#------------------------------------------------------------------------------
#$Date: 2024-05-06 07:19:57 +0300 (Mon, 06 May 2024) $
#$Revision: 291719 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/30/2023064.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_2023064
loop_
_publ_author_name
'Naghiyev, Farid N.'
'Khrustalev, Victor N.'
'Akkurt, Mehmet'
'Dobrokhotova, Ekaterina V.'
'Bhattarai, Ajaya'
'Khalilov, Ali N.'
'Mamedov, İbrahim G'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of
6-imino-8-(4-methyl-phen-yl)-1,3,4,6-tetra-hydro-2H-pyrido[1,2-a]pyrimidine-7,9-dicarbo-nitrile.
;
_journal_coeditor_code NX2006
_journal_issue 'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 378
_journal_page_last 382
_journal_paper_doi 10.1107/S2056989024002500
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C17 H15 N5'
_chemical_formula_moiety 'C17 H15 N5'
_chemical_formula_sum 'C17 H15 N5'
_chemical_formula_weight 289.34
_chemical_name_systematic
6-Imino-8-(4-methylphenyl)-1,3,4,6-tetrahydro-2H-pyrido[1,2-a]pyrimidine-7,9-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 mixed
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 92.435(7)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 6.2459(4)
_cell_length_b 14.1480(9)
_cell_length_c 16.2111(11)
_cell_measurement_reflns_used 600
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 26.0
_cell_measurement_theta_min 2.6
_cell_volume 1431.23(16)
_computing_cell_refinement
;
iMosflm (Battye et al., 2011)
;
_computing_data_collection
;
Marccd (Doyle, 2011)
;
_computing_data_reduction
;
iMosflm (Battye et al., 2011)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Rayonix SX165 CCD'
_diffrn_measurement_method '/f scan'
_diffrn_radiation_type synchrotron
_diffrn_radiation_wavelength 0.74500
_diffrn_reflns_av_R_equivalents 0.0486
_diffrn_reflns_av_unetI/netI 0.0338
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 16784
_diffrn_reflns_theta_full 26.551
_diffrn_reflns_theta_max 31.024
_diffrn_reflns_theta_min 2.636
_exptl_absorpt_coefficient_mu 0.093
_exptl_absorpt_correction_T_max 0.989
_exptl_absorpt_correction_T_min 0.981
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(Scala; Evans, 2006)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.343
_exptl_crystal_description needle
_exptl_crystal_F_000 608
_exptl_crystal_size_max 0.130
_exptl_crystal_size_mid 0.030
_exptl_crystal_size_min 0.010
_refine_diff_density_max 0.303
_refine_diff_density_min -0.244
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.039
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 206
_refine_ls_number_reflns 3956
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.039
_refine_ls_R_factor_all 0.0611
_refine_ls_R_factor_gt 0.0446
_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^)+(0.0455P)^2^+0.6432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1035
_refine_ls_wR_factor_ref 0.1132
_reflns_number_gt 3119
_reflns_number_total 3956
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file nx2006.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2023064.cif.'
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2023064
_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 0.988
_shelx_estimated_absorpt_t_max 0.999
_shelx_hkl_file
;
0 0 1 -2.66 1.97
0 0 1 -4.43 2.04
0 0 -1 -0.27 2.01
0 0 -1 -1.18 2.13
0 0 2 988.70 27.62
0 0 2 959.90 26.76
0 0 -2 986.70 27.59
0 0 -2 946.50 26.38
0 0 3 -3.54 5.76
0 0 3 2.88 5.84
0 0 -3 4.97 6.30
0 0 -3 1.37 5.99
0 0 4 47.28 7.17
