#------------------------------------------------------------------------------
#$Date: 2023-07-06 20:21:34 +0200 (Thu, 06 Jul 2023) $
#$Revision: 285061 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022766.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_2022766
loop_
_publ_author_name
'Banna, Md Hasan Al'
'Sheikh, Md Chanmiya'
'Miyatake, Ryuta'
'Howlader, Md Belayet Hossain'
'Zangrando, Ennio'
_publ_section_title
;
Crystal structure of
4-[(4-methyl-benz-yl)-oxy]-N'-(4-nitro-benzyl-idene)benzohydrazide:
a new hydrazone derivative.
;
_journal_coeditor_code WM5682
_journal_issue 'Pt 6'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 531
_journal_page_last 533
_journal_paper_doi 10.1107/S2056989023003948
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C22 H19 N3 O4'
_chemical_formula_moiety 'C22 H19 N3 O4'
_chemical_formula_sum 'C22 H19 N3 O4'
_chemical_formula_weight 389.40
_chemical_name_systematic
;
4-[(4-Methylbenzyl)oxy]-N'-(4-nitrobenzylidene)benzohydrazide
;
_space_group_crystal_system monoclinic
_space_group_IT_number 4
_space_group_name_Hall 'P 2yb'
_space_group_name_H-M_alt 'P 1 21 1'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2019/2
_cell_angle_alpha 90
_cell_angle_beta 96.585(7)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 8.9485(8)
_cell_length_b 5.0612(5)
_cell_length_c 20.949(2)
_cell_measurement_reflns_used 5984
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 27.45
_cell_measurement_theta_min 2.29
_cell_volume 942.52(16)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 2018)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 2018)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 2018)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Rigaku R-AXIS RAPID'
_diffrn_measurement_method \w
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71075
_diffrn_reflns_av_R_equivalents 0.0501
_diffrn_reflns_av_unetI/netI 0.0645
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 9086
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.469
_diffrn_reflns_theta_min 1.957
_exptl_absorpt_coefficient_mu 0.096
_exptl_absorpt_correction_T_max 0.997
_exptl_absorpt_correction_T_min 0.749
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.372
_exptl_crystal_description platel
_exptl_crystal_F_000 408
