#------------------------------------------------------------------------------
#$Date: 2021-02-23 11:08:08 +0200 (Tue, 23 Feb 2021) $
#$Revision: 262155 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/23/2022330.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_2022330
loop_
_publ_author_name
'Fidan, Ismail'
'Onal, Emel'
'Hirel, Catherine'
_publ_section_title
;
Nitroxide radicals appended to phthalonitriles: synthesis, structural
characterization and photophysical properties
;
_journal_coeditor_code EP3013
_journal_issue 3
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229621001832
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac 'C21 H19 N4 O3'
_chemical_formula_moiety 'C21 H19 N4 O3'
_chemical_formula_sum 'C21 H19 N4 O3'
_chemical_formula_weight 375.40
_chemical_name_systematic
4-[4-(4,4,5,5-Tetramethyl-2-imidazoline-3-oxide-1-oxyl-2-yl)phenoxy]benzene-1,2-dicarbonitrile
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 90
_cell_angle_beta 108.434(14)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.575(3)
_cell_length_b 17.149(5)
_cell_length_c 10.615(3)
_cell_measurement_reflns_used 1457
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 21.94
_cell_measurement_theta_min 2.34
_cell_volume 1826.3(9)
_computing_cell_refinement
;
APEX2 (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009), PLATON (Spek, 2009,
2015) and Mercury (Macrae
et al., 2020)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 173.15
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'multilayer QUAZAR mirrors'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0840
_diffrn_reflns_av_unetI/netI 0.0791
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 12874
_diffrn_reflns_theta_full 25.066
_diffrn_reflns_theta_max 25.066
_diffrn_reflns_theta_min 2.030
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.094
_exptl_absorpt_correction_T_max 0.992
_exptl_absorpt_correction_T_min 0.983
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.365
_exptl_crystal_description plate
_exptl_crystal_F_000 788
_exptl_crystal_size_max 0.237
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.082
_refine_diff_density_max 0.300
_refine_diff_density_min -0.258
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.061
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 257
_refine_ls_number_reflns 3237
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.061
_refine_ls_R_factor_all 0.1115
_refine_ls_R_factor_gt 0.0631
_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^)+(0.0704P)^2^+1.1450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1539
_refine_ls_wR_factor_ref 0.1768
_reflns_number_gt 1988
_reflns_number_total 3237
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ep3013sup1.cif
_cod_data_source_block I
_cod_database_code 2022330
_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 0.978
_shelx_estimated_absorpt_t_max 0.992
_shelx_hkl_file
;
-1 0 0 87.79 4.50
2 0 0 72.49 3.10
-2 0 0 70.79 3.10
-2 0 0 70.39 4.90
3 0 0 116.39 4.90
-3 0 0 117.49 5.00
-3 0 0 113.59 7.40
4 0 0 313.27 12.80
-4 0 0 329.57 16.50
-4 0 0 328.07 12.90
5 0 0 52.39 2.80
-5 0 0 53.59 6.70
-6 0 0 52.29 7.20
-7 0 0 100.99 10.90
-8 0 0 3.90 4.40
-9 0 0 65.79 10.60
-10 0 0 51.19 10.20
11 0 0 2.40 5.80
-11 0 0 5.80 5.70
-11 1 0 0.10 5.90
11 -1 0 -5.10 4.40
-10 1 0 0.80 3.90
10 -1 0 9.00 5.10
-9 1 0 -0.20 3.90
9 -1 0 1.90 4.10
-8 1 0 4.00 4.60
8 -1 0 -1.60 3.90
-7 1 0 -0.50 3.00
7 -1 0 2.40 1.60
-6 1 0 -5.30 1.80
6 -1 0 0.50 1.20
-5 1 0 5.10 3.40
5 -1 0 1.10 1.10
-4 1 0 -2.00 2.30
4 -1 0 0.80 1.00
-3 1 0 -0.40 1.80
3 -1 0 0.00 1.00
-2 1 0 0.10 1.00
-2 1 0 1.00 1.80
2 -1 0 3.30 2.30
2 -1 0 1.00 1.10
-1 1 0 -1.00 0.80
-1 1 0 1.50 1.30
-1 1 0 0.80 1.10
1 -1 0 0.70 1.00
1 -1 0 -3.90 1.30
0 1 0 -0.10 0.80
0 1 0 0.20 0.50
0 -1 0 -0.40 0.70
0 -1 0 -0.20 0.60
1 1 0 1.30 0.70
1 1 0 0.50 1.40
-1 -1 0 0.70 0.70
-1 -1 0 0.50 0.70
2 1 0 0.10 0.50
-2 -1 0 0.30 0.60
-2 -1 0 0.60 1.20
-3 -1 0 -0.40 1.40
-4 -1 0 -0.40 2.10
-5 -1 0 -2.60 1.50
-6 -1 0 3.70 2.70
-7 -1 0 0.70 2.40
-8 -1 0 0.40 3.80
-9 -1 0 3.60 3.90
-10 -1 0 -1.50 3.90
-11 -1 0 3.00 5.20
-12 -1 0 2.60 6.20
-11 2 0 5.50 6.30
11 -2 0 5.70 6.40
-10 2 0 53.29 11.50
10 -2 0 55.29 11.10
-9 2 0 235.48 19.30
9 -2 0 226.08 18.00