0 0 4 43.44 7.07
0 0 -4 49.81 7.68
0 0 -4 41.63 7.12
0 0 5 -0.59 6.62
0 0 5 5.62 6.84
0 0 -5 -13.90 7.96
0 0 -5 -0.59 6.47
0 0 6 211.30 10.51
0 0 6 194.90 9.82
0 0 -6 217.40 10.11
0 0 7 5.88 6.17
0 0 7 -3.78 6.07
0 0 -7 -8.92 6.84
0 0 8 663.20 20.81
0 0 8 665.80 21.41
0 0 -8 632.90 20.17
0 0 9 4.52 6.85
0 0 9 -0.69 6.12
0 0 -9 7.94 6.42
0 0 10 63.72 7.35
0 0 10 57.75 7.00
0 0 -10 49.38 7.10
0 0 11 8.18 6.57
0 0 11 4.28 7.13
0 0 -11 0.13 6.30
0 0 12 203.90 10.62
0 0 12 204.70 10.32
0 0 -12 216.70 10.65
0 0 13 3.88 6.64
0 0 13 13.55 6.68
0 0 -13 0.64 6.55
0 0 14 320.10 13.28
0 0 14 347.30 13.95
0 0 -14 334.50 13.38
0 0 15 -3.29 7.07
0 0 15 6.95 7.70
0 0 -15 -1.73 5.94
0 0 16 474.90 17.36
0 0 16 444.70 16.55
0 0 -16 440.20 16.44
0 0 17 7.03 6.94
0 0 17 10.46 7.13
0 0 -17 0.47 6.91
0 0 18 70.53 8.46
0 0 18 81.36 7.81
0 0 -18 69.50 7.68
0 0 19 13.34 6.89
0 0 19 -0.99 6.95
0 0 -19 -3.24 6.08
0 0 20 32.31 7.82
0 0 20 57.06 7.27
0 0 -20 40.50 7.18
0 0 21 -2.00 6.78
0 0 21 2.74 6.19
0 0 -21 1.20 7.28
0 0 22 334.00 12.38
0 0 22 361.20 13.71
0 0 -22 367.80 12.96
0 1 -22 26.44 6.36
0 -1 22 23.53 6.65
0 -1 22 34.87 6.89
0 1 -21 111.70 8.62
0 -1 21 86.99 8.10
0 -1 21 94.24 7.71
0 1 -20 52.80 7.17
0 -1 20 49.99 7.51
0 -1 20 64.47 7.05
0 1 -19 60.91 7.47
0 -1 19 49.91 7.65
0 -1 19 45.66 7.06
0 1 -18 173.70 9.86
0 -1 18 157.30 9.73
0 -1 18 171.30 9.89
0 1 -17 6.47 6.94
0 -1 17 3.30 6.94
0 -1 17 8.87 7.30
0 1 -16 60.71 7.77
0 -1 16 67.71 8.07
0 -1 16 51.82 8.31
0 1 -15 94.98 8.30
0 -1 15 84.15 8.57
0 -1 15 84.12 9.09
0 1 -14 2.85 6.04
0 -1 14 0.45 6.51
0 -1 14 -5.38 6.68
0 1 -13 144.10 9.45
0 1 -12 3.08 6.37
0 -1 12 10.80 6.93
0 -1 12 0.61 6.63
0 1 -11 21.48 6.31
0 -1 11 23.51 6.54
0 -1 11 24.54 7.10
0 1 -10 158.20 8.86
0 -1 10 134.00 8.86
0 -1 10 144.50 8.65
0 1 -9 198.40 9.96
0 -1 9 184.10 9.99
0 -1 9 189.00 9.54
0 1 -8 1138.00 33.55
0 -1 8 1142.00 33.62
0 -1 8 1131.00 33.02
0 1 -7 3151.00 86.43
0 -1 7 2933.00 80.53
0 -1 7 3058.00 83.90
0 1 -6 207.30 9.61
0 -1 6 194.00 9.68
0 -1 6 188.70 9.78
0 1 -5 1168.00 34.06
0 -1 5 1190.00 34.62
0 -1 5 1235.00 35.65
0 1 -4 352.80 13.33
0 -1 4 339.90 12.93
0 1 -3 581.70 18.28
0 -1 3 563.60 17.70
0 1 -2 92.13 5.70
0 -1 2 92.21 5.95
0 1 0 1.44 2.47
0 -1 0 -3.21 2.21
0 1 2 88.49 5.84
0 1 2 97.50 6.11
0 -1 -2 100.90 6.46
0 -1 -2 100.40 5.99
0 1 3 564.40 17.99
0 1 3 562.50 17.71
0 -1 -3 603.40 19.20
0 -1 -3 605.50 18.70
0 1 4 352.60 13.41
0 1 4 352.10 13.49
0 -1 -4 342.10 13.09
0 -1 -4 362.00 14.01
0 1 5 1199.00 34.92
0 1 5 1162.00 34.02
0 -1 -5 1212.00 35.60
0 -1 -5 1113.00 32.45
0 1 6 209.50 10.34
0 1 6 217.10 10.58
0 -1 -6 214.10 10.14
0 -1 -6 209.00 10.68
0 1 7 3156.00 86.45
0 1 7 3103.00 85.11
0 -1 -7 3078.00 84.53
0 -1 -7 2952.00 81.08
0 1 8 1126.00 32.92
0 1 8 1143.00 33.72
0 -1 -8 1170.00 34.06
0 -1 -8 1160.00 33.84
0 1 9 195.20 10.19
0 1 9 195.60 9.99
0 -1 -9 209.00 10.67
0 -1 -9 202.80 9.92
0 1 10 143.80 8.79
0 1 10 137.70 9.04
0 -1 -10 155.60 9.11
0 1 11 10.59 6.74
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0 1 12 -1.86 6.59
0 -1 -12 -7.52 6.60
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0 1 13 124.00 9.12
0 -1 -13 129.20 9.09
0 1 14 -6.37 7.82
0 1 14 1.70 6.45
0 -1 -14 2.49 5.97
0 1 15 78.34 8.25
0 1 15 95.43 9.06
0 -1 -15 109.30 8.14
0 1 16 48.93 7.72
0 1 16 62.94 8.17
0 -1 -16 58.64 7.33
0 1 17 12.22 7.13
0 1 17 13.48 7.08
0 -1 -17 11.04 6.38
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0 1 18 173.20 10.25
0 -1 -18 160.10 9.20
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0 2 -14 446.50 16.11
