#------------------------------------------------------------------------------
#$Date: 2021-05-29 08:14:06 +0300 (Sat, 29 May 2021) $
#$Revision: 265608 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243839.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_2243839
loop_
_publ_author_name
'Kansiz, Sevgi'
'Tatlidil, Digdem'
'Dege, Necmi'
'Aktas, Feyzi Alkim'
'Al-Asbahy, Samir Osman Mohammed'
'Alaman Agar, Aysen'
_publ_section_title
;
Crystal structure and molecular docking study of
(E)-2-{[(E)-2-hydroxy-5-methylbenzylidene]hydrazinylidene}-1,2-diphenylethan-1-one
;
_journal_coeditor_code YK2152
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 658
_journal_page_last 662
_journal_paper_doi 10.1107/S2056989021005442
_journal_volume 77
_journal_year 2021
_chemical_formula_moiety 'C22 H18 N2 O2'
_chemical_formula_sum 'C22 H18 N2 O2'
_chemical_formula_weight 342.38
_chemical_name_systematic
(E)-2-{[(E)-2-Hydroxy-5-methylbenzylidene]hydrazinylidene}-1,2-diphenylethan-1-one
_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
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 97.814(6)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.4089(6)
_cell_length_b 11.4544(14)
_cell_length_c 21.9491(17)
_cell_measurement_reflns_used 7807
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 29.14
_cell_measurement_theta_min 1.78
_cell_volume 1845.4(3)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_reduction
;
X-RED (Stoe & Cie, 2002)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/3 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 296(2)
_diffrn_detector 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device '2-circle goniometer'
_diffrn_measurement_device_type 'Stoe IPDS 2'
_diffrn_measurement_method 'rotation method'
_diffrn_radiation_monochromator 'plane graphite'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0374
_diffrn_reflns_av_unetI/netI 0.0426
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 8376
_diffrn_reflns_theta_full 25.049
_diffrn_reflns_theta_max 25.049
_diffrn_reflns_theta_min 1.873
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current 45
_diffrn_source_power 2.25
_diffrn_source_voltage 50
_exptl_absorpt_coefficient_mu 0.080
_exptl_absorpt_correction_T_max 0.9870
_exptl_absorpt_correction_T_min 0.9521
_exptl_absorpt_correction_type integration
_exptl_absorpt_process_details
;
(X-RED32; Stoe & Cie, 2002)
;
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.232
_exptl_crystal_description prism
_exptl_crystal_F_000 720
_exptl_crystal_size_max 0.710
_exptl_crystal_size_mid 0.490
_exptl_crystal_size_min 0.210
_refine_diff_density_max 0.497
_refine_diff_density_min -0.449
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.114
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 237
_refine_ls_number_reflns 3262
_refine_ls_number_restraints 84
_refine_ls_restrained_S_all 1.224
_refine_ls_R_factor_all 0.1300
_refine_ls_R_factor_gt 0.0847
_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^)+(0.1388P)^2^+0.7696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2593
_refine_ls_wR_factor_ref 0.2869
_reflns_number_gt 1801
_reflns_number_total 3262
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yk2152sup1.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2243839
_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_hkl_file
;
1 0 0 204.09 7.30 0
-1 0 0 241.02 7.15 0
2 0 0 2200.45 15.65 0
3 0 0 0.28 1.78 0
4 0 0 32.13 2.34 0
5 0 0 -0.07 2.00 0
6 0 0 8.40 2.66 0
7 0 0 10.28 3.74 0
7 0 0 10.97 3.73 0
-1 1 0 633.91 6.97 0
1 -1 0 599.10 7.10 0
2 -1 0 16.71 1.92 0
3 -1 0 7.85 1.54 0
4 -1 0 27.91 1.84 0
5 -1 0 8.54 1.89 0
6 -1 0 5.75 2.06 0
7 -1 0 7.29 2.23 0
8 -1 0 1.44 2.96 0
8 -1 0 1.50 2.88 0
0 -2 0 506.77 5.91 0
-1 -2 0 1193.05 10.60 0
1 -2 0 1209.45 7.78 0
2 -2 0 234.69 3.39 0
-2 -2 0 230.12 6.89 0
3 -2 0 1.01 1.40 0
4 -2 0 19.44 1.87 0
5 -2 0 -0.56 1.91 0
6 -2 0 10.15 2.01 0
7 -2 0 4.96 2.05 0
8 -2 0 2.61 2.24 0
9 -2 0 0.65 3.00 0
9 -2 0 0.58 2.91 0
-1 -3 0 42.13 2.19 0
1 -3 0 41.58 1.60 0