-8 2 0 200.08 16.60
8 -2 0 173.88 14.90
-7 2 0 113.59 12.90
7 -2 0 128.29 12.80
7 -2 0 110.39 7.60
-6 2 0 14.80 5.40
6 -2 0 13.20 5.20
6 -2 0 18.50 3.00
-5 2 0 224.58 14.90
5 -2 0 243.08 11.50
5 -2 0 226.98 14.60
-4 2 0 383.86 20.40
4 -2 0 393.16 17.40
4 -2 0 417.36 20.50
-3 2 0 319.87 17.00
3 -2 0 354.16 14.90
3 -2 0 305.17 16.70
-2 2 0 4489.95 169.28
2 -2 0 4304.97 168.88
2 -2 0 4353.16 167.38
-1 2 0 167.48 9.30
-1 2 0 175.08 9.40
1 -2 0 166.18 8.50
1 -2 0 180.08 9.40
0 2 0 42.10 4.20
0 2 0 35.40 3.40
0 -2 0 36.30 3.30
0 -2 0 33.70 3.10
1 2 0 1146.79 45.30
-1 -2 0 1106.89 44.00
2 2 0 114.59 8.20
-2 -2 0 93.99 5.20
-2 -2 0 102.69 5.80
3 2 0 11.30 3.80
3 2 0 10.00 1.60
-3 -2 0 6.50 2.10
-3 -2 0 10.80 1.60
4 2 0 13.30 1.50
-4 -2 0 16.60 3.10
-4 -2 0 13.00 1.50
-5 -2 0 45.30 5.60
-6 -2 0 24.20 4.80
-7 -2 0 19.40 5.30
-8 -2 0 113.29 12.50
-9 -2 0 461.35 26.70
-10 -2 0 69.69 11.70
-11 -2 0 1.40 6.10
-12 -2 0 3.40 6.90
-10 3 0 -0.10 6.00
10 -3 0 -1.20 6.40
-9 3 0 7.70 6.70
9 -3 0 8.10 6.90
-8 3 0 0.50 4.10
8 -3 0 -8.80 4.10
-7 3 0 0.50 3.80
7 -3 0 1.10 2.60
7 -3 0 3.50 4.50
-6 3 0 3.30 4.40
6 -3 0 0.00 2.10
6 -3 0 4.50 4.40
-5 3 0 -4.20 2.40
5 -3 0 1.80 2.00
5 -3 0 4.90 3.50
-4 3 0 2.20 2.80
4 -3 0 1.60 2.80
4 -3 0 -0.70 1.70
-3 3 0 1.70 3.00
3 -3 0 -3.50 2.10
3 -3 0 0.80 1.90
-2 3 0 1.00 2.40
2 -3 0 1.90 2.00
2 -3 0 -2.30 2.30
-1 3 0 1.50 2.10
-1 3 0 -0.80 1.70
1 -3 0 0.00 2.00
1 -3 0 0.70 2.00
0 3 0 1.00 1.50
0 3 0 0.40 2.10
0 -3 0 2.50 1.80
0 -3 0 1.20 1.80
1 3 0 -3.20 2.30
1 3 0 4.40 2.20
-1 -3 0 1.00 2.30
-1 -3 0 4.50 2.00
2 3 0 -0.60 2.50
-2 -3 0 1.50 1.80
3 3 0 1.50 2.80
-3 -3 0 -1.60 1.30
-3 -3 0 -0.20 1.40
4 3 0 -2.50 3.00
-4 -3 0 -0.20 1.20
-4 -3 0 2.90 1.90
-5 -3 0 -0.50 1.90
-5 -3 0 -1.70 1.00
6 3 0 -0.60 0.80
-6 -3 0 -1.00 1.40
-6 -3 0 0.60 0.90
-6 -3 0 1.00 2.20
-7 -3 0 -3.50 1.90
-8 -3 0 -1.30 2.70
-9 -3 0 -2.20 3.10
-10 -3 0 -2.50 4.00
-11 -3 0 -1.60 5.00
-12 -3 0 -7.70 3.90
-10 4 0 -1.70 6.60
10 -4 0 8.00 7.80
-9 4 0 2.90 5.60
9 -4 0 -1.00 5.80
-8 4 0 5.70 6.20
8 -4 0 8.50 5.90
-7 4 0 8.10 4.80
7 -4 0 4.50 4.50
-6 4 0 -1.50 3.30
6 -4 0 -3.80 3.60
6 -4 0 2.40 2.60
-5 4 0 30.00 7.00
5 -4 0 33.80 6.80
5 -4 0 39.70 5.30
-4 4 0 116.19 10.60
4 -4 0 123.99 12.10
4 -4 0 115.49 8.00
-3 4 0 -1.80 2.30
3 -4 0 -3.40 2.20
3 -4 0 -0.90 2.20
-2 4 0 59.39 7.90
2 -4 0 72.29 5.80
2 -4 0 70.49 7.30
-1 4 0 16.40 4.30
1 -4 0 24.80 3.90
1 -4 0 17.60 3.60
0 4 0 5.70 2.90
0 4 0 8.90 2.60
0 -4 0 3.30 2.30
0 -4 0 11.50 2.50
1 4 0 11.30 3.30
1 4 0 6.00 2.40
-1 -4 0 8.70 2.40
-1 -4 0 5.10 2.30
2 4 0 49.50 6.70
-2 -4 0 52.69 5.20
3 4 0 277.97 16.60
-3 -4 0 295.07 13.80
-3 -4 0 261.37 13.10
4 4 0 715.03 33.90
-4 -4 0 703.33 29.00
-4 -4 0 672.33 30.10
5 4 0 192.48 15.00
-5 -4 0 218.48 10.40
-5 -4 0 197.98 11.90
-6 -4 0 -1.60 1.30
-6 -4 0 0.40 2.50
-7 -4 0 9.60 1.90
-7 -4 0 10.20 3.70
-8 -4 0 172.28 13.00
-9 -4 0 156.68 13.70
-10 -4 0 182.68 15.50
-11 -4 0 78.79 12.50
-12 -4 0 1.70 5.20
-9 5 0 -6.50 6.10
9 -5 0 2.00 6.00
-8 5 0 1.50 6.70
8 -5 0 -3.20 4.60
-7 5 0 -3.90 5.00
7 -5 0 -0.80 4.40
-6 5 0 0.00 4.20
6 -5 0 4.40 4.60
6 -5 0 5.40 3.50
-5 5 0 11.30 5.40
5 -5 0 3.90 3.20
5 -5 0 11.30 5.00
-4 5 0 7.70 4.80
4 -5 0 0.50 2.50
4 -5 0 -0.50 3.30
-3 5 0 -0.60 3.70
3 -5 0 -2.50 2.30
3 -5 0 2.30 2.90
-2 5 0 -1.80 2.40
2 -5 0 -4.00 1.70
2 -5 0 -1.00 2.10
-1 5 0 1.30 3.10
1 -5 0 2.00 2.40
1 -5 0 -1.90 2.40
0 5 0 0.30 3.20
0 5 0 3.20 2.30
0 -5 0 4.50 2.90
0 -5 0 -0.10 1.80
1 5 0 5.50 2.90
1 5 0 3.80 2.70
-1 -5 0 2.10 2.40
-1 -5 0 0.60 2.00
2 5 0 6.30 3.60
2 5 0 -0.60 1.70
-2 -5 0 1.30 1.90
3 5 0 2.40 3.30
-3 -5 0 3.00 2.30
4 5 0 2.90 4.00
-4 -5 0 0.60 1.70
-4 -5 0 -0.70 2.30
5 5 0 -1.30 3.40
-5 -5 0 2.00 2.10
-5 -5 0 0.60 1.70
6 5 0 3.00 5.50
-6 -5 0 -1.90 1.60
-6 -5 0 0.50 2.70
-7 -5 0 1.70 2.60
-7 -5 0 3.10 1.90
-8 -5 0 -3.60 3.00
-9 -5 0 1.10 4.20
-10 -5 0 0.10 3.40
-11 -5 0 3.80 4.20
-12 -5 0 -2.30 4.10
-8 6 0 -2.50 6.70
-7 6 0 74.59 13.30
7 -6 0 59.99 10.90
-6 6 0 81.59 12.60
6 -6 0 71.69 8.70
-5 6 0 59.59 11.10
5 -6 0 49.60 8.70
5 -6 0 64.49 8.40
-4 6 0 13.70 5.90
4 -6 0 21.60 5.80
4 -6 0 15.00 4.60
-3 6 0 218.28 16.50
3 -6 0 226.78 15.20
3 -6 0 204.78 13.30
-2 6 0 17.20 5.80
2 -6 0 25.70 5.40
2 -6 0 26.70 5.10
-1 6 0 22.80 5.60
1 -6 0 28.80 5.50
1 -6 0 39.70 6.20