_exptl_crystal_size_max 0.300
_exptl_crystal_size_mid 0.280
_exptl_crystal_size_min 0.030
_refine_diff_density_max 0.189
_refine_diff_density_min -0.156
_refine_ls_abs_structure_details
;
Flack x determined using 741 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack -0.8(9)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.035
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 266
_refine_ls_number_reflns 3799
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.035
_refine_ls_R_factor_all 0.0867
_refine_ls_R_factor_gt 0.0528
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+0.0221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1136
_refine_ls_wR_factor_ref 0.1255
_reflns_number_gt 2635
_reflns_number_total 3799
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wm5682sup1.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2022766.cif.'
_cod_original_cell_volume 942.54(16)
_cod_original_sg_symbol_H-M 'P 21'
_cod_database_code 2022766
_cod_database_fobs_code 2022766
_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 0.972
_shelx_estimated_absorpt_t_max 0.997
_shelx_hkl_file
;
0 0 2 0.10 0.15
0 0 -2 -0.17 0.19
0 0 3 111.87 1.46
0 0 -3 112.24 1.69
0 0 4 39.83 1.09
0 0 -4 39.37 1.11
0 0 5 166.36 3.35
0 0 -5 161.51 2.77
0 0 6 3.12 0.60
0 0 -6 2.21 0.60
0 0 7 0.13 0.54
0 0 -7 -1.08 0.86
0 0 8 3.73 0.95
0 0 -8 -0.57 0.96
0 0 9 52.11 1.91
0 0 -9 53.04 1.45
0 0 10 200.47 4.13
0 0 -10 195.53 4.51
0 0 11 896.85 26.08
0 0 -11 932.66 28.15
0 0 12 77.36 2.68
0 0 -12 71.72 2.06
0 0 13 22.44 1.24
0 0 -13 22.35 1.31
0 0 14 125.24 3.23
0 0 -14 125.18 4.12
0 0 15 50.13 2.67
0 0 -15 52.00 2.80
0 0 16 80.68 3.61
0 0 -16 87.64 2.83
0 0 17 90.46 3.10
0 0 -17 93.40 3.14
0 0 18 4.29 1.41
0 0 -18 -1.60 2.42
0 0 19 37.09 3.29
0 0 -19 45.93 3.46
0 0 20 5.40 2.56
0 0 -20 7.87 1.79
0 0 21 46.41 2.77
0 0 -21 45.45 2.84
0 0 22 8.09 1.96
0 0 -22 5.07 3.05
0 0 23 11.47 3.29
0 0 -23 9.49 2.59
0 0 -23 12.31 2.20
0 0 24 1.44 2.07
0 0 -24 3.65 2.37
0 0 -24 0.77 2.05
0 0 25 5.02 2.18
0 0 -25 4.65 3.93
0 0 -25 -2.43 3.34
0 0 26 3.66 3.37
0 0 -26 3.03 2.76
0 0 -26 -5.73 3.34
0 0 -27 5.59 2.51
0 1 0 0.70 0.42
0 1 0 -0.17 0.23
0 1 1 22.60 0.81
0 1 1 22.70 0.54
0 1 -1 22.69 0.52
0 -1 -1 21.48 0.65
0 1 2 292.49 5.29
0 1 2 288.22 4.32
0 1 -2 285.18 4.82