2 -3 0 0.05 1.49 0
-2 -3 0 -0.09 1.92 0
3 -3 0 28.01 1.74 0
-3 -3 0 28.93 3.54 0
-3 -3 0 37.03 3.66 0
4 -3 0 4.06 1.53 0
5 -3 0 22.40 1.70 0
6 -3 0 -0.44 1.62 0
7 -3 0 4.05 2.12 0
8 -3 0 0.96 1.86 0
9 -3 0 1.02 2.63 0
0 -4 0 71.68 2.17 0
-1 -4 0 1018.18 6.26 0
1 -4 0 988.36 5.39 0
-2 -4 0 16.82 1.70 0
2 -4 0 17.16 1.62 0
-3 -4 0 26.82 2.29 0
3 -4 0 27.94 1.72 0
4 -4 0 5.92 1.51 0
5 -4 0 4.64 1.47 0
6 -4 0 11.35 1.57 0
7 -4 0 1.22 2.09 0
8 -4 0 0.13 1.85 0
9 -4 0 0.41 2.08 0
1 -5 0 48.78 1.80 0
-1 -5 0 50.55 1.93 0
-2 -5 0 8.42 1.48 0
2 -5 0 8.07 1.45 0
3 -5 0 9.28 1.48 0
-3 -5 0 7.14 1.57 0
4 -5 0 0.11 1.45 0
-4 -5 0 0.24 2.27 0
-4 -5 0 0.50 2.01 0
5 -5 0 0.34 1.48 0
6 -5 0 3.08 1.60 0
7 -5 0 1.38 1.83 0
8 -5 0 1.73 1.96 0
9 -5 0 0.08 2.63 0
0 -6 0 162.00 2.16 0
-1 -6 0 0.75 1.48 0
1 -6 0 1.15 1.43 0
-2 -6 0 5.45 1.40 0
2 -6 0 5.56 1.01 0
3 -6 0 9.84 1.48 0
-3 -6 0 10.14 1.90 0
-4 -6 0 0.80 2.06 0
4 -6 0 0.82 1.09 0
5 -6 0 36.24 1.88 0
6 -6 0 2.77 1.67 0
7 -6 0 0.88 1.80 0
8 -6 0 -1.04 2.05 0
9 -6 0 2.49 2.23 0
1 -7 0 7.93 1.05 0
-1 -7 0 8.94 1.49 0
-2 -7 0 0.39 1.36 0
2 -7 0 -0.32 1.42 0
3 -7 0 8.11 1.54 0
-3 -7 0 7.25 1.62 0
4 -7 0 7.45 1.56 0
-4 -7 0 6.91 1.99 0
-5 -7 0 18.39 2.87 0
-5 -7 0 16.08 2.84 0
5 -7 0 17.47 1.73 0
6 -7 0 5.02 1.84 0
7 -7 0 1.63 1.81 0
8 -7 0 -0.37 2.42 0
9 -7 0 0.90 2.37 0
0 -8 0 11.13 1.54 0
-1 -8 0 28.09 1.63 0
1 -8 0 29.53 1.63 0
2 -8 0 13.95 1.12 0
-2 -8 0 13.42 1.57 0
3 -8 0 1.32 1.47 0
-3 -8 0 0.73 1.58 0
-4 -8 0 40.23 2.41 0
4 -8 0 37.20 1.78 0
-5 -8 0 6.54 2.28 0
-5 -8 0 6.73 2.21 0
5 -8 0 4.34 1.70 0
6 -8 0 0.48 1.80 0
7 -8 0 0.24 1.95 0
8 -8 0 1.55 2.09 0
1 -9 0 4.23 1.46 0
-1 -9 0 2.01 1.04 0
2 -9 0 3.55 1.46 0
-2 -9 0 2.04 1.51 0
3 -9 0 7.42 1.58 0
-3 -9 0 7.70 1.63 0
-4 -9 0 31.98 2.33 0
4 -9 0 28.52 1.78 0
-5 -9 0 3.18 2.18 0
5 -9 0 2.35 1.64 0
6 -9 0 4.16 1.80 0
7 -9 0 0.36 2.03 0
8 -9 0 0.06 2.26 0
0 -10 0 2.71 1.52 0
1 -10 0 12.28 1.64 0
-1 -10 0 12.91 1.24 0
-2 -10 0 20.80 1.75 0
2 -10 0 21.16 1.64 0
3 -10 0 3.38 1.56 0
-3 -10 0 5.81 2.07 0
-4 -10 0 4.20 1.81 0
4 -10 0 5.48 1.73 0
5 -10 0 1.25 1.74 0
-5 -10 0 0.82 2.20 0
-6 -10 0 0.73 3.48 0
6 -10 0 0.65 1.92 0
-6 -10 0 0.22 3.51 0
7 -10 0 1.12 2.07 0
1 -11 0 -0.07 1.62 0
-1 -11 0 0.46 1.12 0
-2 -11 0 1.62 1.74 0
2 -11 0 1.54 1.15 0
3 -11 0 2.10 1.68 0
-3 -11 0 2.47 1.72 0
-4 -11 0 0.87 2.23 0
4 -11 0 -0.02 1.25 0
-5 -11 0 0.45 2.39 0
5 -11 0 0.78 1.86 0
-6 -11 0 0.11 3.25 0
-6 -11 0 0.54 2.94 0
6 -11 0 -0.33 2.03 0
7 -11 0 0.55 2.26 0
0 -12 0 2.33 1.75 0
1 -12 0 7.11 1.74 0
-1 -12 0 4.51 1.26 0
2 -12 0 2.80 1.67 0
-2 -12 0 1.13 1.74 0
-3 -12 0 0.55 1.72 0
3 -12 0 1.89 1.23 0
-4 -12 0 3.78 1.95 0
4 -12 0 1.98 1.90 0
5 -12 0 -0.15 1.41 0
-5 -12 0 0.74 2.55 0
-6 -12 0 0.11 2.80 0
-6 -12 0 0.23 3.22 0
6 -12 0 -1.96 2.20 0
1 -13 0 2.08 1.82 0
-1 -13 0 1.93 1.81 0
2 -13 0 1.78 1.85 0
-2 -13 0 -0.68 1.92 0
-3 -13 0 1.48 1.95 0
3 -13 0 0.46 1.83 0
-4 -13 0 0.44 2.14 0
4 -13 0 0.95 2.00 0
-5 -13 0 0.12 2.75 0
5 -13 0 1.06 2.15 0
0 -14 0 -0.17 1.37 0
1 -14 0 0.81 1.97 0
-1 -14 0 0.95 1.95 0
2 -14 0 2.58 2.01 0
-2 -14 0 1.02 2.04 0
-3 -14 0 -1.27 2.06 0
3 -14 0 2.30 2.00 0
-4 -14 0 -0.70 2.20 0
4 -14 0 -0.25 2.16 0
-1 -15 0 1.14 2.12 0
1 -15 0 1.40 2.21 0
-2 -15 0 1.39 2.13 0
2 -15 0 -0.57 2.18 0
3 -15 0 1.31 2.20 0
8 -1 -1 1.64 2.88 0
8 -1 -1 1.46 2.66 0
7 -1 -1 13.10 2.51 0
6 -1 -1 3.61 1.95 0
5 -1 -1 0.37 1.44 0
4 -1 -1 14.05 1.61 0
3 -1 -1 100.22 2.58 0
2 -1 -1 20.22 2.12 0
-1 -1 1 279.83 8.15 0
1 1 -1 323.15 8.02 0
0 -1 1 1343.21 12.27 0
0 1 -1 1434.98 12.20 0
-1 1 -1 40.50 2.63 0
-1 -1 -1 45.89 3.73 0
1 -1 1 39.41 2.69 0
-2 1 -1 200.42 3.60 0
2 1 1 215.22 7.03 0
2 -1 1 207.89 3.69 0
-2 -1 -1 243.58 6.84 0
-3 1 -1 0.47 1.74 0
3 1 1 -0.01 2.55 0
-3 -1 -1 -0.01 2.45 0
3 -1 1 -0.18 1.46 0
4 -1 1 2.36 1.50 0
4 1 1 1.79 2.95 0
5 -1 1 0.87 1.49 0
6 -1 1 16.93 2.16 0
7 -1 1 0.38 2.00 0
8 -1 1 1.10 2.97 0
9 -2 -1 0.55 2.94 0
9 -2 -1 -0.24 2.84 0
8 -2 -1 0.98 2.24 0
7 -2 -1 9.87 2.16 0
6 -2 -1 1.77 1.91 0
5 -2 -1 1.14 1.51 0
4 -2 -1 1.20 1.32 0
3 -2 -1 122.04 2.50 0
-2 -2 1 875.56 11.89 0