0 6 0 9.90 3.80
0 -6 0 6.50 2.90
0 -6 0 13.90 4.00
1 6 0 57.29 8.00
1 6 0 54.99 6.60
-1 -6 0 65.99 7.00
-1 -6 0 45.60 5.60
2 6 0 33.60 5.00
2 6 0 36.90 6.60
-2 -6 0 24.90 4.00
-2 -6 0 33.10 5.20
3 6 0 184.18 13.90
3 6 0 165.38 10.50
-3 -6 0 175.28 11.00
4 6 0 67.09 10.30
-4 -6 0 75.49 6.60
-4 -6 0 63.69 6.00
5 6 0 31.30 7.40
-5 -6 0 19.30 4.00
-5 -6 0 27.80 4.80
6 6 0 106.49 14.40
-6 -6 0 108.39 9.20
-6 -6 0 101.19 7.50
7 6 0 138.49 16.30
-7 -6 0 98.79 9.30
-7 -6 0 98.79 7.30
-8 -6 0 133.99 11.60
-8 -6 0 134.49 9.70
-9 -6 0 35.60 7.50
-10 -6 0 -3.50 3.20
-11 -6 0 1.90 4.30
-12 -6 0 2.50 5.10
-7 7 0 64.29 13.40
-6 7 0 -5.50 4.90
6 -7 0 -1.20 4.00
-5 7 0 -6.50 5.10
5 -7 0 5.00 4.30
5 -7 0 9.30 6.20
-4 7 0 3.00 5.60
4 -7 0 15.10 5.90
4 -7 0 5.60 4.10
-3 7 0 1.70 4.40
3 -7 0 4.60 3.40
3 -7 0 3.70 3.80
-2 7 0 -1.10 4.30
2 -7 0 1.00 3.00
2 -7 0 3.90 3.40
-1 7 0 -0.20 3.20
1 -7 0 1.50 3.60
1 -7 0 -1.00 3.10
0 7 0 0.20 4.00
0 -7 0 -4.30 2.80
0 -7 0 -0.70 2.80
1 7 0 -1.30 3.10
-1 -7 0 2.50 2.60
-1 -7 0 3.40 2.90
2 7 0 -2.80 2.70
2 7 0 -1.30 2.10
-2 -7 0 -1.30 1.70
-2 -7 0 0.40 2.60
3 7 0 -1.90 2.70
3 7 0 -1.30 3.20
-3 -7 0 2.50 2.50
4 7 0 0.10 4.80
4 7 0 -1.20 2.30
-4 -7 0 3.20 2.50
5 7 0 1.00 5.50
-5 -7 0 -0.40 2.70
-5 -7 0 1.20 2.80
6 7 0 2.20 6.10
-6 -7 0 -3.30 2.10
-6 -7 0 -0.40 2.80
7 7 0 -1.80 5.10
-7 -7 0 7.50 3.10
-7 -7 0 1.00 2.80
8 7 0 3.80 5.70
-8 -7 0 -2.70 2.80
-8 -7 0 5.90 2.90
-9 -7 0 5.30 4.10
-10 -7 0 -2.10 3.20
-11 -7 0 7.00 5.90
-12 -7 0 3.60 4.70
-6 8 0 31.70 11.20
6 -8 0 31.60 7.00
5 -8 0 160.38 13.60
-4 8 0 0.10 5.50
4 -8 0 11.20 4.60
-3 8 0 67.09 11.10
3 -8 0 71.99 9.40
-2 8 0 7.10 5.70
2 -8 0 1.70 3.60
-1 8 0 -1.30 4.70
1 -8 0 -2.20 3.90
0 8 0 0.90 3.90
0 -8 0 7.60 4.40
0 -8 0 0.70 4.00
1 8 0 14.40 6.50
-1 -8 0 28.50 5.80
-1 -8 0 30.10 8.30
2 8 0 17.10 6.10
-2 -8 0 6.60 3.90
3 8 0 6.30 4.70
-3 -8 0 4.80 3.30
4 8 0 29.40 8.90
-4 -8 0 21.20 4.80
5 8 0 20.90 7.60
-5 -8 0 34.60 5.80
-5 -8 0 20.70 5.20
6 8 0 608.34 35.30
-6 -8 0 572.04 27.90
-6 -8 0 588.34 29.20
7 8 0 80.59 13.50
-7 -8 0 82.29 10.00
-7 -8 0 87.89 9.10
8 8 0 32.40 10.70
-8 -8 0 41.50 6.00
-8 -8 0 16.40 6.00
-9 -8 0 5.80 4.30
-10 -8 0 6.50 5.00
-11 -8 0 21.20 8.00
-5 9 0 2.60 6.40
5 -9 0 2.60 5.10
-4 9 0 -13.70 5.40
4 -9 0 10.40 4.80
-3 9 0 3.40 6.70
3 -9 0 -1.30 4.00
-2 9 0 1.50 6.20
2 -9 0 -2.00 3.50
-1 9 0 -3.40 4.40
1 -9 0 9.40 4.90
0 9 0 -10.20 5.10
0 -9 0 -0.40 4.40
1 9 0 6.00 5.40
-1 -9 0 -2.80 2.80
2 9 0 -3.40 5.20
-2 -9 0 -0.80 3.20
3 9 0 2.50 6.00
-3 -9 0 -0.80 3.40
4 9 0 -3.80 5.60
-4 -9 0 2.20 3.60
5 9 0 -0.90 4.90
-5 -9 0 6.80 4.10
-5 -9 0 0.70 2.90
6 9 0 2.60 7.60
-6 -9 0 5.50 3.90
-6 -9 0 -1.80 3.40
7 9 0 4.60 7.60
-7 -9 0 2.30 3.70
-7 -9 0 3.90 4.40
8 9 0 -5.70 5.30
-8 -9 0 2.20 3.30
-8 -9 0 -3.50 2.90
9 9 0 -4.80 6.70
-9 -9 0 -0.40 3.80
-10 -9 0 1.50 4.60
-11 -9 0 -5.50 4.80
-4 10 0 47.20 12.40
4 -10 0 62.69 10.70
3 -10 0 41.60 9.00
2 -10 0 139.29 15.00
-1 10 0 76.09 12.80
1 -10 0 101.79 12.40
0 10 0 -3.00 4.40
0 -10 0 -0.10 3.90
1 10 0 18.00 8.50
-1 -10 0 21.30 6.20
2 10 0 6.80 7.30
-2 -10 0 6.20 4.20
3 10 0 7.60 6.10
-3 -10 0 -1.50 3.90
4 10 0 406.16 29.10
-4 -10 0 466.55 25.10
5 10 0 45.10 11.20
-5 -10 0 55.29 8.70
-5 -10 0 35.10 6.80
6 10 0 -2.40 5.60
-6 -10 0 -0.20 3.00
-6 -10 0 7.50 4.60
7 10 0 5.40 8.70
-7 -10 0 11.10 5.20
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-2 2 17 -1.10 6.10
3 -2 -17 44.30 10.10
-3 2 17 43.70 11.40
-3 2 17 30.90 9.20
4 -2 -17 6.00 5.80
-4 2 17 8.20 7.20
-4 2 17 8.50 8.50
5 -2 -17 7.40 6.30
-5 2 17 3.50 7.50
-5 2 17 -0.40 5.60
6 1 17 1.40 9.00
5 1 17 3.30 8.70
3 1 17 1.00 7.50
2 1 17 4.90 6.30
1 1 17 3.60 7.70
0 1 17 -5.10 4.80
-1 1 17 3.20 7.50
-2 1 17 -2.40 6.20
-3 1 17 24.90 9.60
-3 1 17 6.30 5.40
4 -1 -17 0.30 4.70
-4 1 17 -3.70 6.80
-4 1 17 -5.30 5.00
5 -1 -17 -1.50 5.90
-5 1 17 1.40 6.30
-5 1 17 4.20 8.00
6 -1 -17 7.70 6.90
-6 1 17 1.60 7.50
-6 1 17 1.20 7.00
6 0 17 4.00 9.50
5 0 17 14.30 7.70
4 0 17 1.60 7.90
3 0 17 -1.20 6.60
2 0 17 -0.30 7.40
1 0 17 4.10 6.60
0 0 17 22.10 7.90
-1 0 17 19.60 9.00
-2 0 17 -3.10 5.90
-3 0 17 18.60 8.50
-4 0 17 0.80 7.10
-5 0 17 14.80 7.60
-5 0 17 10.60 8.10
6 0 -17 7.10 5.40
-6 0 17 0.60 5.80
-6 0 17 2.50 7.70
6 -1 17 -2.90 7.30
5 -1 17 -3.10 5.50
4 -1 17 -5.20 7.50