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0 -2 12 430.00 15.72
0 -2 12 439.40 16.33
0 2 -11 218.30 11.00
0 -2 11 190.70 9.75
0 -2 11 209.30 10.77
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0 -2 7 2943.00 80.82
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0 -2 6 6183.00 166.70
0 2 -5 141.50 8.30
0 -2 5 147.90 8.64
0 2 -4 1.76 7.11
0 -2 4 0.32 6.21
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0 -2 3 1832.00 50.80
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0 -2 1 560.10 16.65
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0 2 4 -1.08 7.24
0 -2 -4 1.89 7.32
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0 2 5 168.10 9.47
0 -2 -5 157.90 9.04
0 -2 -5 163.30 9.66
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0 2 6 5967.00 161.00
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0 -2 -6 6248.00 168.70
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0 -2 -9 -11.57 6.34
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0 2 10 329.20 13.17
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0 2 11 186.30 10.43
0 -2 -11 177.30 9.75
0 -2 -11 183.80 10.40
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0 2 12 410.30 15.60
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0 2 17 60.76 7.85
0 2 17 46.61 8.41
0 -2 -17 70.45 7.27
0 2 18 66.81 8.35
0 2 18 70.32 8.23
0 -2 -18 75.71 7.39
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0 2 19 3.48 6.95
0 2 20 5.50 7.03
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0 2 22 9.22 6.04
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0 -3 12 186.30 10.20
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0 -3 4 105.00 7.53
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0 -3 3 5788.00 155.90
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0 -3 0 -0.75 6.77
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0 3 4 108.70 8.74
0 -3 -4 121.40 8.84
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0 3 10 203.20 10.34
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0 -4 18 142.30 9.06
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0 -4 17 153.60 8.74
0 -4 17 179.80 10.03
0 4 -16 326.70 12.85
0 -4 16 314.80 12.56
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0 4 -13 9.56 6.06
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0 4 -11 22.48 6.52
0 -4 11 17.30 6.09
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0 -4 10 243.40 10.70
0 -4 10 232.40 10.99
0 4 -9 353.60 13.86
0 -4 9 337.70 13.16
0 4 -8 10.01 6.18
0 -4 8 9.95 6.02
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0 -4 3 1785.00 50.01
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0 -4 2 3338.00 90.90
0 4 -1 1576.00 44.58
0 -4 1 1517.00 42.72
0 4 1 1710.00 48.34
0 -4 -1 1664.00 46.90
0 4 2 3463.00 94.45
0 -4 -2 3312.00 90.48
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8 3 3 125.00 7.68
8 3 3 127.60 8.26
-8 -2 -7 1.68 6.44
8 2 7 -0.62 8.69
8 2 7 3.19 7.27
-8 -2 -6 227.00 10.30
-8 -2 -5 9.49 6.13
8 2 5 2.78 8.23
8 2 5 13.82 6.94
-8 -2 -4 376.90 13.84
8 2 4 376.70 14.70
8 2 4 427.30 15.16
-8 -2 -3 49.45 6.69
8 2 3 43.88 6.84
8 2 3 50.49 8.03
-8 -2 -2 45.48 6.32
8 2 2 54.70 6.34
8 2 2 38.54 6.95
-8 -2 -1 2.67 5.09
8 2 1 -4.35 5.14
8 2 1 0.43 4.59
-8 -2 0 42.57 4.13
-8 -1 -7 0.94 7.21
8 1 7 3.38 7.76
8 1 7 4.52 6.83
-8 -1 -6 12.03 5.72
8 1 6 14.30 6.83
8 1 6 6.93 9.85
-8 -1 -5 2.87 5.47
8 1 5 -6.34 6.49
8 1 5 -5.70 8.65
-8 -1 -4 -0.28 5.62
8 1 4 -4.63 7.89
8 1 4 0.67 6.78
-8 -1 -3 45.13 6.08