2 -2 -1 863.86 5.89 0
1 2 -1 450.57 6.14 0
-1 -2 1 428.46 6.28 0
0 2 -1 2003.94 10.78 0
0 -2 1 1926.51 10.79 0
1 -2 1 1976.94 9.46 0
-1 2 -1 2039.91 9.37 0
-2 2 -1 12.55 1.23 0
2 -2 1 12.24 1.63 0
-2 -2 -1 15.65 2.70 0
3 -2 1 171.89 3.00 0
-3 2 -1 161.95 2.70 0
4 -2 1 67.41 1.97 0
5 -2 1 67.15 2.09 0
6 -2 1 15.48 1.71 0
7 -2 1 0.87 2.08 0
8 -2 1 0.63 2.22 0
9 -2 1 0.24 2.94 0
9 -2 1 0.60 3.26 0
9 -3 -1 0.29 2.61 0
8 -3 -1 3.33 2.27 0
7 -3 -1 0.41 2.07 0
6 -3 -1 6.65 1.93 0
5 -3 -1 7.46 1.53 0
4 -3 -1 2.40 1.36 0
-3 -3 1 140.08 5.47 0
3 -3 -1 128.97 2.45 0
-2 -3 1 520.30 6.23 0
2 -3 -1 526.42 4.21 0
-1 -3 1 35.88 2.14 0
1 3 -1 35.73 2.06 0
1 -3 -1 33.87 1.55 0
0 3 -1 203.65 3.18 0
0 -3 1 200.14 3.22 0
1 -3 1 248.03 3.08 0
-1 3 -1 260.73 3.28 0
-2 3 -1 119.87 2.34 0
2 -3 1 114.76 2.34 0
3 -3 1 2.97 1.49 0
-3 -3 -1 3.48 2.72 0
-3 -3 -1 2.38 2.42 0
4 -3 1 1.11 1.42 0
5 -3 1 63.43 2.01 0
6 -3 1 22.25 1.75 0
7 -3 1 1.56 1.72 0
8 -3 1 0.39 1.82 0
9 -3 1 0.15 2.60 0
9 -4 -1 -0.17 2.53 0
8 -4 -1 1.24 1.85 0
7 -4 -1 1.19 1.65 0
6 -4 -1 1.24 1.52 0
5 -4 -1 0.06 1.42 0
4 -4 -1 4.60 1.51 0
-3 -4 1 59.93 2.94 0
3 -4 -1 55.48 1.88 0
2 -4 -1 6.59 1.50 0
-2 -4 1 7.10 1.57 0
-1 -4 1 696.36 5.28 0
1 -4 -1 687.31 4.56 0
0 4 -1 237.46 2.89 0
0 -4 -1 232.85 3.07 0
0 -4 1 235.55 3.13 0
1 -4 1 24.04 1.67 0
-1 -4 -1 22.94 1.73 0
-1 4 -1 22.89 1.69 0
-2 -4 -1 7.94 1.58 0
-2 4 -1 8.10 1.17 0
2 -4 1 7.68 1.60 0
3 -4 1 63.09 1.94 0
-3 -4 -1 61.75 2.92 0
4 -4 1 1.74 1.46 0
5 -4 1 37.24 1.77 0
6 -4 1 -0.27 1.53 0
7 -4 1 19.76 2.24 0
8 -4 1 2.39 1.91 0
9 -4 1 0.34 2.64 0
9 -5 -1 0.60 2.15 0
8 -5 -1 0.59 2.34 0
7 -5 -1 2.23 2.09 0
6 -5 -1 2.28 1.56 0
5 -5 -1 9.31 1.52 0
-4 -5 1 2.37 2.07 0
4 -5 -1 2.38 1.45 0
3 -5 -1 0.81 1.01 0
-3 -5 1 1.17 1.81 0
-2 -5 1 17.58 1.59 0
2 -5 -1 19.50 1.51 0
-1 -5 1 231.86 3.00 0
1 -5 -1 212.94 2.42 0
0 -5 1 2.54 1.54 0
0 -5 -1 3.01 1.55 0
1 -5 1 614.37 4.01 0
-1 -5 -1 601.40 4.46 0
-2 -5 -1 102.54 2.32 0
2 -5 1 103.98 1.80 0
3 -5 1 42.75 1.71 0
-3 -5 -1 40.21 2.30 0
4 -5 1 1.46 1.44 0
-4 -5 -1 0.52 2.28 0
-4 -5 -1 -0.03 2.01 0
5 -5 1 0.90 1.53 0
6 -5 1 0.30 1.59 0
7 -5 1 1.47 1.75 0
8 -5 1 -0.02 1.91 0
9 -5 1 0.25 2.16 0
9 -6 -1 1.10 2.24 0
8 -6 -1 1.61 1.99 0
7 -6 -1 0.91 1.75 0
6 -6 -1 29.67 1.86 0
5 -6 -1 1.42 1.60 0
-4 -6 1 -0.29 1.77 0
4 -6 -1 -0.31 1.10 0
3 -6 -1 37.95 1.65 0
-3 -6 1 37.76 2.16 0
-2 -6 1 42.76 1.72 0
2 -6 -1 44.89 1.66 0
1 -6 -1 53.39 1.73 0
-1 -6 1 50.25 1.54 0
0 -6 -1 81.84 1.99 0
0 -6 1 84.86 2.01 0
1 -6 1 383.57 3.11 0
-1 -6 -1 380.50 3.45 0
2 -6 1 66.15 1.74 0
-2 -6 -1 66.35 1.91 0
-3 -6 -1 5.91 1.54 0
3 -6 1 6.45 1.50 0
-4 -6 -1 1.67 1.88 0
-4 -6 -1 1.08 1.80 0
4 -6 1 1.01 1.07 0
5 -6 1 19.14 1.79 0
6 -6 1 -1.72 1.63 0
7 -6 1 2.29 1.76 0
8 -6 1 0.75 2.03 0
9 -6 1 0.09 2.25 0
9 -7 -1 2.36 2.32 0
8 -7 -1 0.90 1.95 0
7 -7 -1 0.15 1.86 0
6 -7 -1 30.89 2.09 0
-5 -7 1 1.96 2.59 0
5 -7 -1 0.95 1.56 0
-5 -7 1 1.34 2.61 0
-4 -7 1 0.98 1.83 0
4 -7 -1 1.43 1.08 0
3 -7 -1 41.92 1.35 0
-3 -7 1 43.74 2.15 0
-2 -7 1 0.70 1.40 0
2 -7 -1 1.31 1.40 0
1 -7 -1 4.06 1.39 0
-1 -7 1 3.93 1.08 0
0 -7 1 35.85 1.60 0
0 -7 -1 34.95 1.59 0
1 -7 1 4.72 1.41 0
-1 -7 -1 4.13 1.44 0
-2 -7 -1 13.38 1.82 0
2 -7 1 13.01 1.50 0
-3 -7 -1 2.72 1.55 0
3 -7 1 2.08 1.53 0
4 -7 1 64.72 1.88 0
-4 -7 -1 64.65 2.54 0
5 -7 1 6.70 1.63 0
-5 -7 -1 8.67 2.78 0
-5 -7 -1 10.32 2.82 0
6 -7 1 0.14 1.89 0
7 -7 1 3.02 1.82 0
8 -7 1 2.39 2.08 0
8 -8 -1 -0.38 2.05 0
7 -8 -1 0.78 1.95 0
6 -8 -1 3.05 1.85 0
-5 -8 1 1.32 2.40 0
5 -8 -1 2.39 1.63 0
4 -8 -1 1.25 1.64 0
-4 -8 1 2.72 1.70 0
3 -8 -1 1.71 1.50 0
-3 -8 1 1.48 1.52 0
2 -8 -1 3.65 1.41 0
-2 -8 1 3.66 1.51 0
1 -8 -1 0.85 1.05 0
-1 -8 1 1.39 1.42 0
0 -8 1 4.40 1.53 0
0 -8 -1 3.13 1.49 0
-1 -8 -1 1.85 1.48 0
1 -8 1 2.14 1.48 0
2 -8 1 28.42 1.58 0
-2 -8 -1 25.71 1.57 0
-3 -8 -1 6.55 1.64 0
3 -8 1 7.64 1.54 0
4 -8 1 81.23 2.10 0
-4 -8 -1 75.01 2.38 0
-5 -8 -1 3.99 2.47 0
5 -8 1 3.74 1.62 0
-5 -8 -1 2.59 2.51 0
6 -8 1 12.49 1.81 0
7 -8 1 1.26 1.89 0
8 -8 1 2.05 2.16 0
8 -9 -1 0.06 2.19 0
7 -9 -1 1.00 1.96 0
6 -9 -1 2.22 1.83 0
5 -9 -1 1.76 1.77 0