3 -1 17 10.50 7.40
2 -1 17 0.10 5.30
1 -1 17 14.10 8.40
0 -1 17 -1.20 6.80
-1 -1 17 1.20 5.60
-2 -1 17 3.60 6.70
-3 -1 17 6.20 6.50
-4 -1 17 20.70 8.40
-5 -1 17 6.90 7.80
-6 -1 17 -4.90 8.00
5 -2 17 2.70 8.00
4 -2 17 -7.50 7.00
3 -2 17 12.60 7.30
2 -2 17 5.00 5.80
1 -2 17 10.90 8.60
0 -2 17 8.40 6.60
-1 -2 17 -5.20 6.50
-2 -2 17 -0.90 5.60
-3 -2 17 -4.70 5.10
-4 -2 17 8.90 7.20
-5 -2 17 1.60 5.60
-6 -2 17 -2.00 7.40
5 -3 17 6.10 7.10
4 -3 17 -4.60 5.80
3 -3 17 4.00 8.10
2 -3 17 1.40 7.50
1 -3 17 30.90 9.90
0 -3 17 24.20 9.10
-1 -3 17 15.50 7.70
-2 -3 17 41.40 9.40
-3 -3 17 1.50 5.50
-4 -3 17 1.00 6.60
-5 -3 17 -8.50 5.20
4 -4 17 -3.90 6.10
3 -4 17 4.00 7.40
2 -4 17 5.10 7.00
1 -4 17 -4.00 6.70
0 -4 17 37.00 9.50
-1 -4 17 11.10 6.90
-2 -4 17 -5.00 6.20
-3 -4 17 16.30 7.40
-4 -4 17 13.10 8.40
-5 -4 17 -3.50 5.30
-6 -4 17 2.50 8.10
3 -5 17 0.10 6.70
2 -5 17 0.10 6.90
1 -5 17 13.40 8.50
0 -5 17 31.40 9.20
-1 -5 17 1.30 5.30
-2 -5 17 -0.10 5.60
-3 -5 17 -3.30 5.50
-4 -5 17 7.50 6.60
-5 -5 17 7.20 7.50
-6 -5 17 -4.20 6.70
1 -6 17 -11.30 6.80
0 -6 17 -8.50 7.50
-1 -6 17 8.90 8.30
-2 -6 17 26.20 9.50
-3 -6 17 12.80 7.00
-4 -6 17 14.20 7.60
-5 -6 17 -4.60 5.40
-4 -5 -18 -4.80 5.20
4 5 18 -0.60 8.90
-3 -5 -18 5.30 6.50
3 5 18 6.50 8.90
3 5 18 -7.10 8.30
-2 -5 -18 24.20 7.90
2 5 18 23.70 10.30
2 5 18 29.30 10.00
-1 -5 -18 65.09 12.60
1 5 18 59.99 13.30
0 -5 -18 1.70 6.10
0 5 18 4.60 7.70
0 5 18 5.60 9.30
1 -5 -18 6.90 6.20
-1 5 18 -12.00 7.20
-1 5 18 7.60 8.50
-5 -4 -18 14.50 6.60
5 4 18 20.50 10.70
-4 -4 -18 -0.50 4.80
4 4 18 3.80 9.20
-3 -4 -18 14.20 7.50
3 4 18 14.60 10.30
-2 -4 -18 26.20 8.60
2 4 18 13.40 10.00
-1 -4 -18 1.80 5.40
1 4 18 6.10 8.10
1 4 18 8.80 8.90
0 -4 -18 1.80 6.70
0 4 18 -4.20 7.80
0 4 18 16.10 9.50
1 -4 -18 1.90 5.30
-1 4 18 15.10 8.00
-1 4 18 8.80 7.10
2 -4 -18 -2.20 6.00
-2 4 18 -1.60 7.50
-2 4 18 4.60 6.80
-5 -3 -18 20.10 7.60
5 3 18 -0.20 9.40
-4 -3 -18 -9.30 4.90
4 3 18 5.00 8.00
-3 -3 -18 6.30 6.30
3 3 18 10.30 8.10
-2 -3 -18 12.50 6.30
2 3 18 -0.50 6.90
-1 -3 -18 -2.30 5.50
1 3 18 -7.90 5.20
0 -3 -18 -4.00 4.50
0 3 18 4.70 6.60
1 -3 -18 5.80 6.70
-1 3 18 4.30 6.70
-1 3 18 7.30 8.00
2 -3 -18 12.50 6.20
-2 3 18 7.20 6.90
-2 3 18 -2.90 7.20
3 -3 -18 13.40 7.90
-3 3 18 4.40 8.40
-3 3 18 25.00 9.30
5 2 18 47.80 11.80
4 2 18 7.50 9.00
3 2 18 5.20 8.80
2 2 18 -2.30 7.70
1 2 18 -1.40 7.40
0 2 18 7.60 8.30
1 -2 -18 8.40 6.50
-1 2 18 1.70 6.50
2 -2 -18 12.10 6.90
-2 2 18 1.50 5.90
3 -2 -18 0.80 6.40
-3 2 18 0.60 5.50
-3 2 18 1.90 5.20
4 -2 -18 1.90 7.10
-4 2 18 0.00 6.60
-4 2 18 -2.80 7.20
5 1 18 -2.30 8.50
4 1 18 -5.70 5.70
3 1 18 -0.90 6.30
2 1 18 1.70 6.40
1 1 18 -0.90 6.10
0 1 18 4.70 7.20
-1 1 18 -0.50 5.80
-2 1 18 0.60 6.30
-3 1 18 20.30 9.10
4 -1 -18 6.40 6.50
-4 1 18 -3.30 5.50
5 -1 -18 1.40 6.50
-5 1 18 6.00 7.90
-5 1 18 4.00 7.30
5 0 18 9.00 10.10
4 0 18 -4.50 7.00
3 0 18 23.50 10.00
2 0 18 3.20 7.70
1 0 18 -2.90 7.20
0 0 18 12.90 7.80
-1 0 18 2.90 7.40
-2 0 18 0.80 7.80
-3 0 18 16.30 9.70
-4 0 18 -7.80 7.60
-5 0 18 5.00 8.40
5 -1 18 8.60 9.10
4 -1 18 -1.10 6.10
3 -1 18 -3.20 7.20
2 -1 18 5.70 7.90
1 -1 18 -2.80 5.30
0 -1 18 15.50 8.50
-1 -1 18 -7.70 6.80
-2 -1 18 -3.00 5.40
-3 -1 18 -5.90 5.50
-4 -1 18 -0.70 7.00
-5 -1 18 -7.10 7.30
4 -2 18 -4.10 8.20
3 -2 18 -4.40 6.20
2 -2 18 -7.80 5.50
1 -2 18 5.10 6.40
0 -2 18 -8.90 4.90
-1 -2 18 5.00 6.50
-2 -2 18 1.10 6.10
-3 -2 18 -6.00 5.20
-4 -2 18 -11.40 6.30
-5 -2 18 20.10 8.00
3 -3 18 5.60 9.20
2 -3 18 0.10 7.40
1 -3 18 -5.60 6.70
0 -3 18 -5.70 7.30
-1 -3 18 -3.20 7.20
-2 -3 18 12.50 7.00
-3 -3 18 3.00 6.60
-4 -3 18 1.30 5.70
-5 -3 18 1.90 6.60
2 -4 18 -5.70 7.40
1 -4 18 0.40 7.50
0 -4 18 12.00 7.10
-1 -4 18 2.20 6.20
-2 -4 18 21.40 9.00
-3 -4 18 0.40 5.90
-4 -4 18 11.50 8.60
-5 -4 18 14.20 7.40
1 -5 18 -3.60 6.10
0 -5 18 4.70 8.50
-1 -5 18 40.40 10.50
-2 -5 18 19.20 9.40
-3 -5 18 5.80 6.50
-4 -5 18 -3.40 5.50
-3 -4 -19 5.00 7.20
3 4 19 12.90 10.70
-2 -4 -19 -1.10 5.00
2 4 19 -6.10 6.70
-1 -4 -19 80.79 14.00
1 4 19 60.49 14.00
0 -4 -19 24.30 8.80
0 4 19 19.70 9.40
-4 -3 -19 31.10 9.70
4 3 19 7.10 10.60
-3 -3 -19 -4.20 4.20
3 3 19 12.70 10.10
-2 -3 -19 3.90 7.40
2 3 19 19.50 10.20
-1 -3 -19 44.80 10.60
1 3 19 61.19 14.30
0 -3 -19 46.90 10.60
0 3 19 27.30 11.10
1 -3 -19 -0.50 6.70
