.9 ?
C35 C36 C31 . . 120.2(4) ?
C35 C36 H36 . . 119.9 ?
C31 C36 H36 . . 119.9 ?
N21 C37 C32 . . 121.5(4) ?
N21 C37 H37 . . 119.3 ?
C32 C37 H37 . . 119.3 ?
N23 C38 C39 . . 112.1(4) ?
N23 C38 C41 . . 122.0(4) ?
C39 C38 C41 . . 125.9(4) ?
C40 C39 C38 . . 105.3(4) ?
C40 C39 H39 . . 127.4 ?
C38 C39 H39 . . 127.4 ?
C39 C40 N22 . . 106.8(3) ?
C39 C40 N21 . . 132.9(4) ?
N22 C40 N21 . . 119.9(4) ?
C38 C41 C43 . . 108.1(4) ?
C38 C41 C44 . . 109.2(4) ?
C43 C41 C44 . . 109.6(5) ?
C38 C41 C42 . . 111.1(4) ?
C43 C41 C42 . . 108.8(4) ?
C44 C41 C42 . . 110.0(4) ?
C41 C42 H42A . . 109.5 ?
C41 C42 H42B . . 109.5 ?
H42A C42 H42B . . 109.5 ?
C41 C42 H42C . . 109.5 ?
H42A C42 H42C . . 109.5 ?
H42B C42 H42C . . 109.5 ?
C41 C43 H43A . . 109.5 ?
C41 C43 H43B . . 109.5 ?
H43A C43 H43B . . 109.5 ?
C41 C43 H43C . . 109.5 ?
H43A C43 H43C . . 109.5 ?
H43B C43 H43C . . 109.5 ?
C41 C44 H44A . . 109.5 ?
C41 C44 H44B . . 109.5 ?
H44A C44 H44B . . 109.5 ?
C41 C44 H44C . . 109.5 ?
H44A C44 H44C . . 109.5 ?
H44B C44 H44C . . 109.5 ?
C46 C45 C50 . . 119.8(4) ?
C46 C45 N22 . . 121.0(4) ?
C50 C45 N22 . . 119.2(4) ?
C45 C46 C47 . . 120.4(4) ?
C45 C46 H46 . . 119.8 ?
C47 C46 H46 . . 119.8 ?
C48 C47 C46 . . 118.7(4) ?
C48 C47 H47 . . 120.7 ?
C46 C47 H47 . . 120.7 ?
C47 C48 C49 . . 121.9(4) ?
C47 C48 N26 . . 118.1(4) ?
C49 C48 N26 . . 120.0(4) ?
C50 C49 C48 . . 118.7(4) ?
C50 C49 H49 . . 120.6 ?
C48 C49 H49 . . 120.6 ?
C49 C50 C45 . . 120.2(4) ?
C49 C50 H50 . . 119.9 ?
C45 C50 H50 . . 119.9 ?
C56 C51 C52 . . 118.9(4) ?
C56 C51 N25 . . 115.8(4) ?
C52 C51 N25 . . 125.3(4) ?
C53 C52 C51 . . 120.2(4) ?
C53 C52 H52 . . 119.9 ?
C51 C52 H52 . . 119.9 ?
C52 C53 C54 . . 120.8(5) ?
C52 C53 H53 . . 119.6 ?
C54 C53 H53 . . 119.6 ?
C55 C54 C53 . . 118.4(5) ?
C55 C54 C57 . . 121.7(5) ?
C53 C54 C57 . . 119.9(5) ?
C54 C55 C56 . . 121.4(4) ?
C54 C55 H55 . . 119.3 ?
C56 C55 H55 . . 119.3 ?
C55 C56 C51 . . 120.2(5) ?
C55 C56 H56 . . 119.9 ?
C51 C56 H56 . . 119.9 ?
C54 C57 H57A . . 109.5 ?
C54 C57 H57B . . 109.5 ?
H57A C57 H57B . . 109.5 ?
C54 C57 H57C . . 109.5 ?
H57A C57 H57C . . 109.5 ?
H57B C57 H57C . . 109.5 ?
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 . 1.347(5) ?
O1 H1 . 0.91(3) ?
O2 N6 . 1.221(5) ?
O3 N6 . 1.217(5) ?
N1 C7 . 1.290(5) ?
N1 C10 . 1.395(5) ?
N2 C10 . 1.376(5) ?
N2 N3 . 1.377(4) ?
N2 C15 . 1.417(5) ?
N3 C8 . 1.330(5) ?
N4 N5 . 1.259(4) ?
N4 C4 . 1.428(5) ?
N5 C21 . 1.434(5) ?
N6 C18 . 1.472(5) ?
C1 C6 . 1.399(5) ?
C1 C2 . 1.402(5) ?
C2 C3 . 1.404(5) ?