-5 -9 1 1.61 2.17 0
4 -9 -1 0.63 1.65 0
-4 -9 1 2.65 1.71 0
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1 -1 -27 1.29 1.39 0
-1 -1 27 -0.69 1.98 0
-1 1 27 0.39 1.39 0
0 1 -27 0.53 1.98 0
0 1 27 -0.15 1.40 0
0 -1 27 0.18 1.96 0
0 -1 -27 0.05 2.01 0
-1 1 -27 1.00 2.14 0
1 1 27 0.37 1.44 0
1 -1 27 -0.16 1.50 0
-1 -1 -27 1.03 1.51 0
-2 1 -27 -0.32 1.44 0
2 1 27 1.50 2.15 0
2 -1 27 0.14 2.12 0
-2 -1 -27 1.74 1.53 0
3 1 27 0.90 2.19 0
-3 -1 -27 1.79 2.26 0
3 -1 27 -0.04 2.28 0
-5 -2 27 0.10 2.24 0
5 2 -27 0.23 2.22 0
5 -2 -27 1.30 2.23 0
4 2 -27 0.74 2.15 0
-4 -2 27 -0.81 2.16 0
4 -2 -27 2.55 2.20 0
-3 -2 27 2.61 2.12 0
3 2 -27 -1.12 1.45 0
3 -2 -27 0.27 1.46 0
2 2 -27 -0.81 1.42 0
-2 -2 27 0.81 2.04 0
2 -2 -27 3.40 1.92 0
1 2 -27 1.82 1.99 0
-1 -2 27 0.45 1.97 0
1 -2 -27 2.86 1.96 0
-1 2 27 0.58 1.41 0
0 -2 27 1.09 2.00 0
0 2 -27 -0.04 2.00 0
0 -2 -27 1.51 2.07 0
0 2 27 -1.30 2.04 0
1 -2 27 1.67 2.11 0
1 2 27 2.59 1.47 0
-1 2 -27 3.00 1.46 0
-1 -2 -27 5.01 2.14 0
2 -2 27 -0.54 1.55 0
2 2 27 1.00 2.20 0
-2 2 -27 0.83 2.18 0
-2 -2 -27 0.36 2.20 0
3 -2 27 0.16 1.71 0
3 2 27 1.43 2.34 0
5 3 -27 3.03 2.29 0
-5 -3 27 1.37 2.28 0
5 -3 -27 2.93 2.45 0
-4 -3 27 1.58 2.24 0
4 3 -27 3.02 2.17 0
4 -3 -27 1.45 2.21 0
3 3 -27 1.24 2.13 0
-3 -3 27 2.69 2.08 0
3 -3 -27 3.97 2.09 0
2 3 -27 1.78 2.05 0
-2 -3 27 -0.58 1.49 0
2 -3 -27 1.90 1.39 0
-1 -3 27 -0.53 2.01 0
1 3 -27 -0.38 1.42 0
1 -3 -27 0.20 2.07 0
0 3 -27 2.03 2.02 0
0 -3 -27 0.66 1.47 0
0 -3 27 -0.63 1.97 0
-1 3 -27 0.30 1.52 0
-1 -3 -27 1.10 2.10 0
1 -3 27 0.50 2.12 0
-2 3 -27 3.54 2.20 0
2 3 27 1.24 1.54 0
-2 -3 -27 3.51 2.12 0
2 -3 27 1.91 2.26 0
4 4 -27 -0.46 2.19 0
-4 -4 27 0.09 2.21 0
4 -4 -27 0.28 2.27 0
3 4 -27 1.06 2.16 0
-3 -4 27 1.32 2.16 0
3 -4 -27 2.15 2.14 0
-2 -4 27 0.98 1.46 0
2 4 -27 0.60 2.06 0
2 -4 -27 -0.45 1.42 0
1 4 -27 1.27 2.06 0
1 -4 -27 1.00 2.09 0
-1 -4 27 1.51 1.99 0
0 4 -27 0.77 2.09 0
0 -4 -27 1.13 1.52 0
0 -4 27 1.09 2.07 0
-1 4 -27 0.73 2.16 0
-1 -4 -27 -0.41 2.07 0
1 -4 27 0.76 1.54 0
-2 -4 -27 0.91 2.15 0
2 -4 27 -0.19 2.23 0
-2 4 -27 -0.07 1.63 0
4 5 -27 0.90 2.26 0
4 -5 -27 1.08 2.27 0
-4 -5 27 -0.82 2.27 0
3 -5 -27 1.93 2.18 0
3 5 -27 1.31 2.09 0
-3 -5 27 -0.90 2.23 0
2 5 -27 1.85 1.52 0
-2 -5 27 2.55 1.62 0
2 -5 -27 0.01 2.16 0
1 5 -27 1.13 2.18 0
-1 -5 27 1.70 2.11 0
1 -5 -27 0.94 2.17 0
0 5 -27 3.14 2.21 0
0 -5 27 0.98 2.12 0
0 -5 -27 -0.35 2.29 0
1 -5 27 1.29 2.26 0
-1 -5 -27 1.61 2.23 0
-1 5 -27 2.15 2.17 0
3 -6 -27 -0.83 2.25 0
-3 -6 27 0.08 2.25 0
3 6 -27 0.45 1.56 0
2 -6 -27 -0.60 2.17 0
-2 -6 27 0.79 2.18 0
2 6 -27 1.43 2.25 0
1 -6 -27 2.03 2.16 0
-1 -6 27 -0.04 1.63 0
1 6 -27 0.76 2.25 0
0 -6 27 1.26 1.60 0
0 -6 -27 -0.23 2.34 0
0 6 -27 3.97 2.24 0
1 -6 27 1.42 2.25 0
-1 -7 27 0.75 2.35 0
4 0 -28 0.13 2.21 0
-3 0 28 2.05 2.07 0
3 0 -28 2.21 2.10 0
2 0 -28 1.41 1.46 0
-2 0 28 2.03 2.14 0
-1 0 28 1.97 1.48 0
1 0 -28 2.81 1.48 0
0 0 28 0.46 2.10 0
0 0 -28 0.21 2.06 0
-1 0 -28 22.15 2.15 0
1 0 28 16.84 1.66 0
-2 0 -28 1.64 2.25 0
2 0 28 0.92 2.17 0
-4 -1 28 0.94 2.20 0
4 1 -28 -0.39 2.23 0
4 -1 -28 1.04 2.17 0
3 1 -28 0.88 2.07 0
3 -1 -28 -0.75 1.53 0
-3 -1 28 0.22 1.54 0
-2 1 28 0.83 1.53 0
-2 -1 28 0.30 2.07 0
2 1 -28 1.09 1.42 0
2 -1 -28 1.95 2.07 0
-1 1 28 0.25 2.02 0
1 1 -28 -0.65 2.02 0
1 -1 -28 1.19 2.02 0
-1 -1 28 -1.41 2.02 0
0 1 -28 1.18 2.02 0
0 -1 -28 0.76 1.55 0
0 -1 28 0.46 2.03 0
0 1 28 -0.20 1.50 0
-1 1 -28 1.81 2.13 0
-1 -1 -28 -1.27 2.25 0
1 1 28 0.40 2.10 0
1 -1 28 0.16 2.15 0
-2 1 -28 1.21 2.32 0
-2 -1 -28 0.29 1.53 0
2 -1 28 0.35 2.24 0
2 1 28 1.93 2.17 0
4 2 -28 0.96 2.18 0
4 -2 -28 2.80 2.26 0
-4 -2 28 -0.51 2.15 0
-3 -2 28 2.09 2.14 0
3 2 -28 0.87 2.12 0
3 -2 -28 0.90 2.15 0
2 2 -28 1.01 1.48 0
2 -2 -28 0.92 1.42 0
-2 -2 28 0.31 2.14 0
1 2 -28 1.06 2.02 0
-1 -2 28 -0.56 1.43 0
1 -2 -28 0.33 1.41 0
-1 2 28 1.79 2.02 0
0 2 -28 1.04 1.47 0
0 -2 28 -1.21 1.43 0
0 -2 -28 0.34 2.17 0
0 2 28 -0.18 1.47 0
1 -2 28 0.95 1.51 0
-1 2 -28 3.20 2.19 0
-1 -2 -28 -0.20 2.17 0
1 2 28 1.15 1.56 0
2 -2 28 1.11 2.31 0
-2 -2 -28 0.78 2.21 0
2 2 28 1.42 2.19 0
4 3 -28 0.87 2.30 0