-1 3 19 3.70 7.40
2 -3 -19 11.00 8.30
-2 3 19 -0.50 6.70
4 2 19 19.90 12.20
3 2 19 6.80 8.00
2 2 19 1.70 8.90
1 2 19 -0.20 6.50
0 -2 -19 94.29 14.20
0 2 19 9.00 7.70
1 -2 -19 42.50 10.80
-1 2 19 19.30 10.50
2 -2 -19 12.70 7.30
-2 2 19 -5.10 7.60
3 -2 -19 -0.80 6.00
-3 2 19 -3.60 8.00
4 1 19 7.70 8.80
3 1 19 -5.10 7.00
2 1 19 9.20 7.20
1 1 19 -8.40 5.30
0 1 19 -8.60 5.50
-1 1 19 -1.10 5.70
-2 1 19 4.80 7.30
3 -1 -19 -2.30 5.40
-3 1 19 -0.40 6.40
4 0 19 -5.20 8.10
3 0 19 2.50 7.60
2 0 19 2.80 7.40
1 0 19 7.70 8.30
0 0 19 -1.50 8.00
-1 0 19 15.50 7.80
-2 0 19 5.40 8.60
-3 0 19 -5.90 7.30
-4 0 19 1.60 7.30
3 -1 19 0.20 7.00
2 -1 19 1.50 8.80
1 -1 19 3.80 8.40
0 -1 19 4.80 8.70
-1 -1 19 -2.80 5.40
-2 -1 19 -6.50 7.70
-3 -1 19 4.10 7.90
-4 -1 19 2.20 6.40
3 -2 19 10.00 9.00
2 -2 19 8.50 9.00
1 -2 19 2.30 7.30
0 -2 19 19.90 9.40
-1 -2 19 3.80 6.80
-2 -2 19 -12.00 6.90
-3 -2 19 10.00 8.60
-4 -2 19 13.20 10.00
2 -3 19 -3.40 7.70
1 -3 19 -5.70 6.50
0 -3 19 18.00 9.90
-1 -3 19 15.60 9.10
-2 -3 19 -7.90 4.90
-3 -3 19 5.00 8.90
-4 -3 19 17.30 8.20
0 -4 19 4.40 8.40
-1 -4 19 36.90 11.70
-2 -4 19 5.60 8.50
-3 -4 19 2.40 8.20
2 2 20 5.60 10.20
1 2 20 1.10 7.50
0 -2 -20 17.50 9.10
0 2 20 -4.00 7.20
2 1 20 7.10 9.50
1 1 20 7.50 8.30
0 1 20 -6.40 6.30
-1 1 20 -10.50 6.20
2 0 20 -6.80 8.40
1 0 20 0.90 6.90
0 0 20 5.60 7.70
-1 0 20 7.90 7.60
-2 0 20 4.20 7.50
1 -1 20 5.60 8.90
0 -1 20 6.40 8.00
-1 -1 20 3.10 8.90
-2 -1 20 -4.30 6.60
0 -2 20 5.60 8.80
-1 -2 20 6.60 9.30
-2 -2 20 6.70 8.00
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 2354
_shelx_res_file
;
TITL 18gtu060_if_430a_a_a.res in P-1 New:P21/c
18gtu060_if_430a_a_pl.res
created by SHELXL-2018/3 at 11:37:02 on 29-Apr-2019
CELL 0.71073 10.575 17.149 10.615 90 108.434 90
ZERR 4 0.003 0.005 0.003 0 0.014 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 84 76 16 12
L.S. 20
PLAN -5
SIZE 0.082 0.15 0.237
TEMP -100
BOND $H
CONF
fmap 2
acta
REM
REM
REM
WGHT 0.070400 1.145000
FVAR 0.41164
O1 4 0.858394 0.079002 0.586145 11.00000 0.02692 0.05245 =
0.03075 0.00746 0.01580 0.00693
O2 4 0.290596 0.040398 0.693637 11.00000 0.03160 0.04534 =
0.03808 -0.01860 0.01121 -0.00862
O3 4 0.569113 0.215118 0.983429 11.00000 0.03081 0.04741 =
0.03649 -0.01518 0.01027 -0.01283
N5 3 1.248824 0.096415 0.314151 11.00000 0.04262 0.05773 =
0.05308 0.01054 0.02701 0.01081
N6 3 0.977903 0.204976 0.037555 11.00000 0.03617 0.05770 =
0.02872 0.00165 0.00796 -0.00325
N7 3 0.339873 0.087346 0.790626 11.00000 0.02451 0.03100 =
0.02534 -0.00445 0.00840 -0.00118
N8 3 0.473471 0.167003 0.930428 11.00000 0.02247 0.03481 =
0.02692 -0.00142 0.00922 -0.00195
C101 1 1.146550 0.104936 0.327112 11.00000 0.03756 0.03525 =
0.02902 0.00360 0.01393 0.00180
C102 1 0.948804 0.186546 0.128438 11.00000 0.02923 0.03885 =
0.02545 -0.00118 0.00546 -0.00320
C103 1 1.018067 0.119491 0.342408 11.00000 0.02743 0.02658 =
0.02251 -0.00397 0.01118 -0.00192
C104 1 0.921017 0.161757 0.246396 11.00000 0.02686 0.03401 =
0.02043 -0.00614 0.00651 -0.00338
C105 1 0.800840 0.179018 0.266727 11.00000 0.02742 0.03233 =
0.02542 -0.00135 0.00424 -0.00192
AFIX 43
H105 2 0.735443 0.208496 0.202293 11.00000 -1.20000
AFIX 0
C106 1 0.775504 0.153771 0.379598 11.00000 0.02103 0.04135 =
0.03029 -0.00586 0.00685 -0.00221
AFIX 43
H106 2 0.693805 0.166436 0.394219 11.00000 -1.20000
AFIX 0
C107 1 0.870625 0.109770 0.471215 11.00000 0.02783 0.03308 =
0.02264 -0.00240 0.01080 -0.00173
C108 1 0.993302 0.093235 0.454971 11.00000 0.02360 0.03184 =
0.02710 -0.00175 0.00684 0.00057
AFIX 43
H108 2 1.058814 0.064359 0.520326 11.00000 -1.20000
AFIX 0
C109 1 0.751194 0.095162 0.631805 11.00000 0.02691 0.03548 =
0.02818 0.00341 0.01575 0.00392
C110 1 0.620092 0.081519 0.558907 11.00000 0.03029 0.03914 =
0.02434 -0.00061 0.01151 -0.00208
AFIX 43
H110 2 0.596564 0.065001 0.469015 11.00000 -1.20000
AFIX 0
C111 1 0.522826 0.092543 0.620260 11.00000 0.02248 0.03752 =
0.02437 0.00008 0.00456 -0.00047
AFIX 43
H111 2 0.431814 0.083932 0.571168 11.00000 -1.20000
AFIX 0
C112 1 0.556758 0.115872 0.751777 11.00000 0.02404 0.02607 =
0.02282 0.00193 0.00737 0.00319
C113 1 0.691265 0.128672 0.822606 11.00000 0.02714 0.04473 =
0.02365 0.00183 0.00543 -0.00223
AFIX 43
H113 2 0.716074 0.144591 0.912874 11.00000 -1.20000
AFIX 0