8 1 3 50.98 8.34
8 1 3 47.90 6.73
-8 -1 -2 65.60 6.90
8 1 2 75.66 8.39
8 1 2 64.33 6.91
-8 -1 -1 74.75 6.50
-8 -1 0 57.94 5.66
8 1 0 60.12 6.86
8 1 0 53.39 5.69
-8 -1 1 26.59 4.49
8 1 -1 7.47 4.76
8 1 -1 17.07 4.42
-8 0 -7 -12.31 8.26
8 0 7 -1.27 7.20
8 0 7 3.20 6.48
-8 0 -6 -7.06 5.99
8 0 6 -0.32 6.92
8 0 6 7.47 8.07
-8 0 -5 -0.13 5.13
8 0 5 -6.02 8.94
8 0 5 8.59 6.97
-8 0 -4 9.09 5.25
8 0 4 -6.68 7.10
8 0 4 5.02 8.63
-8 0 -3 -8.46 5.18
8 0 3 -6.78 6.85
8 0 3 -3.38 8.29
-8 0 -2 8.65 5.34
8 0 2 18.07 6.97
8 0 2 9.77 7.99
-8 0 -1 10.14 5.93
8 0 1 -2.52 6.49
8 0 1 8.21 7.51
-8 0 0 408.60 14.16
8 0 0 405.50 14.93
8 0 0 399.40 13.79
-8 0 1 6.41 5.81
8 0 -1 -0.73 5.54
8 0 -1 6.11 7.05
-8 0 2 29.58 5.42
8 0 -2 18.64 5.36
8 0 -2 23.68 6.09
-8 0 3 -3.65 4.86
8 0 -3 3.27 5.21
8 0 -3 3.80 4.52
-8 0 4 83.54 5.10
-8 0 4 75.90 5.77
-8 1 -7 3.50 7.07
8 -1 7 8.69 7.52
8 -1 7 -5.13 6.28
-8 1 -6 -0.74 6.86
8 -1 6 -2.32 7.69
8 -1 6 1.10 6.40
-8 1 -5 -3.89 5.60
8 -1 5 -2.18 8.17
8 -1 5 0.20 7.92
-8 1 -4 -0.11 4.92
8 -1 4 10.39 9.89
8 -1 4 -3.69 8.48
-8 1 -3 51.15 5.99
8 -1 3 60.74 9.32
8 -1 3 39.39 8.90
-8 1 -2 82.48 6.75
8 -1 2 79.53 8.89
-8 1 -1 68.00 6.19
8 -1 1 78.47 9.21
-8 1 0 68.49 6.58
8 -1 0 56.85 8.90
-8 1 1 30.45 6.21
8 -1 -1 28.69 8.13
-8 1 2 17.64 6.25
8 -1 -2 26.54 7.46
-8 1 3 24.73 6.11
8 -1 -3 39.02 7.89
-8 1 4 40.26 6.45
8 -1 -4 38.34 7.11
-8 1 5 218.00 9.30
-8 1 5 204.80 9.21
8 -1 -5 212.70 10.38
-8 1 6 26.19 5.97
-8 1 6 7.62 5.67
8 -1 -6 19.33 6.20
-8 1 7 6.81 5.75
-8 1 7 12.08 5.76
8 -1 -7 5.94 5.57
-8 1 8 11.77 6.24
-8 1 8 2.59 5.38
8 -1 -8 1.41 5.01
-8 1 9 5.26 6.56
-8 1 9 5.20 6.03
8 -1 -9 5.87 5.32
-8 2 -7 11.04 7.28
8 -2 7 4.37 7.52
8 -2 7 2.96 5.92
-8 2 -6 139.60 9.30
8 -2 6 238.90 10.25
8 -2 6 213.30 11.51
-8 2 -5 1.46 6.07
8 -2 5 4.57 8.06
-8 2 -4 421.70 14.48
8 -2 4 407.70 15.75
-8 2 -3 54.99 5.78
8 -2 3 51.68 8.73
-8 2 -2 41.88 5.48
8 -2 2 77.04 9.83
-8 2 -1 0.07 4.93
8 -2 1 13.95 9.17
-8 2 0 26.87 6.09
8 -2 0 38.32 9.00
-8 2 1 29.97 6.13
8 -2 -1 25.73 8.97
-8 2 2 4.45 5.28
8 -2 -2 7.78 7.57
-8 2 3 1.75 5.84
8 -2 -3 1.79 8.48
-8 2 4 41.37 7.14
8 -2 -4 40.23 8.32
-8 2 5 2.81 6.03
8 -2 -5 -9.53 7.48
-8 2 6 -1.84 6.75
-8 2 6 -4.07 6.50
8 -2 -6 -1.71 7.61
-8 2 7 31.90 6.83
-8 2 7 54.39 7.37
8 -2 -7 33.22 7.79
-8 2 8 4.28 6.58
-8 2 8 3.68 7.33
8 -2 -8 -0.29 6.91
8 -2 -9 0.18 8.74
-8 3 -6 1.24 7.12
8 -3 6 27.00 8.09
-8 3 -5 34.67 6.81
8 -3 5 24.94 8.71
-8 3 -4 51.84 6.87
8 -3 4 41.35 8.13
-8 3 -3 125.80 7.79
8 -3 3 132.20 10.30
-8 3 -2 51.44 6.59
8 -3 2 67.83 9.68
-8 3 -1 103.70 7.09
8 -3 1 89.89 9.68
-8 3 0 2.11 5.55
8 -3 0 22.57 8.91
-8 3 1 33.48 5.84
8 -3 -1 29.36 9.12
-8 3 2 1.72 5.99
8 -3 -2 -5.19 7.78
-8 3 3 26.24 6.00
8 -3 -3 45.64 9.29
-8 3 4 -0.36 6.78
8 -3 -4 -3.63 8.77
-8 3 5 24.48 7.23
8 -3 -5 15.76 9.04
-8 3 6 259.70 11.55
8 -3 -6 278.20 12.76
-8 3 7 18.18 7.13
-8 3 7 32.42 7.63
8 -3 -7 36.33 8.57
-8 3 8 8.76 7.88
-8 3 8 11.59 8.84
8 -3 -8 5.27 8.14
-8 4 -6 -3.81 8.26
8 -4 6 12.38 7.49
-8 4 -5 4.60 7.77
8 -4 5 9.15 7.42
-8 4 -4 20.29 7.02
8 -4 4 8.45 7.76
-8 4 -3 196.40 10.19
8 -4 3 182.40 11.12
-8 4 -2 209.00 10.10
8 -4 2 211.30 11.59
-8 4 -1 11.83 6.15
8 -4 1 -3.70 8.77
-8 4 0 410.00 14.82
8 -4 0 445.20 17.01
-8 4 1 -0.78 5.59
8 -4 -1 -5.24 8.38
-8 4 2 18.36 5.80
8 -4 -2 11.06 8.78
-8 4 3 8.46 6.38
8 -4 -3 19.57 9.64
-8 4 4 5.23 6.15
8 -4 -4 9.73 10.03
-8 4 5 3.78 6.24
8 -4 -5 2.48 10.27
-8 4 6 -6.35 6.76
8 -4 -6 -5.14 9.52
-8 4 7 1.11 6.80
-8 4 7 16.47 7.19
8 -4 -7 -1.06 8.67
-8 5 -5 7.56 8.81
8 -5 5 13.01 7.10
-8 5 -4 4.82 8.12