0 -1 2 282.90 4.53
0 -1 -2 282.65 4.09
0 -1 -2 284.37 4.74
0 1 3 166.76 2.84
0 1 3 157.90 2.32
0 1 -3 165.16 2.59
0 -1 3 160.00 2.59
0 -1 -3 166.44 2.52
0 -1 -3 164.32 2.80
0 1 4 258.75 4.58
0 1 4 252.35 4.09
0 1 -4 261.03 4.90
0 -1 4 254.00 4.81
0 -1 -4 257.34 4.24
0 -1 -4 252.65 5.16
0 1 5 233.33 3.99
0 1 -5 239.54 4.68
0 -1 5 235.97 4.65
0 -1 -5 232.52 3.66
0 -1 -5 228.54 4.32
0 1 6 246.89 4.24
0 1 -6 253.79 5.18
0 -1 6 253.37 4.66
0 -1 -6 248.15 4.48
0 -1 -6 261.20 5.76
0 1 7 111.96 2.32
0 1 -7 116.29 2.76
0 -1 7 108.36 2.71
0 -1 -7 109.67 2.26
0 -1 -7 102.26 2.35
0 1 8 3.70 1.00
0 1 -8 8.19 0.81
0 -1 8 6.98 0.83
0 -1 -8 6.12 0.62
0 -1 -8 7.34 0.90
0 1 9 45.01 1.85
0 1 -9 46.14 1.54
0 -1 9 49.62 1.47
0 -1 -9 46.49 1.67
0 -1 -9 43.49 2.21
0 1 -10 17.20 1.54
0 -1 10 14.50 1.04
0 -1 -10 14.98 1.24
0 -1 -10 15.19 1.69
0 1 11 105.86 2.98
0 1 -11 102.51 2.63
0 -1 11 99.00 2.56
0 -1 -11 100.85 2.31
0 -1 -11 98.93 3.55
0 1 12 56.16 2.24
0 1 -12 61.05 2.61
0 -1 12 53.95 1.88
0 -1 -12 54.09 1.63
0 -1 -12 63.23 2.17
0 1 13 77.07 2.14
0 1 -13 79.89 2.39
0 -1 13 73.14 2.27
0 -1 -13 78.56 2.14
0 -1 -13 86.62 3.55
0 1 14 105.57 3.70
0 1 -14 109.20 4.38
0 -1 14 102.34 3.05
0 -1 -14 102.58 2.67
0 -1 -14 101.22 4.37
0 1 15 16.26 1.33
0 1 -15 18.59 1.60
0 -1 15 16.19 1.50
0 -1 -15 20.65 1.33
0 -1 -15 21.48 2.53
0 1 16 36.60 2.53
0 1 -16 42.29 3.20
0 -1 16 35.12 2.01
0 -1 -16 35.56 1.75
0 -1 -16 29.35 3.09
0 1 17 33.60 2.76
0 1 -17 31.47 3.36
0 -1 17 34.41 2.13
0 -1 -17 34.02 1.83
0 -1 -17 33.72 3.70
0 1 18 46.02 2.24
0 1 -18 45.17 2.55
0 -1 18 48.55 3.51
0 -1 -18 42.90 2.98
0 -1 -18 43.74 2.99
0 1 19 45.34 3.35
0 1 -19 47.03 4.16
0 -1 19 45.55 3.81
0 -1 -19 46.12 3.28
0 -1 -19 44.92 3.12
0 1 20 2.00 1.52
0 1 -20 3.92 1.94
0 -1 20 -0.25 2.65
0 -1 -20 4.72 2.28
0 -1 -20 2.02 2.10
0 1 21 9.54 2.71
0 1 -21 8.83 2.10
0 -1 21 9.43 2.04
0 -1 -21 8.79 2.66
0 -1 -21 12.20 2.49
0 1 22 0.91 2.58
0 1 -22 2.41 3.01
0 -1 22 -0.53 1.93
0 -1 -22 2.28 1.71
0 -1 -22 1.59 3.54
0 1 23 6.74 1.91
0 1 -23 4.81 2.30
0 -1 23 6.91 2.16
0 -1 -23 1.74 1.87
0 -1 -23 7.65 3.90
0 1 24 4.25 3.04
0 1 -24 5.26 2.38
0 -1 24 2.62 3.48
0 -1 -24 4.84 3.06
0 -1 -24 1.38 2.75
0 1 25 -3.22 3.11
0 1 -25 3.56 3.66
0 -1 25 4.99 3.53
0 -1 -25 3.06 3.00
0 -1 -25 1.82 2.91
0 1 26 5.13 2.22
0 1 -26 2.40 2.57