C114 1 0.787698 0.118373 0.762483 11.00000 0.02362 0.04063 =
0.02931 0.00167 0.00915 0.00001
AFIX 43
H114 2 0.878847 0.127216 0.810801 11.00000 -1.20000
AFIX 0
C115 1 0.458726 0.124185 0.819988 11.00000 0.02265 0.02800 =
0.02076 -0.00003 0.00532 0.00025
C116 1 0.373131 0.146477 0.998101 11.00000 0.02292 0.03637 =
0.02434 -0.00192 0.00992 0.00039
C117 1 0.259766 0.114167 0.877806 11.00000 0.02638 0.03389 =
0.02808 -0.00020 0.01274 0.00210
C118 1 0.438921 0.085344 1.101681 11.00000 0.04040 0.05743 =
0.02651 0.00565 0.01384 0.00896
AFIX 137
H11A 2 0.520580 0.106914 1.164184 11.00000 -1.50000
H11B 2 0.461049 0.039459 1.057753 11.00000 -1.50000
H11C 2 0.377570 0.070227 1.149917 11.00000 -1.50000
AFIX 0
C119 1 0.336691 0.217828 1.062235 11.00000 0.03471 0.04342 =
0.03834 -0.00997 0.01809 -0.00202
AFIX 137
H11D 2 0.311834 0.260221 0.997127 11.00000 -1.50000
H11E 2 0.413254 0.233953 1.137429 11.00000 -1.50000
H11F 2 0.261308 0.205667 1.093820 11.00000 -1.50000
AFIX 0
C120 1 0.183759 0.046292 0.908006 11.00000 0.03827 0.04341 =
0.04537 -0.00398 0.02236 -0.01220
AFIX 137
H12A 2 0.245343 0.003152 0.944094 11.00000 -1.50000
H12B 2 0.115673 0.029329 0.826294 11.00000 -1.50000
H12C 2 0.140785 0.062212 0.973286 11.00000 -1.50000
AFIX 0
C121 1 0.166680 0.177037 0.801557 11.00000 0.02718 0.04565 =
0.03665 0.00346 0.00998 0.00716
AFIX 137
H12D 2 0.106826 0.155151 0.718881 11.00000 -1.50000
H12E 2 0.218831 0.219520 0.780791 11.00000 -1.50000
H12F 2 0.114003 0.197222 0.855542 11.00000 -1.50000
AFIX 0
HKLF 4 1 -1 0 0 0 0 1 0 1 0
REM 18gtu060_if_430a_a_a.res in P-1 New:P21/c
REM wR2 = 0.1768, GooF = S = 1.061, Restrained GooF = 1.061 for all data
REM R1 = 0.0631 for 1988 Fo > 4sig(Fo) and 0.1115 for all 3237 data
REM 257 parameters refined using 0 restraints
END
WGHT 0.0690 1.1976
REM Highest difference peak 0.300, deepest hole -0.258, 1-sigma level 0.060
Q1 1 1.1208 0.1692 0.0364 11.00000 0.05 0.30
Q2 1 0.3906 0.0376 0.6638 11.00000 0.05 0.26
Q3 1 0.6817 0.1150 0.3617 11.00000 0.05 0.26
Q4 1 0.3489 0.0714 0.6335 11.00000 0.05 0.24
Q5 1 1.0923 0.0392 0.2271 11.00000 0.05 0.22
;
_shelx_res_checksum 74519
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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 0.8584(2) 0.07900(15) 0.5861(2) 0.0351(7) Uani d 1 . .
O O2 0.2906(2) 0.04040(15) 0.6936(2) 0.0383(7) Uani d 1 . .
O O3 0.5691(2) 0.21512(15) 0.9834(2) 0.0383(7) Uani d 1 . .
N N5 1.2488(4) 0.0964(2) 0.3142(3) 0.0484(9) Uani d 1 . .
N N6 0.9779(3) 0.2050(2) 0.0376(3) 0.0414(9) Uani d 1 . .
N N7 0.3399(3) 0.08735(17) 0.7906(3) 0.0268(7) Uani d 1 . .
N N8 0.4735(3) 0.16700(17) 0.9304(3) 0.0277(7) Uani d 1 . .
C C101 1.1465(4) 0.1049(2) 0.3271(3) 0.0331(9) Uani d 1 . .
C C102 0.9488(3) 0.1865(2) 0.1284(3) 0.0319(9) Uani d 1 . .
C C103 1.0181(3) 0.1195(2) 0.3424(3) 0.0247(8) Uani d 1 . .
C C104 0.9210(3) 0.1618(2) 0.2464(3) 0.0273(8) Uani d 1 . .
C C105 0.8008(3) 0.1790(2) 0.2667(3) 0.0294(9) Uani d 1 . .
H H105 0.735443 0.208496 0.202293 0.035 Uiso calc 1 . .
C C106 0.7755(3) 0.1538(2) 0.3796(3) 0.0312(9) Uani d 1 . .
H H106 0.693805 0.166436 0.394219 0.037 Uiso calc 1 . .
C C107 0.8706(3) 0.1098(2) 0.4712(3) 0.0272(8) Uani d 1 . .
C C108 0.9933(3) 0.0932(2) 0.4550(3) 0.0278(8) Uani d 1 . .
H H108 1.058814 0.064359 0.520326 0.033 Uiso calc 1 . .
C C109 0.7512(3) 0.0952(2) 0.6318(3) 0.0285(8) Uani d 1 . .
C C110 0.6201(3) 0.0815(2) 0.5589(3) 0.0306(9) Uani d 1 . .
H H110 0.596564 0.065001 0.469015 0.037 Uiso calc 1 . .
C C111 0.5228(3) 0.0925(2) 0.6203(3) 0.0288(8) Uani d 1 . .
H H111 0.431814 0.083932 0.571168 0.035 Uiso calc 1 . .
C C112 0.5568(3) 0.1159(2) 0.7518(3) 0.0243(8) Uani d 1 . .
C C113 0.6913(3) 0.1287(2) 0.8226(3) 0.0324(9) Uani d 1 . .
H H113 0.716074 0.144591 0.912874 0.039 Uiso calc 1 . .
C C114 0.7877(3) 0.1184(2) 0.7625(3) 0.0310(9) Uani d 1 . .
H H114 0.878847 0.127216 0.810801 0.037 Uiso calc 1 . .
C C115 0.4587(3) 0.1242(2) 0.8200(3) 0.0242(8) Uani d 1 . .
C C116 0.3731(3) 0.1465(2) 0.9981(3) 0.0273(8) Uani d 1 . .
C C117 0.2598(3) 0.1142(2) 0.8778(3) 0.0285(8) Uani d 1 . .
C C118 0.4389(4) 0.0853(2) 1.1017(3) 0.0407(10) Uani d 1 . .
H H11A 0.520580 0.106914 1.164184 0.061 Uiso calc 1 . .
H H11B 0.461049 0.039459 1.057753 0.061 Uiso calc 1 . .