8 -5 4 9.44 6.87
-8 5 -3 8.97 7.68
8 -5 3 14.73 6.82
-8 5 -2 28.70 7.18
8 -5 2 15.18 9.01
-8 5 -1 670.90 21.65
8 -5 1 644.50 21.29
-8 5 0 25.70 7.01
8 -5 0 25.73 8.72
-8 5 1 10.13 7.08
8 -5 -1 -12.41 8.33
-8 5 2 90.47 8.45
8 -5 -2 93.34 9.69
-8 5 3 44.58 7.33
8 -5 -3 51.44 8.82
-8 5 4 4.61 6.95
8 -5 -4 8.90 9.14
-8 5 5 52.35 8.14
8 -5 -5 53.41 9.66
-8 5 6 18.70 6.92
8 -5 -6 10.59 8.66
8 -5 -7 91.02 10.36
-8 6 -3 6.96 8.49
8 -6 3 132.50 8.34
-8 6 -2 33.71 7.88
8 -6 2 62.55 7.43
-8 6 -1 78.28 9.07
8 -6 1 69.55 8.13
-8 6 0 30.65 7.29
8 -6 0 29.59 8.19
-8 6 1 22.66 7.91
8 -6 -1 23.93 7.78
-8 6 2 13.55 7.51
8 -6 -2 -2.82 7.59
-8 6 3 21.43 7.96
8 -6 -3 4.05 8.04
-8 6 4 -5.08 9.13
8 -6 -4 10.32 8.62
-8 6 5 5.24 9.93
8 -6 -5 -4.20 7.59
-8 7 -1 17.13 9.34
8 -7 1 19.02 7.28
-8 7 0 19.54 8.70
8 -7 0 -6.34 6.34
-8 7 1 14.34 8.74
8 -7 -1 4.50 6.65
-8 7 2 -3.08 8.21
8 -7 -2 -0.06 6.40
-8 7 3 4.22 8.79
8 -7 -3 19.22 7.22
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 66617
_shelx_res_file
;
TITL T-320 in P2(1)/c
shelx.res
created by SHELXL-2018/3 at 17:42:04 on 08-Mar-2024
CELL 0.74500 6.2459 14.1480 16.2111 90.000 92.435 90.000
ZERR 4.00 0.0004 0.0009 0.0011 0.000 0.007 0.000
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H N
DISP C 0.004 0.0018 12.639
DISP H -0 0 0.6258
DISP N 0.0074 0.0036 21.8413
UNIT 68 60 20
MERG 2
FMAP 2
PLAN 5
SIZE 0.010 0.030 0.130
ACTA
BOND $H
CONF
L.S. 13
TEMP -173.00
WGHT 0.045500 0.643200
FVAR 1.10903
N1 3 1.228462 0.859620 0.435978 11.00000 0.01966 0.02260 =
0.01876 -0.00233 0.00258 -0.00251
H1 2 1.338372 0.896805 0.451938 11.00000 -1.20000
C2 1 1.241736 0.806202 0.359399 11.00000 0.02396 0.02268 =
0.01892 -0.00171 0.00362 -0.00041
AFIX 23
H2A 2 1.303447 0.742845 0.370787 11.00000 -1.20000
H2B 2 1.334227 0.839650 0.320792 11.00000 -1.20000
AFIX 0
C3 1 1.016502 0.797181 0.322198 11.00000 0.02489 0.02269 =
0.01741 -0.00146 0.00102 0.00006
AFIX 23
H3A 2 1.018198 0.760667 0.270134 11.00000 -1.20000
H3B 2 0.957031 0.860657 0.309545 11.00000 -1.20000
AFIX 0
C4 1 0.878671 0.747162 0.383294 11.00000 0.02364 0.02295 =
0.01948 -0.00351 0.00067 -0.00212
AFIX 23
H4A 2 0.726345 0.751480 0.364155 11.00000 -1.20000
H4B 2 0.918397 0.679453 0.385898 11.00000 -1.20000
AFIX 0
N5 3 0.905624 0.789391 0.467056 11.00000 0.01933 0.01994 =
0.01728 -0.00104 0.00108 -0.00078
C6 1 0.743720 0.767175 0.522085 11.00000 0.01859 0.02066 =
0.01947 0.00157 0.00115 -0.00041
N6 3 0.602516 0.706367 0.497204 11.00000 0.02399 0.02639 =
0.02361 -0.00150 0.00226 -0.00547
H6 2 0.504365 0.696342 0.539002 11.00000 -1.20000
C7 1 0.759050 0.814779 0.601714 11.00000 0.01947 0.01944 =
0.01857 0.00102 0.00214 -0.00057
C8 1 0.916507 0.880515 0.622067 11.00000 0.01825 0.01881 =
0.01734 0.00131 0.00038 0.00267
C9 1 1.073400 0.898456 0.564215 11.00000 0.01790 0.01914 =
0.01813 0.00027 0.00000 -0.00118
C9A 1 1.070544 0.848598 0.487733 11.00000 0.01704 0.01749 =
0.01839 0.00194 -0.00038 0.00141
C10 1 0.601329 0.786736 0.657818 11.00000 0.02348 0.02164 =
0.02030 -0.00132 0.00150 -0.00123
N10 3 0.467371 0.759988 0.698627 11.00000 0.03154 0.02842 =
0.02784 -0.00062 0.00825 -0.00523
C11 1 0.919758 0.931413 0.702289 11.00000 0.01952 0.01877 =
0.01726 0.00076 0.00165 -0.00087
C12 1 1.105794 0.939592 0.752786 11.00000 0.02040 0.02143 =
0.02003 0.00197 0.00129 0.00016
AFIX 43
H12 2 1.235238 0.911116 0.736637 11.00000 -1.20000
AFIX 0
C13 1 1.101568 0.989492 0.826820 11.00000 0.02159 0.02460 =
0.02077 0.00093 -0.00113 -0.00286
AFIX 43
H13 2 1.228854 0.994184 0.860790 11.00000 -1.20000