0 -1 26 4.80 2.53
0 -1 -26 0.88 3.30
0 -1 -26 2.80 3.12
0 2 0 24.41 0.71
0 2 0 26.16 0.91
0 2 1 202.20 3.71
0 2 1 208.68 3.65
0 2 -1 207.68 3.96
0 2 -1 209.01 4.06
0 -2 -1 215.41 4.37
0 2 2 125.39 2.37
0 2 2 127.98 2.24
0 2 -2 125.37 2.22
0 -2 -2 119.59 2.04
0 -2 -2 128.39 2.84
0 2 3 189.32 4.20
0 2 3 186.62 3.28
0 2 -3 191.10 3.89
0 -2 -3 191.59 3.49
0 -2 -3 188.72 4.22
0 2 4 226.21 4.57
0 2 4 218.98 4.00
0 2 -4 222.22 4.28
0 -2 4 224.47 4.45
0 -2 -4 211.72 4.03
0 -2 -4 226.11 5.19
0 2 5 3.46 1.09
0 2 5 0.74 0.59
0 2 -5 0.75 0.66
0 -2 5 -0.47 0.70
0 -2 -5 0.50 0.68
0 -2 -5 2.65 0.73
0 2 6 157.31 4.22
0 2 6 153.93 2.99
0 2 -6 161.86 3.33
0 -2 6 154.32 3.90
0 -2 -6 159.02 3.14
0 -2 -6 161.06 3.54
0 2 7 255.99 4.93
0 2 -7 263.80 5.61
0 -2 7 258.37 6.41
0 -2 -7 257.92 5.15
0 -2 -7 258.77 6.74
0 2 8 282.75 6.18
0 2 -8 295.94 6.47
0 -2 8 289.79 6.48
0 -2 -8 274.47 5.94
0 -2 -8 285.69 6.81
0 2 9 16.28 1.21
0 2 -9 16.15 1.63
0 -2 9 17.43 1.68
0 -2 -9 18.44 0.84
0 -2 -9 18.72 1.92
0 2 10 26.42 1.46
0 2 -10 31.19 1.93
0 -2 10 24.35 1.91
0 -2 -10 25.89 1.00
0 -2 -10 27.34 1.54
0 2 11 83.05 2.56
0 2 -11 80.55 2.37
0 -2 11 75.00 2.32
0 -2 -11 72.84 2.24
0 -2 -11 83.06 3.54
0 2 12 1.59 1.31
0 2 -12 -1.29 1.68
0 -2 12 0.35 1.07
0 -2 -12 -0.06 0.69
0 -2 -12 -0.20 1.84
0 2 13 41.20 2.17
0 2 -13 41.11 1.94
0 -2 13 40.23 2.67
0 -2 -13 38.27 1.85
0 -2 -13 40.24 2.17
0 2 14 120.84 3.34
0 2 -14 136.17 5.15
0 -2 14 121.71 4.85
0 -2 -14 118.36 3.85
0 -2 -14 131.02 4.27
0 2 15 60.67 2.97
0 2 -15 68.34 2.91
0 -2 15 70.99 3.68
0 -2 -15 62.73 2.09
0 -2 -15 68.18 3.02
0 2 16 53.08 3.11
0 2 -16 55.01 3.95
0 -2 16 58.17 3.88
0 -2 -16 58.65 2.08
0 -2 -16 59.42 3.12
0 2 17 36.70 2.00
0 2 -17 34.93 2.48
0 -2 17 41.27 3.55
0 -2 -17 38.27 1.87
0 -2 -17 34.73 2.79
0 2 18 54.10 3.31
0 2 -18 52.65 4.21
0 -2 18 49.86 4.07
0 -2 -18 51.04 3.03
0 -2 -18 49.88 3.33
0 2 -19 0.04 1.95
0 -2 19 4.77 2.70
0 -2 -19 5.94 2.01
0 -2 -19 2.86 2.16
0 2 20 6.50 2.42
0 2 -20 7.06 3.24
0 -2 20 9.23 3.16
0 -2 -20 7.56 2.22
0 -2 -20 7.62 2.45
0 2 21 3.73 1.63
0 2 -21 0.87 3.38
0 -2 21 0.85 3.19
0 -2 -21 4.06 2.29
0 -2 -21 5.89 2.40
0 2 22 6.34 2.76
0 2 -22 5.58 2.33
0 -2 22 4.68 2.17
0 -2 -22 4.22 1.65
0 -2 -22 1.04 3.88
0 2 23 2.53 2.70
0 2 -23 4.03 3.62
0 -2 23 1.50 2.29
0 -2 -23 -1.15 1.65