-4 -3 28 2.10 2.21 0
4 -3 -28 -0.05 2.22 0
3 3 -28 0.12 2.14 0
-3 -3 28 0.03 2.15 0
3 -3 -28 0.59 2.22 0
2 3 -28 -0.07 1.50 0
-2 -3 28 1.82 2.13 0
2 -3 -28 1.40 2.14 0
-1 -3 28 0.46 2.11 0
1 3 -28 0.73 2.13 0
1 -3 -28 -0.53 2.12 0
0 -3 28 -0.13 1.47 0
0 3 -28 2.56 2.14 0
0 -3 -28 0.37 2.14 0
-1 3 -28 1.36 2.22 0
-1 -3 -28 0.34 2.21 0
1 -3 28 1.53 2.15 0
-4 -4 28 0.78 2.32 0
3 4 -28 1.37 2.28 0
-3 -4 28 0.61 2.19 0
3 -4 -28 1.84 2.22 0
2 4 -28 0.50 2.21 0
-2 -4 28 -0.68 2.29 0
2 -4 -28 0.23 2.14 0
1 4 -28 1.31 2.16 0
1 -4 -28 3.30 2.17 0
-1 -4 28 0.07 2.17 0
0 4 -28 0.27 2.12 0
0 -4 -28 2.88 2.22 0
0 -4 28 0.54 1.49 0
-1 4 -28 1.76 2.29 0
-1 -4 -28 -0.61 2.24 0
1 -4 28 -0.08 2.22 0
-3 -5 28 1.19 2.32 0
2 5 -28 1.68 2.23 0
2 -5 -28 1.97 1.53 0
-2 -5 28 -0.93 2.23 0
1 5 -28 1.12 2.20 0
-1 -5 28 0.82 1.55 0
1 -5 -28 1.16 1.63 0
0 5 -28 7.04 2.27 0
0 -5 28 7.51 2.23 0
0 -5 -28 9.56 2.30 0
-4 -1 29 0.47 2.35 0
3 1 -29 2.19 2.24 0
3 -1 -29 1.99 2.19 0
-3 -1 29 6.32 2.23 0
-2 -1 29 1.00 2.15 0
2 1 -29 -0.18 1.56 0
2 -1 -29 1.56 2.21 0
-2 1 29 0.26 2.18 0
1 1 -29 1.20 2.13 0
1 -1 -29 3.42 2.19 0
-1 1 29 1.51 2.13 0
-1 -1 29 0.24 2.15 0
0 1 -29 -0.32 1.57 0
0 -1 -29 1.04 2.17 0
0 -1 29 1.32 2.19 0
0 1 29 1.06 1.52 0
-1 1 -29 2.06 1.58 0
-1 -1 -29 0.55 2.30 0
1 -1 29 1.50 2.28 0
1 1 29 2.21 2.23 0
-3 -2 29 -0.22 2.16 0
3 2 -29 0.40 2.17 0
3 -2 -29 1.23 1.62 0
2 2 -29 -0.96 2.22 0
2 -2 -29 1.17 2.18 0
-2 -2 29 -0.45 2.25 0
1 2 -29 2.52 2.16 0
-1 -2 29 -0.05 1.56 0
1 -2 -29 0.12 2.16 0
0 2 -29 2.73 2.17 0
0 -2 29 -0.68 2.15 0
0 -2 -29 0.99 1.61 0
0 2 29 0.18 2.24 0
1 -2 29 2.70 2.27 0
1 2 29 -0.12 2.35 0
3 -3 -29 -1.05 2.25 0
-3 -3 29 0.86 2.23 0
2 3 -29 0.67 2.20 0
-2 -3 29 -1.76 2.20 0
2 -3 -29 1.01 2.18 0
1 3 -29 1.96 2.25 0
-1 -3 29 -0.29 1.52 0
1 -3 -29 1.28 2.20 0
0 3 -29 -0.16 2.20 0
0 -3 29 -0.24 2.16 0
0 -3 -29 0.05 2.21 0
-2 -4 29 1.35 2.25 0
-1 -4 29 0.15 2.29 0
-2 0 30 0.98 1.62 0
-1 0 30 1.53 1.58 0
-2 1 30 -0.25 2.32 0
-2 -1 30 1.90 2.22 0
-1 1 30 2.64 2.26 0
-1 -1 30 0.34 2.20 0
;
_shelx_hkl_checksum 63988
_shelx_res_file
;
TITL shelxt_a.res in P2(1)/c
shelx.res
created by SHELXL-2018/3 at 19:55:42 on 12-Jan-2021
CELL 0.71073 7.4089 11.4544 21.9491 90.000 97.814 90.000
ZERR 4.00 0.0006 0.0014 0.0017 0.000 0.006 0.000
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H N O
UNIT 88 72 8 8
MERG 2
OMIT -2.00 50.10
MORE -1
DELU 0.010 C3 C2 C6 C1 C5 C4
SIMU 0.0020 C3 C2 C6 C1 C5 C4
ISOR 0.0100 C3 C2 C6 C1 C5 C4
EQIV $1 -x+1, 2-y, -z+1
HTAB O2 N2
HTAB C3 O2_$1
FMAP 2
PLAN 20
ACTA
BOND $H
CONF
LIST 6
L.S. 25
WGHT 0.138800 0.769600
FVAR 0.52887
N2 3 0.807293 0.598848 0.509052 11.00000 0.06560 0.06814 =
0.05307 -0.00648 -0.00173 0.00893
N1 3 0.726406 0.509793 0.470150 11.00000 0.07317 0.06934 =
0.04987 -0.00524 -0.00156 0.01039
O2 4 0.905500 0.813473 0.544429 11.00000 0.13732 0.06810 =
0.07645 0.00185 -0.01583 0.00963
AFIX 147
H2 2 0.866243 0.762928 0.519659 11.00000 -1.50000
AFIX 0
O1 4 0.830529 0.696055 0.373206 11.00000 0.12267 0.13711 =
0.08586 0.00999 0.03270 -0.04637
C16 1 0.952061 0.643768 0.610583 11.00000 0.05444 0.06980 =
0.05152 -0.00512 0.00620 0.01072
C9 1 0.571814 0.472148 0.368341 11.00000 0.05440 0.07586 =
0.05106 -0.00572 0.00800 0.00653
C15 1 0.872718 0.563439 0.563199 11.00000 0.05939 0.06671 =
0.05517 -0.00407 0.00675 0.01191
AFIX 43
H15 2 0.869084 0.484218 0.572232 11.00000 -1.20000
AFIX 0
C8 1 0.667374 0.548811 0.416033 11.00000 0.05455 0.07126 =
0.05003 0.00023 0.00630 0.00766
C21 1 1.012726 0.600824 0.669842 11.00000 0.06144 0.08280 =
0.04975 -0.00303 0.00764 0.00084
AFIX 43
H21 2 1.008655 0.520813 0.676726 11.00000 -1.20000
AFIX 0
C14 1 0.547535 0.353688 0.379110 11.00000 0.07710 0.07325 =
0.05841 -0.00166 0.00398 0.00581
AFIX 43
H14 2 0.592287 0.321938 0.417175 11.00000 -1.20000
AFIX 0
C20 1 1.078166 0.673144 0.718221 11.00000 0.05837 0.10335 =
0.05412 -0.01088 0.00513 0.00293
C7 1 0.701135 0.674848 0.399514 11.00000 0.08427 0.08530 =
0.04700 0.00510 0.00116 -0.01993
C17 1 0.962560 0.763251 0.599817 11.00000 0.07783 0.06955 =