AFIX 0
C14 1 0.914982 1.032642 0.852145 11.00000 0.02564 0.02103 =
0.01913 -0.00091 0.00232 -0.00244
C15 1 0.729550 1.022846 0.801843 11.00000 0.02182 0.02111 =
0.02331 -0.00032 0.00293 0.00184
AFIX 43
H15 2 0.599979 1.050941 0.818303 11.00000 -1.20000
AFIX 0
C16 1 0.730668 0.972930 0.728333 11.00000 0.01902 0.02147 =
0.02072 0.00091 0.00029 -0.00079
AFIX 43
H16 2 0.602065 0.966821 0.695323 11.00000 -1.20000
AFIX 0
C17 1 0.908759 1.090513 0.929905 11.00000 0.03281 0.02927 =
0.02324 -0.00765 -0.00016 0.00088
AFIX 137
H17A 2 1.047423 1.086173 0.960301 11.00000 -1.50000
H17B 2 0.795831 1.066382 0.964407 11.00000 -1.50000
H17C 2 0.878970 1.156666 0.915642 11.00000 -1.50000
AFIX 0
C18 1 1.231622 0.969478 0.575324 11.00000 0.02036 0.02125 =
0.01541 -0.00006 0.00043 0.00218
N18 3 1.362927 1.027169 0.578594 11.00000 0.02228 0.02500 =
0.02111 -0.00042 -0.00030 -0.00196
HKLF 4
REM T-320 in P2(1)/c
REM wR2 = 0.1132, GooF = S = 1.039, Restrained GooF = 1.039 for all data
REM R1 = 0.0446 for 3119 Fo > 4sig(Fo) and 0.0611 for all 3956 data
REM 206 parameters refined using 0 restraints
END
WGHT 0.0455 0.6432
REM Highest difference peak 0.303, deepest hole -0.244, 1-sigma level 0.049
Q1 1 1.0682 0.8773 0.5293 11.00000 0.05 0.30
Q2 1 0.9157 0.9080 0.6591 11.00000 0.05 0.28
Q3 1 1.0235 0.9427 0.7209 11.00000 0.05 0.28
Q4 1 0.7644 0.7888 0.5637 11.00000 0.05 0.27
Q5 1 1.1296 0.7956 0.3428 11.00000 0.05 0.25
;
_shelx_res_checksum 42651
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 N1 1.22846(18) 0.85962(8) 0.43598(6) 0.0203(2) Uani d 1 . .
H H1 1.338(3) 0.8968(12) 0.4519(10) 0.024 Uiso d 1 . .
C C2 1.2417(2) 0.80620(10) 0.35940(7) 0.0218(2) Uani d 1 . .
H H2A 1.303447 0.742845 0.370787 0.026 Uiso calc 1 . .
H H2B 1.334227 0.839650 0.320792 0.026 Uiso calc 1 . .
C C3 1.0165(2) 0.79718(10) 0.32220(7) 0.0217(2) Uani d 1 . .
H H3A 1.018198 0.760667 0.270134 0.026 Uiso calc 1 . .
H H3B 0.957031 0.860657 0.309545 0.026 Uiso calc 1 . .
C C4 0.8787(2) 0.74716(9) 0.38329(8) 0.0220(3) Uani d 1 . .
H H4A 0.726345 0.751480 0.364155 0.026 Uiso calc 1 . .
H H4B 0.918397 0.679453 0.385898 0.026 Uiso calc 1 . .
N N5 0.90562(17) 0.78939(8) 0.46706(6) 0.0188(2) Uani d 1 . .
C C6 0.7437(2) 0.76717(9) 0.52209(7) 0.0196(2) Uani d 1 . .
N N6 0.60252(19) 0.70637(8) 0.49720(7) 0.0246(2) Uani d 1 . .
H H6 0.504(3) 0.6963(13) 0.5390(11) 0.030 Uiso d 1 . .
C C7 0.7591(2) 0.81478(9) 0.60171(7) 0.0191(2) Uani d 1 . .
C C8 0.91651(19) 0.88052(9) 0.62207(7) 0.0181(2) Uani d 1 . .
C C9 1.07340(19) 0.89846(9) 0.56422(7) 0.0184(2) Uani d 1 . .
C C9A 1.07054(19) 0.84860(9) 0.48773(7) 0.0177(2) Uani d 1 . .
C C10 0.6013(2) 0.78674(9) 0.65782(8) 0.0218(3) Uani d 1 . .
N N10 0.4674(2) 0.75999(9) 0.69863(8) 0.0291(3) Uani d 1 . .
C C11 0.91976(19) 0.93141(9) 0.70229(7) 0.0185(2) Uani d 1 . .
C C12 1.1058(2) 0.93959(9) 0.75279(7) 0.0206(2) Uani d 1 . .
H H12 1.235238 0.911116 0.736637 0.025 Uiso calc 1 . .
C C13 1.1016(2) 0.98949(10) 0.82682(8) 0.0224(3) Uani d 1 . .
H H13 1.228854 0.994184 0.860790 0.027 Uiso calc 1 . .
C C14 0.9150(2) 1.03264(9) 0.85215(8) 0.0219(3) Uani d 1 . .
C C15 0.7295(2) 1.02285(9) 0.80184(8) 0.0220(3) Uani d 1 . .
H H15 0.599979 1.050941 0.818303 0.026 Uiso calc 1 . .
C C16 0.7307(2) 0.97293(9) 0.72833(7) 0.0204(2) Uani d 1 . .
H H16 0.602065 0.966821 0.695323 0.025 Uiso calc 1 . .
C C17 0.9088(2) 1.09051(11) 0.92991(8) 0.0285(3) Uani d 1 . .
H H17A 1.047423 1.086173 0.960301 0.043 Uiso calc 1 . .
H H17B 0.795831 1.066382 0.964407 0.043 Uiso calc 1 . .