0 -2 -23 2.16 4.15
0 2 24 0.48 2.81
0 2 -24 0.10 2.56
0 -2 -24 -6.98 4.40
0 -2 24 1.02 2.22
0 2 25 4.82 3.18
0 2 -25 5.36 2.78
0 -2 25 2.05 2.57
0 -2 -25 5.80 2.01
0 -2 -25 2.37 4.88
0 3 0 -0.39 1.00
0 3 0 0.95 0.83
0 3 0 0.15 0.59
0 3 1 4.08 0.76
0 3 1 2.84 0.85
0 3 -1 3.15 0.67
0 3 -1 3.47 0.62
0 3 -1 3.85 0.65
0 3 2 42.51 1.37
0 3 2 48.35 1.13
0 3 -2 44.40 1.69
0 3 -2 47.26 1.75
0 3 3 29.97 1.72
0 3 3 27.92 0.88
0 3 -3 27.63 1.50
0 3 -3 29.58 1.40
0 -3 -3 29.71 1.23
0 3 4 32.31 1.88
0 3 4 33.73 1.25
0 3 -4 35.69 1.71
0 -3 -4 30.09 1.90
0 3 5 62.07 2.58
0 3 5 65.77 1.78
0 3 -5 66.28 2.38
0 -3 -5 65.61 1.91
0 -3 -5 59.29 2.52
0 3 6 15.69 1.74
0 3 6 14.85 0.70
0 3 -6 11.22 1.56
0 -3 -6 12.43 1.15
0 -3 -6 16.93 1.74
0 3 7 30.77 2.21
0 3 -7 26.70 1.33
0 -3 -7 26.97 1.37
0 -3 -7 28.45 1.52
0 3 8 3.45 1.08
0 3 8 2.23 0.64
0 3 -8 0.40 0.98
0 -3 8 1.45 1.02
0 -3 -8 1.75 0.97
0 -3 -8 1.98 1.13
0 3 9 8.85 1.20
0 3 -9 8.06 1.75
0 -3 9 8.50 1.87
0 -3 -9 8.20 0.80
0 -3 -9 11.26 2.08
0 3 10 2.15 1.14
0 3 -10 2.71 1.11
0 -3 10 2.97 1.74
0 -3 -10 1.91 1.10
0 -3 -10 -0.38 1.29
0 3 11 3.78 1.25
0 3 -11 0.83 1.23
0 -3 11 1.21 1.24
0 -3 -11 1.82 1.20
0 -3 -11 0.48 2.14
0 3 12 8.77 1.55
0 3 -12 9.98 2.29
0 -3 12 8.33 2.22
0 -3 -12 8.15 1.47
0 -3 -12 14.01 2.53
0 3 13 23.99 2.26
0 3 -13 21.40 1.93
0 -3 13 24.32 2.74
0 -3 -13 21.66 1.79
0 -3 -13 20.69 2.08
0 3 14 6.37 1.77
0 3 -14 10.00 2.41
0 -3 14 6.92 1.65
0 -3 -14 8.07 1.59
0 -3 -14 5.00 1.84
0 3 15 109.39 3.39
0 3 -15 119.92 4.38
0 -3 15 111.63 4.18
0 -3 -15 112.88 3.84
0 -3 -15 107.91 6.10
0 3 16 13.38 2.19
0 3 -16 14.07 3.03
0 -3 16 16.64 1.97
0 -3 -16 12.96 1.31
0 -3 -16 15.37 3.32
0 3 17 4.99 2.06
0 3 -17 6.01 1.88
0 -3 17 4.17 1.88
0 -3 -17 3.89 1.89
0 -3 -17 10.08 3.39
0 3 18 0.66 1.33
0 3 -18 -3.62 2.92
0 -3 18 -0.45 2.79
0 -3 -18 -1.34 1.81
0 -3 -18 5.45 3.26
0 3 19 5.64 2.51
0 3 -19 7.53 2.32
0 -3 19 11.73 3.36
0 -3 -19 8.44 2.30
0 -3 -19 11.28 3.88
0 3 20 4.21 2.48
0 3 -20 0.02 3.51
0 -3 20 8.90 3.47
0 -3 -20 7.14 2.37
0 -3 -20 5.31 3.80
0 3 21 5.33 1.68
0 3 -21 0.81 3.59
0 -3 21 0.64 3.47
0 -3 -21 1.00 1.61
0 -3 -21 4.12 4.03
0 3 22 3.35 2.92
0 3 -22 11.08 2.64
0 -3 22 7.57 3.86
0 -3 -22 5.14 1.75
0 -3 -22 -1.58 4.53
0 3 23 -1.12 1.79
0 3 -23 2.32 3.83
0 -3 23 -3.70 2.55
0 -3 -23 0.48 1.67
0 -3 -23 3.15 4.40