0.06114 -0.00673 -0.00025 0.01170
C10 1 0.500807 0.517187 0.311105 11.00000 0.08716 0.08225 =
0.05062 -0.00267 0.00256 0.00251
AFIX 43
H10 2 0.513452 0.596328 0.303221 11.00000 -1.20000
AFIX 0
C13 1 0.457363 0.282650 0.333677 11.00000 0.08254 0.07634 =
0.08248 -0.01571 0.01001 0.00216
AFIX 43
H13 2 0.442179 0.203596 0.341196 11.00000 -1.20000
AFIX 0
C12 1 0.390042 0.329820 0.277101 11.00000 0.07254 0.10062 =
0.06765 -0.02868 0.00302 0.00615
AFIX 43
H12 2 0.329630 0.282317 0.246532 11.00000 -1.20000
AFIX 0
C19 1 1.087735 0.790568 0.705669 11.00000 0.07738 0.10457 =
0.06820 -0.02590 -0.00064 -0.00543
AFIX 43
H19 2 1.134050 0.840615 0.737345 11.00000 -1.20000
AFIX 0
C11 1 0.412039 0.445960 0.266002 11.00000 0.08711 0.10502 =
0.05442 -0.00902 -0.00173 0.00804
AFIX 43
H11 2 0.366915 0.477135 0.227836 11.00000 -1.20000
AFIX 0
C18 1 1.031694 0.837638 0.648146 11.00000 0.09795 0.07447 =
0.08651 -0.01565 0.00084 0.00093
AFIX 43
H18 2 1.039779 0.917581 0.641626 11.00000 -1.20000
AFIX 0
C22 1 1.137364 0.625796 0.782198 11.00000 0.09712 0.14663 =
0.05177 -0.00724 0.00009 -0.00977
AFIX 137
H22A 2 1.044825 0.641737 0.807719 11.00000 -1.50000
H22B 2 1.249168 0.662613 0.799408 11.00000 -1.50000
H22C 2 1.155645 0.543006 0.780046 11.00000 -1.50000
AFIX 0
C3 1 0.329982 0.932212 0.440658 11.00000 0.16320 0.10372 =
0.08460 -0.01129 -0.02832 0.03753
AFIX 43
H3 2 0.245666 0.989489 0.447121 11.00000 -1.20000
AFIX 0
C2 1 0.291935 0.818754 0.454413 11.00000 0.15679 0.10464 =
0.08168 -0.01290 -0.02317 0.03647
AFIX 43
H2A 2 0.188797 0.799054 0.472040 11.00000 -1.20000
AFIX 0
C6 1 0.572351 0.764542 0.414430 11.00000 0.15319 0.08362 =
0.06168 -0.00206 -0.02399 0.02374
C1 1 0.417733 0.733414 0.440383 11.00000 0.15011 0.09330 =
0.07065 -0.01004 -0.02203 0.03295
AFIX 43
H1 2 0.396996 0.655268 0.448600 11.00000 -1.20000
AFIX 0
C5 1 0.606864 0.882362 0.403885 11.00000 0.16508 0.09141 =
0.07309 0.00044 -0.02526 0.02167
AFIX 43
H5 2 0.710653 0.905524 0.387565 11.00000 -1.20000
AFIX 0
C4 1 0.478987 0.964438 0.418852 11.00000 0.16892 0.09743 =
0.08193 -0.00166 -0.02922 0.02759
AFIX 43
H4 2 0.500278 1.043459 0.413196 11.00000 -1.20000
AFIX 0
HKLF 4
REM shelxt_a.res in P2(1)/c
REM wR2 = 0.2869, GooF = S = 1.114, Restrained GooF = 1.224 for all data
REM R1 = 0.0847 for 1801 Fo > 4sig(Fo) and 0.1300 for all 3262 data
REM 237 parameters refined using 84 restraints
END
WGHT 0.1388 0.7697
REM Highest difference peak 0.497, deepest hole -0.449, 1-sigma level 0.051
Q1 1 0.6046 0.9821 0.4106 11.00000 0.05 0.50
Q2 1 0.2242 0.9024 0.4572 11.00000 0.05 0.49
Q3 1 0.3865 0.9719 0.4335 11.00000 0.05 0.47
Q4 1 0.4979 0.8828 0.4060 11.00000 0.05 0.30
Q5 1 0.7061 0.8662 0.3995 11.00000 0.05 0.25
Q6 1 0.2364 0.7597 0.4647 11.00000 0.05 0.24
Q7 1 0.7882 0.7815 0.3791 11.00000 0.05 0.16
Q8 1 0.7469 0.6630 0.5046 11.00000 0.05 0.14
Q9 1 0.7298 1.0220 0.4215 11.00000 0.05 0.14
Q10 1 0.3274 1.0724 0.4386 11.00000 0.05 0.14
Q11 1 0.7423 0.4177 0.4772 11.00000 0.05 0.13
Q12 1 0.6549 0.6174 0.4086 11.00000 0.05 0.12
Q13 1 0.6728 0.3314 0.4193 11.00000 0.05 0.12
Q14 1 0.3694 0.8609 0.4454 11.00000 0.05 0.12
Q15 1 0.8029 0.3699 0.3914 11.00000 0.05 0.12
Q16 1 0.7701 0.2650 0.4183 11.00000 0.05 0.11
Q17 1 0.3051 0.1259 0.3656 11.00000 0.05 0.11
Q18 1 0.1300 0.7287 0.4861 11.00000 0.05 0.11
Q19 1 0.4841 0.6381 0.3081 11.00000 0.05 0.11
Q20 1 0.9042 0.5812 0.4068 11.00000 0.05 0.11
;
_shelx_res_checksum 16738
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
N N2 0.8073(5) 0.5988(3) 0.50905(13) 0.0632(9) Uani d 1 . .
N N1 0.7264(5) 0.5098(3) 0.47015(13) 0.0650(9) Uani d 1 . .
O O2 0.9055(6) 0.8135(3) 0.54443(14) 0.0968(12) Uani d 1 . .
H H2 0.866243 0.762928 0.519659 0.145 Uiso calc 1 . .
O O1 0.8305(6) 0.6961(4) 0.37321(16) 0.1135(14) Uani d 1 . .
C C16 0.9521(5) 0.6438(4) 0.61058(16) 0.0587(10) Uani d 1 . .
C C9 0.5718(5) 0.4721(4) 0.36834(16) 0.0604(10) Uani d 1 . .
C C15 0.8727(5) 0.5634(4) 0.56320(16) 0.0605(10) Uani d 1 . .
H H15 0.869084 0.484218 0.572232 0.073 Uiso calc 1 . .
C C8 0.6674(5) 0.5488(3) 0.41603(16) 0.0587(10) Uani d 1 . .