H H17C 0.878970 1.156666 0.915642 0.043 Uiso calc 1 . .
C C18 1.2316(2) 0.96948(9) 0.57532(7) 0.0190(2) Uani d 1 . .
N N18 1.36293(18) 1.02717(8) 0.57859(7) 0.0228(2) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
N1 0.0197(5) 0.0226(5) 0.0188(5) -0.0025(4) 0.0026(4) -0.0023(4)
C2 0.0240(6) 0.0227(6) 0.0189(5) -0.0004(5) 0.0036(4) -0.0017(5)
C3 0.0249(6) 0.0227(6) 0.0174(5) 0.0001(5) 0.0010(4) -0.0015(4)
C4 0.0236(6) 0.0229(6) 0.0195(5) -0.0021(5) 0.0007(4) -0.0035(4)
N5 0.0193(5) 0.0199(5) 0.0173(4) -0.0008(4) 0.0011(4) -0.0010(4)
C6 0.0186(5) 0.0207(6) 0.0195(5) -0.0004(5) 0.0011(4) 0.0016(4)
N6 0.0240(5) 0.0264(6) 0.0236(5) -0.0055(5) 0.0023(4) -0.0015(4)
C7 0.0195(5) 0.0194(6) 0.0186(5) -0.0006(5) 0.0021(4) 0.0010(4)
C8 0.0182(5) 0.0188(6) 0.0173(5) 0.0027(5) 0.0004(4) 0.0013(4)
C9 0.0179(5) 0.0191(6) 0.0181(5) -0.0012(5) 0.0000(4) 0.0003(4)
C9A 0.0170(5) 0.0175(5) 0.0184(5) 0.0014(4) -0.0004(4) 0.0019(4)
C10 0.0235(6) 0.0216(6) 0.0203(5) -0.0012(5) 0.0015(5) -0.0013(4)
N10 0.0315(6) 0.0284(6) 0.0278(6) -0.0052(5) 0.0082(5) -0.0006(5)
C11 0.0195(6) 0.0188(5) 0.0173(5) -0.0009(5) 0.0016(4) 0.0008(4)
C12 0.0204(6) 0.0214(6) 0.0200(5) 0.0002(5) 0.0013(4) 0.0020(4)
C13 0.0216(6) 0.0246(6) 0.0208(6) -0.0029(5) -0.0011(4) 0.0009(5)
C14 0.0256(6) 0.0210(6) 0.0191(5) -0.0024(5) 0.0023(5) -0.0009(4)
C15 0.0218(6) 0.0211(6) 0.0233(6) 0.0018(5) 0.0029(4) -0.0003(5)
C16 0.0190(6) 0.0215(6) 0.0207(5) -0.0008(5) 0.0003(4) 0.0009(4)
C17 0.0328(7) 0.0293(7) 0.0232(6) 0.0009(6) -0.0002(5) -0.0077(5)
C18 0.0204(5) 0.0213(6) 0.0154(5) 0.0022(5) 0.0004(4) -0.0001(4)
N18 0.0223(5) 0.0250(5) 0.0211(5) -0.0020(5) -0.0003(4) -0.0004(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0018 '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 0.0074 0.0036 '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
C9A N1 C2 . . 123.11(11) ?
C9A N1 H1 . . 117.8(10) ?
C2 N1 H1 . . 118.7(11) ?
N1 C2 C3 . . 107.31(10) ?
N1 C2 H2A . . 110.3 ?
C3 C2 H2A . . 110.3 ?
N1 C2 H2B . . 110.3 ?
C3 C2 H2B . . 110.3 ?
H2A C2 H2B . . 108.5 ?
C2 C3 C4 . . 108.88(10) ?
C2 C3 H3A . . 109.9 ?
C4 C3 H3A . . 109.9 ?
C2 C3 H3B . . 109.9 ?
C4 C3 H3B . . 109.9 ?
H3A C3 H3B . . 108.3 ?
N5 C4 C3 . . 111.35(10) ?
N5 C4 H4A . . 109.4 ?
C3 C4 H4A . . 109.4 ?
N5 C4 H4B . . 109.4 ?
C3 C4 H4B . . 109.4 ?
H4A C4 H4B . . 108.0 ?
C9A N5 C6 . . 122.49(10) ?
C9A N5 C4 . . 121.90(10) ?
C6 N5 C4 . . 115.55(10) ?
N6 C6 N5 . . 116.82(11) ?
N6 C6 C7 . . 127.35(12) ?
N5 C6 C7 . . 115.81(11) ?
C6 N6 H6 . . 109.5(11) ?
C8 C7 C10 . . 122.59(11) ?
C8 C7 C6 . . 122.82(11) ?
C10 C7 C6 . . 114.58(11) ?
C7 C8 C9 . . 118.05(11) ?
C7 C8 C11 . . 121.18(11) ?
C9 C8 C11 . . 120.77(11) ?
C8 C9 C18 . . 123.04(11) ?
C8 C9 C9A . . 120.44(11) ?
C18 C9 C9A . . 116.40(11) ?
N1 C9A N5 . . 119.41(11) ?
N1 C9A C9 . . 120.53(11) ?
N5 C9A C9 . . 120.06(11) ?
N10 C10 C7 . . 174.99(14) ?
C12 C11 C16 . . 118.66(11) ?
C12 C11 C8 . . 122.20(11) ?
C16 C11 C8 . . 119.13(11) ?
C13 C12 C11 . . 120.05(12) ?
C13 C12 H12 . . 120.0 ?