C2 C7 . 1.449(5) ?
C3 C4 . 1.378(5) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.404(6) ?
C5 C6 . 1.375(6) ?
C5 H5 . 0.9500 ?
C6 H6 . 0.9500 ?
C7 H7 . 0.9500 ?
C8 C9 . 1.411(5) ?
C8 C11 . 1.519(5) ?
C9 C10 . 1.369(5) ?
C9 H9 . 0.9500 ?
C11 C13 . 1.525(7) ?
C11 C12 . 1.525(6) ?
C11 C14 . 1.538(6) ?
C12 H12A . 0.9800 ?
C12 H12B . 0.9800 ?
C12 H12C . 0.9800 ?
C13 H13A . 0.9800 ?
C13 H13B . 0.9800 ?
C13 H13C . 0.9800 ?
C14 H14A . 0.9800 ?
C14 H14B . 0.9800 ?
C14 H14C . 0.9800 ?
C15 C20 . 1.385(6) ?
C15 C16 . 1.388(5) ?
C16 C17 . 1.391(6) ?
C16 H16 . 0.9500 ?
C17 C18 . 1.376(6) ?
C17 H17 . 0.9500 ?
C18 C19 . 1.374(6) ?
C19 C20 . 1.399(6) ?
C19 H19 . 0.9500 ?
C20 H20 . 0.9500 ?
C21 C22 . 1.383(6) ?
C21 C26 . 1.387(6) ?
C22 C23 . 1.383(6) ?
C22 H22 . 0.9500 ?
C23 C24 . 1.396(6) ?
C23 H23 . 0.9500 ?
C24 C25 . 1.383(7) ?
C24 C27 . 1.516(6) ?
C25 C26 . 1.380(7) ?
C25 H25 . 0.9500 ?
C26 H26 . 0.9500 ?
C27 H27A . 0.9800 ?
C27 H27B . 0.9800 ?
C27 H27C . 0.9800 ?
O21 C31 . 1.355(5) ?
O21 H21 . 0.91(3) ?
O22 N26 . 1.228(4) ?
O23 N26 . 1.224(5) ?
N21 C37 . 1.285(5) ?
N21 C40 . 1.393(5) ?
N22 N23 . 1.371(4) ?
N22 C40 . 1.392(5) ?
N22 C45 . 1.410(5) ?
N23 C38 . 1.336(5) ?
N24 N25 . 1.260(5) ?
N24 C34 . 1.430(5) ?
N25 C51 . 1.416(6) ?
N26 C48 . 1.461(5) ?
C31 C36 . 1.387(5) ?
C31 C32 . 1.407(6) ?
C32 C33 . 1.397(6) ?
C32 C37 . 1.442(5) ?
C33 C34 . 1.381(5) ?
C33 H33 . 0.9500 ?
C34 C35 . 1.400(6) ?
C35 C36 . 1.385(6) ?
C35 H35 . 0.9500 ?
C36 H36 . 0.9500 ?
C37 H37 . 0.9500 ?
C38 C39 . 1.408(6) ?
C38 C41 . 1.511(6) ?
C39 C40 . 1.373(6) ?
C39 H39 . 0.9500 ?
C41 C43 . 1.528(7) ?
C41 C44 . 1.530(7) ?
C41 C42 . 1.532(6) ?
C42 H42A . 0.9800 ?
C42 H42B . 0.9800 ?
C42 H42C . 0.9800 ?
C43 H43A . 0.9800 ?
C43 H43B . 0.9800 ?
C43 H43C . 0.9800 ?
C44 H44A . 0.9800 ?
C44 H44B . 0.9800 ?
C44 H44C . 0.9800 ?
C45 C46 . 1.380(5) ?
C45 C50 . 1.390(6) ?
C46 C47 . 1.384(6) ?
C46 H46 . 0.9500 ?
C47 C48 . 1.378(6) ?
C47 H47 . 0.9500 ?
C48 C49 . 1.381(6) ?
C49 C50 . 1.380(6) ?
C49 H49 . 0.9500 ?
C50 H50 . 0.9500 ?
C51 C56 . 1.390(6) ?
C51 C52 . 1.397(6) ?
C52 C53 . 1.389(6) ?
C52 H52 . 0.9500 ?
C53 C54 . 1.395(6) ?
C53 H53 . 0.9500 ?
C54 C55 . 1.381(7) ?
C54 C57 . 1.507(7) ?
C55 C56 . 1.387(6) ?
C55 H55 . 0.9500 ?
C56 H56 . 0.9500 ?
C57 H57A . 0.9800 ?
C57 H57B . 0.9800 ?
C57 H57C . 0.9800 ?