C C21 1.0127(6) 0.6008(4) 0.66984(15) 0.0647(11) Uani d 1 . .
H H21 1.008655 0.520813 0.676726 0.078 Uiso calc 1 . .
C C14 0.5475(6) 0.3537(4) 0.37911(18) 0.0701(12) Uani d 1 . .
H H14 0.592287 0.321938 0.417175 0.084 Uiso calc 1 . .
C C20 1.0782(6) 0.6731(5) 0.71822(17) 0.0722(12) Uani d 1 . .
C C7 0.7011(7) 0.6748(4) 0.39951(17) 0.0729(12) Uani d 1 . .
C C17 0.9626(6) 0.7633(4) 0.59982(19) 0.0704(12) Uani d 1 . .
C C10 0.5008(6) 0.5172(4) 0.31111(17) 0.0740(12) Uani d 1 . .
H H10 0.513452 0.596328 0.303221 0.089 Uiso calc 1 . .
C C13 0.4574(7) 0.2826(4) 0.3337(2) 0.0806(13) Uani d 1 . .
H H13 0.442179 0.203596 0.341196 0.097 Uiso calc 1 . .
C C12 0.3900(7) 0.3298(5) 0.2771(2) 0.0809(14) Uani d 1 . .
H H12 0.329630 0.282317 0.246532 0.097 Uiso calc 1 . .
C C19 1.0877(7) 0.7906(5) 0.7057(2) 0.0844(15) Uani d 1 . .
H H19 1.134050 0.840615 0.737345 0.101 Uiso calc 1 . .
C C11 0.4120(7) 0.4460(5) 0.26600(19) 0.0832(14) Uani d 1 . .
H H11 0.366915 0.477135 0.227836 0.100 Uiso calc 1 . .
C C18 1.0317(7) 0.8376(4) 0.6481(2) 0.0874(14) Uani d 1 . .
H H18 1.039779 0.917581 0.641626 0.105 Uiso calc 1 . .
C C22 1.1374(8) 0.6258(6) 0.78220(19) 0.0994(18) Uani d 1 . .
H H22A 1.044825 0.641737 0.807719 0.149 Uiso calc 1 . .
H H22B 1.249168 0.662613 0.799408 0.149 Uiso calc 1 . .
H H22C 1.155645 0.543006 0.780046 0.149 Uiso calc 1 . .
C C3 0.3300(11) 0.9322(6) 0.4407(3) 0.1213(13) Uani d 1 . .
H H3 0.245666 0.989489 0.447121 0.146 Uiso calc 1 . .
C C2 0.2919(10) 0.8188(5) 0.4544(3) 0.1180(12) Uani d 1 . .
H H2A 0.188797 0.799054 0.472040 0.142 Uiso calc 1 . .
C C6 0.5724(10) 0.7645(5) 0.4144(2) 0.1031(12) Uani d 1 . .
C C1 0.4177(10) 0.7334(5) 0.4404(2) 0.1081(12) Uani d 1 . .
H H1 0.396996 0.655268 0.448600 0.130 Uiso calc 1 . .
C C5 0.6069(10) 0.8824(5) 0.4039(2) 0.1137(12) Uani d 1 . .
H H5 0.710653 0.905524 0.387565 0.136 Uiso calc 1 . .
C C4 0.4790(11) 0.9644(6) 0.4189(2) 0.1204(13) Uani d 1 . .
H H4 0.500278 1.043459 0.413196 0.144 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
N2 0.066(2) 0.068(2) 0.0531(17) 0.0089(17) -0.0017(14) -0.0065(15)
N1 0.073(2) 0.069(2) 0.0499(17) 0.0104(17) -0.0016(15) -0.0052(15)
O2 0.137(3) 0.0681(19) 0.076(2) 0.010(2) -0.0158(19) 0.0019(16)
O1 0.123(3) 0.137(3) 0.086(2) -0.046(3) 0.033(2) 0.010(2)
C16 0.054(2) 0.070(3) 0.0515(19) 0.0107(19) 0.0062(16) -0.0051(17)
C9 0.054(2) 0.076(3) 0.0511(19) 0.007(2) 0.0080(16) -0.0057(18)
C15 0.059(2) 0.067(2) 0.055(2) 0.0119(19) 0.0068(17) -0.0041(17)
C8 0.055(2) 0.071(3) 0.0500(19) 0.0077(19) 0.0063(16) 0.0002(17)
C21 0.061(3) 0.083(3) 0.050(2) 0.001(2) 0.0076(17) -0.0030(18)
C14 0.077(3) 0.073(3) 0.058(2) 0.006(2) 0.004(2) -0.002(2)
C20 0.058(3) 0.103(4) 0.054(2) 0.003(2) 0.0051(18) -0.011(2)
C7 0.084(3) 0.085(3) 0.047(2) -0.020(3) 0.001(2) 0.0051(19)
C17 0.078(3) 0.070(3) 0.061(2) 0.012(2) 0.000(2) -0.007(2)
C10 0.087(3) 0.082(3) 0.051(2) 0.003(2) 0.0026(19) -0.003(2)
C13 0.083(3) 0.076(3) 0.082(3) 0.002(2) 0.010(2) -0.016(2)
C12 0.073(3) 0.101(4) 0.068(3) 0.006(3) 0.003(2) -0.029(3)
C19 0.077(3) 0.105(4) 0.068(3) -0.005(3) -0.001(2) -0.026(3)
C11 0.087(4) 0.105(4) 0.054(2) 0.008(3) -0.002(2) -0.009(2)
C18 0.098(4) 0.074(3) 0.087(3) 0.001(3) 0.001(3) -0.016(2)
C22 0.097(4) 0.147(5) 0.052(2) -0.010(3) 0.000(2) -0.007(3)
C3 0.163(3) 0.104(2) 0.0846(19) 0.038(2) -0.0283(19) -0.0113(17)
C2 0.157(3) 0.105(2) 0.0817(18) 0.036(2) -0.0232(18) -0.0129(17)
C6 0.153(3) 0.0836(19) 0.0617(17) 0.024(2) -0.0240(17) -0.0021(16)
C1 0.150(3) 0.0933(19) 0.0707(18) 0.033(2) -0.0220(18) -0.0100(16)
C5 0.165(3) 0.0914(19) 0.0731(18) 0.022(2) -0.0253(18) 0.0004(16)
C4 0.169(3) 0.097(2) 0.0819(19) 0.028(2) -0.0292(19) -0.0017(17)
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
C15 N2 N1 . . 114.0(3) ?
C8 N1 N2 . . 111.7(3) ?
C17 O2 H2 . . 109.5 ?
C17 C16 C21 . . 118.9(4) ?
C17 C16 C15 . . 121.9(3) ?
C21 C16 C15 . . 119.2(4) ?
C14 C9 C10 . . 118.2(4) ?
C14 C9 C8 . . 121.4(3) ?
C10 C9 C8 . . 120.4(4) ?
N2 C15 C16 . . 121.8(4) ?
N2 C15 H15 . . 119.1 ?
C16 C15 H15 . . 119.1 ?
N1 C8 C9 . . 121.2(4) ?
N1 C8 C7 . . 120.3(3) ?
C9 C8 C7 . . 118.5(3) ?
C20 C21 C16 . . 122.4(4) ?
C20 C21 H21 . . 118.8 ?
C16 C21 H21 . . 118.8 ?
C13 C14 C9 . . 120.7(4) ?
C13 C14 H14 . . 119.7 ?
C9 C14 H14 . . 119.7 ?