0 3 24 6.70 3.08
0 -3 -24 1.24 5.07
0 4 0 2.39 0.98
0 4 0 1.33 0.80
0 4 0 0.67 1.32
0 4 1 0.71 0.99
0 4 1 0.81 1.11
0 4 1 0.85 1.29
0 4 -1 1.87 0.94
0 4 -1 0.34 0.82
0 4 -1 0.93 1.33
0 4 2 29.45 1.51
0 4 2 29.83 1.62
0 4 -2 30.11 1.97
0 4 -2 27.98 1.33
0 4 -2 30.80 1.41
0 4 3 16.66 1.39
0 4 3 19.42 1.00
0 4 -3 18.71 1.75
0 4 -3 16.87 1.74
0 4 -3 18.06 1.25
0 4 4 64.39 2.27
0 4 -4 61.84 2.54
0 4 -4 61.44 2.10
0 4 -4 62.23 2.11
0 4 5 2.62 1.87
0 4 5 1.49 0.75
0 4 -5 4.12 1.63
0 4 -5 3.22 1.43
0 -4 -5 4.04 1.75
0 4 6 6.08 2.01
0 4 6 5.58 1.23
0 4 -6 1.53 1.79
0 4 -6 4.25 1.54
0 -4 -6 6.82 1.92
0 4 7 2.99 1.40
0 4 7 2.68 1.17
0 4 -7 3.61 1.21
0 -4 -7 3.40 2.07
0 4 8 20.14 1.75
0 4 8 19.85 1.57
0 4 -8 15.94 2.30
0 -4 -8 20.38 1.71
0 -4 -8 20.16 1.78
0 4 9 26.50 1.25
0 4 -9 23.31 2.59
0 -4 -9 22.77 1.83
0 -4 -9 26.74 2.96
0 4 10 13.50 1.66
0 4 -10 14.19 1.68
0 -4 -10 15.10 1.70
0 -4 -10 15.75 1.82
0 4 11 -0.25 1.45
0 4 -11 3.96 2.19
0 -4 -11 1.34 0.96
0 -4 -11 5.12 2.44
0 4 12 4.82 1.68
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-10 -2 4 1.88 0.91
10 2 -3 -3.64 3.58
-10 2 3 4.59 2.01
10 2 -2 3.30 3.82
-10 2 2 5.89 3.10
10 2 -1 -0.69 2.33
-10 2 1 2.96 2.85
10 2 0 2.16 3.48
-10 2 0 -1.05 1.79
10 2 1 5.61 3.76
-10 2 -1 0.79 2.76
10 2 2 -1.56 2.35
-10 2 -2 0.48 1.83
10 2 3 4.30 3.76
-10 2 -3 1.83 2.98
-10 2 -3 3.37 2.13
10 2 4 -7.48 3.87
-10 2 -4 -1.60 1.99
-10 2 -4 -4.74 3.28
10 2 5 2.39 2.50
-10 2 -5 0.48 2.83
-10 2 -5 -0.56 3.14
10 2 6 -0.26 2.45
-10 2 -6 0.44 2.86
-10 2 -6 0.98 2.06
10 2 7 3.62 3.80
-10 2 -7 0.18 1.95
-10 2 -7 1.81 3.27
10 2 8 0.59 2.54
-10 2 -8 2.92 2.98
-10 2 -8 -4.61 3.27
10 3 -8 4.35 2.97
-10 3 8 2.96 2.37
10 -3 -8 -1.68 2.62
10 3 -7 -0.29 4.36
-10 3 7 6.64 3.53
10 3 -6 4.08 3.06
-10 3 6 5.31 2.39
10 3 -5 -0.92 4.21
-10 3 5 4.20 2.33
10 3 -4 5.32 2.87
-10 3 4 5.48 3.61
10 3 -3 -1.33 4.19
-10 3 3 -0.96 2.24
10 3 -2 -0.97 2.67
-10 3 2 1.79 3.23
10 3 -1 5.44 4.22
-10 3 1 -1.01 2.13
10 3 0 -0.36 2.79
-10 3 0 5.92 3.43
10 3 1 -4.94 2.73
-10 3 -1 5.93 3.19
10 3 2 -6.38 4.30
-10 3 -2 3.00 2.16
10 3 3 0.08 2.85
-10 3 -3 2.65 3.52
-10 3 -3 3.86 2.49
11 0 -11 0.24 2.97
-11 0 11 2.60 2.09
11 0 -10 5.70 2.05
-11 0 10 5.51 3.22
11 0 -9 17.61 3.39
-11 0 9 12.77 2.27
11 0 -8 -1.54 2.70
-11 0 8 2.49 2.79
11 0 -7 2.31 3.32
11 0 -7 5.55 1.85