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
O1 H1 N1 . 0.91(3) 1.78(4) 2.606(4) 150(5)
C3 H3 O23 4_565 0.95 2.64 3.457(6) 144.4
C7 H7 O23 4_565 0.95 2.35 3.232(5) 153.9
C16 H16 O21 . 0.95 2.55 3.181(5) 123.7
O21 H21 N21 . 0.91(3) 1.79(4) 2.612(4) 149(5)
C33 H33 O22 4_565 0.95 2.61 3.351(5) 135.5
C37 H37 O3 4_565 0.95 2.49 3.287(6) 141.1
C46 H46 N3 . 0.95 2.59 3.439(5) 148.4
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
C10 N2 N3 C8 . . . . -2.0(4) ?
C15 N2 N3 C8 . . . . -178.0(4) ?
C4 N4 N5 C21 . . . . -177.9(3) ?
O1 C1 C2 C3 . . . . -178.8(4) ?
C6 C1 C2 C3 . . . . 2.4(6) ?
O1 C1 C2 C7 . . . . 2.0(6) ?
C6 C1 C2 C7 . . . . -176.7(4) ?
C1 C2 C3 C4 . . . . -0.9(6) ?
C7 C2 C3 C4 . . . . 178.3(4) ?
C2 C3 C4 C5 . . . . -1.0(6) ?
C2 C3 C4 N4 . . . . 179.6(4) ?
N5 N4 C4 C3 . . . . -174.9(4) ?
N5 N4 C4 C5 . . . . 5.7(6) ?
C3 C4 C5 C6 . . . . 1.4(6) ?
N4 C4 C5 C6 . . . . -179.3(4) ?
C4 C5 C6 C1 . . . . 0.2(7) ?
O1 C1 C6 C5 . . . . 179.1(4) ?
C2 C1 C6 C5 . . . . -2.1(6) ?
C10 N1 C7 C2 . . . . 178.3(3) ?
C1 C2 C7 N1 . . . . 0.3(6) ?
C3 C2 C7 N1 . . . . -178.9(4) ?
N2 N3 C8 C9 . . . . 1.1(5) ?
N2 N3 C8 C11 . . . . 177.5(4) ?
N3 C8 C9 C10 . . . . 0.2(5) ?
C11 C8 C9 C10 . . . . -176.0(4) ?
C8 C9 C10 N2 . . . . -1.4(4) ?
C8 C9 C10 N1 . . . . 175.5(4) ?
N3 N2 C10 C9 . . . . 2.1(4) ?
C15 N2 C10 C9 . . . . 177.7(4) ?
N3 N2 C10 N1 . . . . -175.3(3) ?
C15 N2 C10 N1 . . . . 0.2(6) ?
C7 N1 C10 C9 . . . . -3.6(7) ?
C7 N1 C10 N2 . . . . 173.0(4) ?
N3 C8 C11 C13 . . . . 142.8(4) ?
C9 C8 C11 C13 . . . . -41.4(6) ?
N3 C8 C11 C12 . . . . 22.2(6) ?
C9 C8 C11 C12 . . . . -162.0(4) ?
N3 C8 C11 C14 . . . . -97.3(5) ?
C9 C8 C11 C14 . . . . 78.5(6) ?
C10 N2 C15 C20 . . . . -141.7(4) ?
N3 N2 C15 C20 . . . . 33.5(5) ?
C10 N2 C15 C16 . . . . 40.1(6) ?
N3 N2 C15 C16 . . . . -144.7(4) ?
C20 C15 C16 C17 . . . . 2.3(6) ?
N2 C15 C16 C17 . . . . -179.5(4) ?
C15 C16 C17 C18 . . . . -1.3(6) ?
C16 C17 C18 C19 . . . . 0.0(6) ?
C16 C17 C18 N6 . . . . -179.9(4) ?
O3 N6 C18 C19 . . . . 5.4(6) ?
O2 N6 C18 C19 . . . . -174.8(4) ?
O3 N6 C18 C17 . . . . -174.7(4) ?
O2 N6 C18 C17 . . . . 5.2(6) ?
C17 C18 C19 C20 . . . . 0.2(7) ?
N6 C18 C19 C20 . . . . -179.9(4) ?
C16 C15 C20 C19 . . . . -2.1(6) ?
N2 C15 C20 C19 . . . . 179.7(4) ?
C18 C19 C20 C15 . . . . 0.8(6) ?
N4 N5 C21 C22 . . . . 1.4(6) ?
N4 N5 C21 C26 . . . . 179.6(4) ?
C26 C21 C22 C23 . . . . 0.9(7) ?
N5 C21 C22 C23 . . . . 179.0(4) ?
C21 C22 C23 C24 . . . . -0.3(7) ?
C22 C23 C24 C25 . . . . -0.4(7) ?
C22 C23 C24 C27 . . . . 179.3(4) ?
C23 C24 C25 C26 . . . . 0.4(7) ?