H H11C 0.377570 0.070227 1.149917 0.061 Uiso calc 1 . .
C C119 0.3367(4) 0.2178(2) 1.0622(4) 0.0373(9) Uani d 1 . .
H H11D 0.311834 0.260221 0.997127 0.056 Uiso calc 1 . .
H H11E 0.413254 0.233953 1.137429 0.056 Uiso calc 1 . .
H H11F 0.261308 0.205667 1.093820 0.056 Uiso calc 1 . .
C C120 0.1838(4) 0.0463(2) 0.9080(4) 0.0402(10) Uani d 1 . .
H H12A 0.245343 0.003152 0.944094 0.060 Uiso calc 1 . .
H H12B 0.115673 0.029329 0.826294 0.060 Uiso calc 1 . .
H H12C 0.140785 0.062212 0.973286 0.060 Uiso calc 1 . .
C C121 0.1667(3) 0.1770(2) 0.8016(3) 0.0365(9) Uani d 1 . .
H H12D 0.106826 0.155151 0.718881 0.055 Uiso calc 1 . .
H H12E 0.218831 0.219520 0.780791 0.055 Uiso calc 1 . .
H H12F 0.114003 0.197222 0.855542 0.055 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 0.0269(14) 0.0525(18) 0.0307(14) 0.0069(11) 0.0158(11) 0.0075(12)
O2 0.0316(14) 0.0453(18) 0.0381(15) -0.0086(12) 0.0112(12) -0.0186(13)
O3 0.0308(14) 0.0474(18) 0.0365(14) -0.0128(12) 0.0103(11) -0.0152(13)
N5 0.043(2) 0.058(3) 0.053(2) 0.0108(17) 0.0270(18) 0.0105(18)
N6 0.0362(19) 0.058(2) 0.0287(18) -0.0032(16) 0.0080(14) 0.0016(16)
N7 0.0245(16) 0.0310(18) 0.0253(16) -0.0012(13) 0.0084(12) -0.0044(13)
N8 0.0225(15) 0.0348(19) 0.0269(16) -0.0019(13) 0.0092(12) -0.0014(14)
C101 0.038(2) 0.035(2) 0.029(2) 0.0018(17) 0.0139(17) 0.0036(17)
C102 0.029(2) 0.039(2) 0.025(2) -0.0032(16) 0.0055(16) -0.0012(17)
C103 0.0274(19) 0.027(2) 0.0225(18) -0.0019(15) 0.0112(14) -0.0040(15)
C104 0.027(2) 0.034(2) 0.0204(18) -0.0034(15) 0.0065(14) -0.0061(16)
C105 0.027(2) 0.032(2) 0.0254(19) -0.0019(15) 0.0042(15) -0.0013(16)
C106 0.0210(19) 0.041(2) 0.030(2) -0.0022(16) 0.0069(15) -0.0059(17)
C107 0.028(2) 0.033(2) 0.0226(18) -0.0017(16) 0.0108(15) -0.0024(16)
C108 0.0236(19) 0.032(2) 0.0271(19) 0.0006(15) 0.0068(15) -0.0017(16)
C109 0.027(2) 0.035(2) 0.0282(19) 0.0039(15) 0.0158(15) 0.0034(16)
C110 0.030(2) 0.039(2) 0.0243(18) -0.0021(16) 0.0115(15) -0.0006(16)
C111 0.0225(19) 0.038(2) 0.0244(19) -0.0005(15) 0.0046(15) 0.0001(16)
C112 0.0240(19) 0.026(2) 0.0228(18) 0.0032(14) 0.0074(14) 0.0019(15)
C113 0.027(2) 0.045(2) 0.0236(19) -0.0022(16) 0.0054(15) 0.0018(17)
C114 0.0236(19) 0.041(2) 0.029(2) 0.0000(16) 0.0092(15) 0.0017(17)
C115 0.0227(19) 0.028(2) 0.0208(18) 0.0002(15) 0.0053(14) 0.0000(15)
C116 0.0229(19) 0.036(2) 0.0243(18) 0.0004(15) 0.0099(14) -0.0019(16)
C117 0.026(2) 0.034(2) 0.0281(19) 0.0021(15) 0.0127(15) -0.0002(16)
C118 0.040(2) 0.057(3) 0.027(2) 0.0090(19) 0.0138(17) 0.0057(19)
C119 0.035(2) 0.043(3) 0.038(2) -0.0020(18) 0.0181(17) -0.0100(19)
C120 0.038(2) 0.043(3) 0.045(2) -0.0122(18) 0.0224(19) -0.0040(19)
C121 0.027(2) 0.046(3) 0.037(2) 0.0072(17) 0.0100(16) 0.0035(18)
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
C107 O1 C109 . . 123.2(3) ?
O2 N7 C115 . . 126.2(3) ?
O2 N7 C117 . . 121.3(3) ?
C115 N7 C117 . . 112.2(3) ?
O3 N8 C115 . . 125.9(3) ?
O3 N8 C116 . . 121.2(3) ?
C115 N8 C116 . . 112.5(3) ?
N5 C101 C103 . . 177.3(4) ?
N6 C102 C104 . . 176.3(4) ?
C104 C103 C101 . . 120.6(3) ?
C108 C103 C101 . . 119.1(3) ?
C108 C103 C104 . . 120.3(3) ?
C103 C104 C102 . . 118.9(3) ?
C105 C104 C102 . . 121.5(3) ?
C105 C104 C103 . . 119.7(3) ?
C104 C105 H105 . . 119.7 ?
C106 C105 C104 . . 120.5(3) ?
C106 C105 H105 . . 119.7 ?
C105 C106 H106 . . 120.5 ?
C105 C106 C107 . . 119.0(3) ?
C107 C106 H106 . . 120.5 ?
O1 C107 C106 . . 125.7(3) ?
O1 C107 C108 . . 112.7(3) ?
C106 C107 C108 . . 121.6(3) ?
C103 C108 C107 . . 118.8(3) ?
C103 C108 H108 . . 120.6 ?
C107 C108 H108 . . 120.6 ?
C110 C109 O1 . . 123.7(3) ?
C114 C109 O1 . . 114.1(3) ?
C114 C109 C110 . . 121.8(3) ?
C109 C110 H110 . . 120.8 ?
C109 C110 C111 . . 118.4(3) ?
C111 C110 H110 . . 120.8 ?
C110 C111 H111 . . 119.5 ?
C112 C111 C110 . . 121.0(3) ?
C112 C111 H111 . . 119.5 ?
C111 C112 C113 . . 118.8(3) ?
C111 C112 C115 . . 122.3(3) ?
C113 C112 C115 . . 118.9(3) ?
C112 C113 H113 . . 119.8 ?
C114 C113 C112 . . 120.5(3) ?
C114 C113 H113 . . 119.8 ?
C109 C114 H114 . . 120.3 ?
C113 C114 C109 . . 119.5(3) ?
C113 C114 H114 . . 120.3 ?
N7 C115 C112 . . 126.8(3) ?
N8 C115 N7 . . 107.3(3) ?
N8 C115 C112 . . 125.7(3) ?
N8 C116 C117 . . 99.7(2) ?
N8 C116 C118 . . 106.1(3) ?
N8 C116 C119 . . 110.3(3) ?
C118 C116 C117 . . 114.0(3) ?
C119 C116 C117 . . 114.8(3) ?
C119 C116 C118 . . 110.9(3) ?
N7 C117 C116 . . 100.1(2) ?
C120 C117 N7 . . 109.6(3) ?
C120 C117 C116 . . 115.2(3) ?