C11 C12 H12 . . 120.0 ?
C14 C13 C12 . . 121.50(12) ?
C14 C13 H13 . . 119.2 ?
C12 C13 H13 . . 119.2 ?
C13 C14 C15 . . 117.94(11) ?
C13 C14 C17 . . 122.48(12) ?
C15 C14 C17 . . 119.56(12) ?
C16 C15 C14 . . 121.27(12) ?
C16 C15 H15 . . 119.4 ?
C14 C15 H15 . . 119.4 ?
C15 C16 C11 . . 120.55(12) ?
C15 C16 H16 . . 119.7 ?
C11 C16 H16 . . 119.7 ?
C14 C17 H17A . . 109.5 ?
C14 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
C14 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
N18 C18 C9 . . 175.26(13) ?
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
N1 C9A . 1.3310(16) ?
N1 C2 . 1.4587(16) ?
N1 H1 . 0.894(17) ?
C2 C3 . 1.5123(18) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 C4 . 1.5150(18) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 N5 . 1.4865(15) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
N5 C9A . 1.3586(16) ?
N5 C6 . 1.4120(16) ?
C6 N6 . 1.2847(17) ?
C6 C7 . 1.4555(17) ?
N6 H6 . 0.944(18) ?
C7 C8 . 1.3833(17) ?
C7 C10 . 1.4252(17) ?
C8 C9 . 1.4080(17) ?
C8 C11 . 1.4859(16) ?
C9 C18 . 1.4155(17) ?
C9 C9A . 1.4259(16) ?
C10 N10 . 1.1524(18) ?
C11 C12 . 1.3974(17) ?
C11 C16 . 1.4002(17) ?
C12 C13 . 1.3936(17) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.3929(19) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.3947(18) ?
C14 C17 . 1.5050(18) ?
C15 C16 . 1.3855(17) ?
C15 H15 . 0.9500 ?
C16 H16 . 0.9500 ?
C17 H17A . 0.9800 ?
C17 H17B . 0.9800 ?
C17 H17C . 0.9800 ?
C18 N18 . 1.1567(17) ?
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
N1 H1 N18 3_876 0.892(18) 2.229(18) 3.0308(16) 149.3(14) yes
C2 H2B N10 4_675 0.99 2.60 3.1574(18) 116 yes
C16 H16 N18 1_455 0.95 2.51 3.3592(17) 149 yes
C3 H3B Cg3 3_776 0.99 2.77 3.5553(15) 136 yes
C4 H4B Cg3 4_564 0.99 2.88 3.6750(14) 138 yes
C17 H17C Cg2 2_756 0.98 2.88 3.6306(16) 134 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
C9A N1 C2 C3 . . . . 38.85(16) ?
N1 C2 C3 C4 . . . . -59.02(13) ?
C2 C3 C4 N5 . . . . 48.56(14) ?
C3 C4 N5 C9A . . . . -14.66(16) ?
C3 C4 N5 C6 . . . . 162.65(11) ?
C9A N5 C6 N6 . . . . -176.32(12) ?
C4 N5 C6 N6 . . . . 6.39(17) ?
C9A N5 C6 C7 . . . . 2.43(17) ?
C4 N5 C6 C7 . . . . -174.86(11) ?
N6 C6 C7 C8 . . . . -179.04(13) ?
N5 C6 C7 C8 . . . . 2.36(18) ?
N6 C6 C7 C10 . . . . 2.2(2) ?
N5 C6 C7 C10 . . . . -176.36(11) ?
C10 C7 C8 C9 . . . . 175.72(12) ?
C6 C7 C8 C9 . . . . -2.91(18) ?
C10 C7 C8 C11 . . . . -4.73(19) ?
C6 C7 C8 C11 . . . . 176.65(11) ?
C7 C8 C9 C18 . . . . 174.72(11) ?
C11 C8 C9 C18 . . . . -4.83(18) ?
C7 C8 C9 C9A . . . . -1.12(18) ?
C11 C8 C9 C9A . . . . 179.33(11) ?
C2 N1 C9A N5 . . . . -4.15(18) ?
C2 N1 C9A C9 . . . . 175.97(11) ?
C6 N5 C9A N1 . . . . 173.71(11) ?
C4 N5 C9A N1 . . . . -9.17(18) ?
C6 N5 C9A C9 . . . . -6.41(18) ?
C4 N5 C9A C9 . . . . 170.71(11) ?
C8 C9 C9A N1 . . . . -174.37(11) ?
C18 C9 C9A N1 . . . . 9.52(17) ?
C8 C9 C9A N5 . . . . 5.75(18) ?
C18 C9 C9A N5 . . . . -170.36(11) ?
C7 C8 C11 C12 . . . . 132.01(13) ?
C9 C8 C11 C12 . . . . -48.44(17) ?
C7 C8 C11 C16 . . . . -48.17(17) ?
C9 C8 C11 C16 . . . . 131.37(13) ?
C16 C11 C12 C13 . . . . -0.95(18) ?
C8 C11 C12 C13 . . . . 178.86(12) ?
C11 C12 C13 C14 . . . . -0.42(19) ?
C12 C13 C14 C15 . . . . 1.33(19) ?
C12 C13 C14 C17 . . . . -177.21(13) ?
C13 C14 C15 C16 . . . . -0.88(19) ?
C17 C14 C15 C16 . . . . 177.71(12) ?
C14 C15 C16 C11 . . . . -0.48(19) ?
C12 C11 C16 C15 . . . . 1.40(18) ?
C8 C11 C16 C15 . . . . -178.42(12) ?