C27 C24 C25 C26 . . . . -179.2(5) ?
C24 C25 C26 C21 . . . . 0.2(8) ?
C22 C21 C26 C25 . . . . -0.9(7) ?
N5 C21 C26 C25 . . . . -179.2(4) ?
C40 N22 N23 C38 . . . . 0.5(4) ?
C45 N22 N23 C38 . . . . 172.5(4) ?
C34 N24 N25 C51 . . . . -178.7(3) ?
O21 C31 C32 C33 . . . . 178.0(4) ?
C36 C31 C32 C33 . . . . -2.3(6) ?
O21 C31 C32 C37 . . . . -0.6(6) ?
C36 C31 C32 C37 . . . . 179.1(4) ?
C31 C32 C33 C34 . . . . 0.2(6) ?
C37 C32 C33 C34 . . . . 178.8(4) ?
C32 C33 C34 C35 . . . . 1.6(7) ?
C32 C33 C34 N24 . . . . -177.9(4) ?
N25 N24 C34 C33 . . . . 173.9(4) ?
N25 N24 C34 C35 . . . . -5.5(6) ?
C33 C34 C35 C36 . . . . -1.3(6) ?
N24 C34 C35 C36 . . . . 178.1(4) ?
C34 C35 C36 C31 . . . . -0.8(6) ?
O21 C31 C36 C35 . . . . -177.6(4) ?
C32 C31 C36 C35 . . . . 2.6(6) ?
C40 N21 C37 C32 . . . . 174.5(4) ?
C33 C32 C37 N21 . . . . -178.0(4) ?
C31 C32 C37 N21 . . . . 0.6(6) ?
N22 N23 C38 C39 . . . . 0.3(5) ?
N22 N23 C38 C41 . . . . -178.6(4) ?
N23 C38 C39 C40 . . . . -1.0(5) ?
C41 C38 C39 C40 . . . . 177.8(4) ?
C38 C39 C40 N22 . . . . 1.2(5) ?
C38 C39 C40 N21 . . . . -171.7(4) ?
N23 N22 C40 C39 . . . . -1.1(5) ?
C45 N22 C40 C39 . . . . -172.4(4) ?
N23 N22 C40 N21 . . . . 172.9(3) ?
C45 N22 C40 N21 . . . . 1.6(6) ?
C37 N21 C40 C39 . . . . -18.7(7) ?
C37 N21 C40 N22 . . . . 169.1(4) ?
N23 C38 C41 C43 . . . . 108.4(5) ?
C39 C38 C41 C43 . . . . -70.2(6) ?
N23 C38 C41 C44 . . . . -132.3(5) ?
C39 C38 C41 C44 . . . . 49.0(6) ?
N23 C38 C41 C42 . . . . -10.9(6) ?
C39 C38 C41 C42 . . . . 170.4(4) ?
N23 N22 C45 C46 . . . . 152.7(4) ?
C40 N22 C45 C46 . . . . -36.8(6) ?
N23 N22 C45 C50 . . . . -27.5(6) ?
C40 N22 C45 C50 . . . . 143.0(4) ?
C50 C45 C46 C47 . . . . -6.3(6) ?
N22 C45 C46 C47 . . . . 173.4(4) ?
C45 C46 C47 C48 . . . . 2.3(6) ?
C46 C47 C48 C49 . . . . 2.5(7) ?
C46 C47 C48 N26 . . . . -176.3(4) ?
O23 N26 C48 C47 . . . . 175.1(4) ?
O22 N26 C48 C47 . . . . -4.2(6) ?
O23 N26 C48 C49 . . . . -3.7(6) ?
O22 N26 C48 C49 . . . . 177.0(4) ?
C47 C48 C49 C50 . . . . -3.1(7) ?
N26 C48 C49 C50 . . . . 175.7(4) ?
C48 C49 C50 C45 . . . . -1.0(7) ?
C46 C45 C50 C49 . . . . 5.6(6) ?
N22 C45 C50 C49 . . . . -174.1(4) ?
N24 N25 C51 C56 . . . . -167.0(4) ?
N24 N25 C51 C52 . . . . 14.5(6) ?
C56 C51 C52 C53 . . . . 0.7(7) ?
N25 C51 C52 C53 . . . . 179.2(4) ?
C51 C52 C53 C54 . . . . 1.2(7) ?
C52 C53 C54 C55 . . . . -1.8(7) ?
C52 C53 C54 C57 . . . . 178.8(4) ?
C53 C54 C55 C56 . . . . 0.6(7) ?
C57 C54 C55 C56 . . . . 180.0(4) ?
C54 C55 C56 C51 . . . . 1.3(7) ?
C52 C51 C56 C55 . . . . -1.9(6) ?
N25 C51 C56 C55 . . . . 179.5(4) ?
_cod_database_fobs_code 2023562