C120 C117 C121 . . 111.4(3) ?
C121 C117 N7 . . 106.6(3) ?
C121 C117 C116 . . 112.9(3) ?
C116 C118 H11A . . 109.5 ?
C116 C118 H11B . . 109.5 ?
C116 C118 H11C . . 109.5 ?
H11A C118 H11B . . 109.5 ?
H11A C118 H11C . . 109.5 ?
H11B C118 H11C . . 109.5 ?
C116 C119 H11D . . 109.5 ?
C116 C119 H11E . . 109.5 ?
C116 C119 H11F . . 109.5 ?
H11D C119 H11E . . 109.5 ?
H11D C119 H11F . . 109.5 ?
H11E C119 H11F . . 109.5 ?
C117 C120 H12A . . 109.5 ?
C117 C120 H12B . . 109.5 ?
C117 C120 H12C . . 109.5 ?
H12A C120 H12B . . 109.5 ?
H12A C120 H12C . . 109.5 ?
H12B C120 H12C . . 109.5 ?
C117 C121 H12D . . 109.5 ?
C117 C121 H12E . . 109.5 ?
C117 C121 H12F . . 109.5 ?
H12D C121 H12E . . 109.5 ?
H12D C121 H12F . . 109.5 ?
H12E C121 H12F . . 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 C107 . 1.372(4) ?
O1 C109 . 1.394(4) ?
O2 N7 . 1.281(3) ?
O3 N8 . 1.289(3) ?
N5 C101 . 1.142(4) ?
N6 C102 . 1.146(4) ?
N7 C115 . 1.352(4) ?
N7 C117 . 1.510(4) ?
N8 C115 . 1.350(4) ?
N8 C116 . 1.499(4) ?
C101 C103 . 1.440(5) ?
C102 C104 . 1.438(5) ?
C103 C104 . 1.399(5) ?
C103 C108 . 1.377(4) ?
C104 C105 . 1.387(5) ?
C105 H105 . 0.9500 ?
C105 C106 . 1.378(5) ?
C106 H106 . 0.9500 ?
C106 C107 . 1.381(5) ?
C107 C108 . 1.391(5) ?
C108 H108 . 0.9500 ?
C109 C110 . 1.377(5) ?
C109 C114 . 1.376(5) ?
C110 H110 . 0.9500 ?
C110 C111 . 1.393(5) ?
C111 H111 . 0.9500 ?
C111 C112 . 1.386(4) ?
C112 C113 . 1.400(5) ?
C112 C115 . 1.447(4) ?
C113 H113 . 0.9500 ?
C113 C114 . 1.375(5) ?
C114 H114 . 0.9500 ?
C116 C117 . 1.551(5) ?
C116 C118 . 1.519(5) ?
C116 C119 . 1.508(5) ?
C117 C120 . 1.506(5) ?
C117 C121 . 1.511(5) ?
C118 H11A . 0.9800 ?
C118 H11B . 0.9800 ?
C118 H11C . 0.9800 ?
C119 H11D . 0.9800 ?
C119 H11E . 0.9800 ?
C119 H11F . 0.9800 ?
C120 H12A . 0.9800 ?
C120 H12B . 0.9800 ?
C120 H12C . 0.9800 ?
C121 H12D . 0.9800 ?
C121 H12E . 0.9800 ?
C121 H12F . 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
_geom_hbond_publ_flag
C118 H11C N5 1_456 0.98 2.57 3.469(6) 153 yes
C105 H105 O3 1_554 0.95 2.43 3.282(4) 149 yes
C108 H108 O2 1_655 0.95 2.59 3.476(4) 155 yes
C111 H111 O2 . 0.95 2.39 2.940(4) 117 yes
C113 H113 O3 . 0.95 2.27 2.859(4) 119 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1 C107 C108 C103 . . . . 178.9(3) ?
O1 C109 C110 C111 . . . . 173.5(3) ?
O1 C109 C114 C113 . . . . -173.7(3) ?
O2 N7 C115 N8 . . . . -179.0(3) ?
O2 N7 C115 C112 . . . . -2.7(5) ?
O2 N7 C117 C116 . . . . 163.6(3) ?
O2 N7 C117 C120 . . . . 42.0(4) ?
O2 N7 C117 C121 . . . . -78.7(4) ?
O3 N8 C115 N7 . . . . -174.2(3) ?
O3 N8 C115 C112 . . . . 9.5(5) ?
O3 N8 C116 C117 . . . . 160.8(3) ?
O3 N8 C116 C118 . . . . -80.6(4) ?
O3 N8 C116 C119 . . . . 39.6(4) ?
N8 C116 C117 N7 . . . . 26.2(3) ?
N8 C116 C117 C120 . . . . 143.6(3) ?
N8 C116 C117 C121 . . . . -86.8(3) ?
C101 C103 C104 C102 . . . . 3.6(5) ?
C101 C103 C104 C105 . . . . -176.3(3) ?
C101 C103 C108 C107 . . . . 177.9(3) ?
C102 C104 C105 C106 . . . . 179.1(3) ?
C103 C104 C105 C106 . . . . -1.1(5) ?
C104 C103 C108 C107 . . . . -0.2(5) ?
C104 C105 C106 C107 . . . . -1.2(5) ?
C105 C106 C107 O1 . . . . -178.3(3) ?
C105 C106 C107 C108 . . . . 2.8(5) ?
C106 C107 C108 C103 . . . . -2.1(5) ?
C107 O1 C109 C110 . . . . 57.1(5) ?
C107 O1 C109 C114 . . . . -129.5(3) ?
C108 C103 C104 C102 . . . . -178.4(3) ?
C108 C103 C104 C105 . . . . 1.8(5) ?
C109 O1 C107 C106 . . . . -6.6(5) ?
C109 O1 C107 C108 . . . . 172.4(3) ?
C109 C110 C111 C112 . . . . -0.7(5) ?
C110 C109 C114 C113 . . . . -0.3(6) ?
C110 C111 C112 C113 . . . . 0.3(5) ?
C110 C111 C112 C115 . . . . -177.0(3) ?
C111 C112 C113 C114 . . . . 0.1(5) ?
C111 C112 C115 N7 . . . . 25.1(5) ?
C111 C112 C115 N8 . . . . -159.3(3) ?
C112 C113 C114 C109 . . . . -0.1(5) ?
C113 C112 C115 N7 . . . . -152.2(3) ?
C113 C112 C115 N8 . . . . 23.5(5) ?
C114 C109 C110 C111 . . . . 0.6(5) ?
C115 N7 C117 C116 . . . . -22.4(3) ?
C115 N7 C117 C120 . . . . -144.0(3) ?
C115 N7 C117 C121 . . . . 95.4(3) ?
C115 N8 C116 C117 . . . . -25.6(3) ?
C115 N8 C116 C118 . . . . 93.1(3) ?
C115 N8 C116 C119 . . . . -146.8(3) ?
C115 C112 C113 C114 . . . . 177.5(3) ?
C116 N8 C115 N7 . . . . 12.5(4) ?
C116 N8 C115 C112 . . . . -163.9(3) ?
C117 N7 C115 N8 . . . . 7.3(4) ?
C117 N7 C115 C112 . . . . -176.4(3) ?
C118 C116 C117 N7 . . . . -86.5(3) ?
C118 C116 C117 C120 . . . . 31.0(4) ?
C118 C116 C117 C121 . . . . 160.6(3) ?
C119 C116 C117 N7 . . . . 144.0(3) ?
C119 C116 C117 C120 . . . . -98.6(4) ?
C119 C116 C117 C121 . . . . 31.0(4) ?
_cod_database_fobs_code 2022330