C19 C20 C21 . . 117.0(4) ?
C19 C20 C22 . . 121.3(4) ?
C21 C20 C22 . . 121.7(5) ?
O1 C7 C6 . . 123.2(5) ?
O1 C7 C8 . . 118.2(5) ?
C6 C7 C8 . . 118.6(4) ?
O2 C17 C16 . . 123.4(4) ?
O2 C17 C18 . . 117.2(4) ?
C16 C17 C18 . . 119.5(4) ?
C11 C10 C9 . . 120.9(5) ?
C11 C10 H10 . . 119.6 ?
C9 C10 H10 . . 119.6 ?
C12 C13 C14 . . 119.7(5) ?
C12 C13 H13 . . 120.1 ?
C14 C13 H13 . . 120.1 ?
C11 C12 C13 . . 120.2(4) ?
C11 C12 H12 . . 119.9 ?
C13 C12 H12 . . 119.9 ?
C20 C19 C18 . . 123.1(4) ?
C20 C19 H19 . . 118.5 ?
C18 C19 H19 . . 118.5 ?
C12 C11 C10 . . 120.3(4) ?
C12 C11 H11 . . 119.8 ?
C10 C11 H11 . . 119.8 ?
C19 C18 C17 . . 119.1(5) ?
C19 C18 H18 . . 120.4 ?
C17 C18 H18 . . 120.4 ?
C20 C22 H22A . . 109.5 ?
C20 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
C20 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
C4 C3 C2 . . 123.6(7) ?
C4 C3 H3 . . 118.2 ?
C2 C3 H3 . . 118.2 ?
C3 C2 C1 . . 116.5(7) ?
C3 C2 H2A . . 121.8 ?
C1 C2 H2A . . 121.8 ?
C1 C6 C5 . . 119.6(6) ?
C1 C6 C7 . . 120.5(5) ?
C5 C6 C7 . . 119.9(7) ?
C6 C1 C2 . . 121.0(6) ?
C6 C1 H1 . . 119.5 ?
C2 C1 H1 . . 119.5 ?
C6 C5 C4 . . 117.6(7) ?
C6 C5 H5 . . 121.2 ?
C4 C5 H5 . . 121.2 ?
C3 C4 C5 . . 121.6(7) ?
C3 C4 H4 . . 119.2 ?
C5 C4 H4 . . 119.2 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
N2 C15 . 1.287(5) ?
N2 N1 . 1.411(4) ?
N1 C8 . 1.289(4) ?
O2 C17 . 1.359(5) ?
O2 H2 . 0.8200 ?
O1 C7 . 1.209(5) ?
C16 C17 . 1.393(6) ?
C16 C21 . 1.406(5) ?
C16 C15 . 1.452(5) ?
C9 C14 . 1.393(6) ?
C9 C10 . 1.393(5) ?
C9 C8 . 1.472(5) ?
C15 H15 . 0.9300 ?
C8 C7 . 1.518(6) ?
C21 C20 . 1.382(6) ?
C21 H21 . 0.9300 ?
C14 C13 . 1.386(6) ?
C14 H14 . 0.9300 ?
C20 C19 . 1.377(7) ?
C20 C22 . 1.514(6) ?
C7 C6 . 1.469(7) ?
C17 C18 . 1.402(6) ?
C10 C11 . 1.379(6) ?
C10 H10 . 0.9300 ?
C13 C12 . 1.384(6) ?
C13 H13 . 0.9300 ?
C12 C11 . 1.366(7) ?
C12 H12 . 0.9300 ?
C19 C18 . 1.384(7) ?
C19 H19 . 0.9300 ?
C11 H11 . 0.9300 ?
C18 H18 . 0.9300 ?
C22 H22A . 0.9600 ?
C22 H22B . 0.9600 ?
C22 H22C . 0.9600 ?
C3 C4 . 1.314(9) ?
C3 C2 . 1.372(9) ?
C3 H3 . 0.9300 ?
C2 C1 . 1.413(8) ?
C2 H2A . 0.9300 ?
C6 C1 . 1.393(9) ?
C6 C5 . 1.399(8) ?
C1 H1 . 0.9300 ?
C5 C4 . 1.405(9) ?
C5 H5 . 0.9300 ?
C4 H4 . 0.9300 ?
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
O2 H2 N2 . 0.82 1.94 2.650(5) 145.0 yes
C3 H3 O2 3_676 0.93 2.54 3.434(8) 162.0 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
C15 N2 N1 C8 . . . . -178.3(3) ?
N1 N2 C15 C16 . . . . -176.5(3) ?
C17 C16 C15 N2 . . . . -0.4(6) ?
C21 C16 C15 N2 . . . . 176.7(4) ?
N2 N1 C8 C9 . . . . -177.8(3) ?
N2 N1 C8 C7 . . . . 4.3(5) ?
C14 C9 C8 N1 . . . . -2.4(6) ?
C10 C9 C8 N1 . . . . 176.7(4) ?
C14 C9 C8 C7 . . . . 175.5(4) ?
C10 C9 C8 C7 . . . . -5.3(6) ?
C17 C16 C21 C20 . . . . 1.7(6) ?
C15 C16 C21 C20 . . . . -175.5(4) ?
C10 C9 C14 C13 . . . . 0.9(6) ?
C8 C9 C14 C13 . . . . -179.9(4) ?
C16 C21 C20 C19 . . . . -2.1(6) ?
C16 C21 C20 C22 . . . . 178.0(4) ?
N1 C8 C7 O1 . . . . 96.0(5) ?
C9 C8 C7 O1 . . . . -81.9(5) ?
N1 C8 C7 C6 . . . . -85.9(5) ?
C9 C8 C7 C6 . . . . 96.2(4) ?
C21 C16 C17 O2 . . . . -179.2(4) ?
C15 C16 C17 O2 . . . . -2.1(7) ?
C21 C16 C17 C18 . . . . -0.5(6) ?
C15 C16 C17 C18 . . . . 176.6(4) ?
C14 C9 C10 C11 . . . . -1.2(6) ?
C8 C9 C10 C11 . . . . 179.6(4) ?
C9 C14 C13 C12 . . . . -0.3(7) ?
C14 C13 C12 C11 . . . . -0.1(7) ?
C21 C20 C19 C18 . . . . 1.5(7) ?
C22 C20 C19 C18 . . . . -178.7(5) ?
C13 C12 C11 C10 . . . . -0.2(7) ?
C9 C10 C11 C12 . . . . 0.9(7) ?
C20 C19 C18 C17 . . . . -0.4(8) ?
O2 C17 C18 C19 . . . . 178.6(4) ?
C16 C17 C18 C19 . . . . -0.1(7) ?
C4 C3 C2 C1 . . . . -3.8(8) ?
O1 C7 C6 C1 . . . . 174.8(4) ?
C8 C7 C6 C1 . . . . -3.2(6) ?
O1 C7 C6 C5 . . . . -6.6(7) ?
C8 C7 C6 C5 . . . . 175.3(4) ?
C5 C6 C1 C2 . . . . 2.1(7) ?
C7 C6 C1 C2 . . . . -179.4(4) ?
C3 C2 C1 C6 . . . . 0.5(7) ?
C1 C6 C5 C4 . . . . -1.6(7) ?
C7 C6 C5 C4 . . . . 179.9(4) ?
C2 C3 C4 C5 . . . . 4.4(9) ?
C6 C5 C4 C3 . . . . -1.5(8) ?
_cod_database_fobs_code 2243839