-11 0 7 4.28 1.84
11 0 -6 1.58 1.97
11 0 -6 -1.50 2.64
-11 0 6 -2.02 2.58
11 0 -5 1.50 2.05
-11 0 5 4.11 1.75
11 0 -4 0.10 2.90
-11 0 4 1.12 2.39
11 0 -3 -0.69 2.84
-11 0 3 -1.83 2.39
11 0 -2 1.78 2.87
-11 0 2 1.53 2.26
11 0 -1 -1.01 1.85
-11 0 1 1.04 2.16
11 0 0 -0.21 1.83
-11 0 0 0.43 1.42
11 0 1 -3.12 2.97
-11 0 -1 1.09 2.12
11 0 2 1.49 2.84
-11 0 -2 1.18 1.39
-11 0 -2 0.77 2.39
11 0 3 3.85 2.91
-11 0 -3 0.12 2.08
-11 0 -3 -0.56 2.36
11 0 4 2.35 2.93
-11 0 -4 1.35 1.45
-11 0 -4 1.26 1.51
11 0 5 0.98 2.84
-11 0 -5 -0.82 2.13
-11 0 -5 -0.62 1.47
-11 1 10 11.14 3.45
11 1 -10 3.87 2.66
11 -1 -10 4.63 2.27
-11 -1 10 0.69 1.99
-11 1 9 -0.37 2.16
11 1 -9 2.20 1.60
11 -1 -9 4.88 3.14
-11 -1 9 2.51 2.74
11 1 -8 3.18 2.59
-11 1 8 4.90 3.19
11 1 -8 2.22 1.68
11 -1 -8 3.84 2.23
-11 -1 8 3.95 2.59
11 1 -7 7.07 3.66
11 1 -7 3.69 2.38
-11 1 7 1.56 2.06
11 -1 -7 4.02 2.70
11 -1 -7 10.22 3.26
-11 -1 7 3.67 2.47
11 1 -6 7.07 3.49
11 1 -6 -0.85 2.21
-11 1 6 2.02 2.86
11 -1 -6 2.70 2.47
11 -1 -6 -0.12 2.06
-11 -1 6 1.11 2.33
11 1 -5 2.01 2.27
-11 1 5 0.75 1.78
11 -1 -5 0.22 2.34
-11 -1 5 -0.17 1.39
11 1 -4 -2.21 3.33
-11 1 4 -0.14 2.75
11 -1 -4 -0.35 2.15
-11 -1 4 1.47 1.95
-11 1 3 9.43 2.99
11 1 -3 9.53 3.73
11 -1 -3 6.60 2.41
-11 1 2 4.27 2.74
11 1 -2 3.80 2.27
11 -1 -2 2.14 2.24
-11 -1 2 2.93 1.85
-11 1 1 0.70 2.68
11 1 -1 7.45 3.57
11 -1 -1 2.92 2.14
-11 1 0 -0.59 1.74
11 1 0 2.28 3.34
11 -1 0 -1.18 1.99
-11 -1 0 -0.42 1.51
11 1 1 -0.85 2.27
-11 1 -1 -2.17 2.68
11 1 2 0.57 2.26
-11 1 -2 0.39 1.74
11 1 3 1.46 3.59
-11 1 -3 2.00 2.91
-11 1 -3 6.99 3.05
11 1 4 2.86 3.68
-11 1 -4 2.22 2.82
-11 1 -4 5.81 3.10
11 2 -5 9.74 4.43
11 2 -4 -2.65 2.61
-11 2 4 -3.84 2.14
11 2 -3 2.85 4.08
-11 2 3 1.47 3.11
11 2 -2 0.76 2.53
-11 2 2 0.99 2.02
11 2 -1 -0.77 2.63
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 51020
_shelx_res_file
;
TITL SH197
shelx.res
created by SHELXL-2019/2 at 14:38:37 on 03-Apr-2023
CELL 0.71075 8.9485 5.0612 20.9493 90.000 96.585 90.000
ZERR 2.00 0.0008 0.0005 0.0020 0.000 0.007 0.000
LATT -1
SYMM - X, 1/2 + Y, - Z
SFAC C H N O
UNIT 44 38 6 8
MERG 2
OMIT 1 0 0
OMIT -2 0 3
EQIV $1 -x+1, y+1/2, -z+1
HTAB C14 N2_$1
EQIV $2 x, y+1, z
HTAB C16 O2_$2
EQIV $3 -x+1, y+1/2, -z
HTAB C21 O4_$3
HTAB N1 O2_$2
FMAP 2
PLAN 10
SIZE 0.030 0.280 0.300
ACTA
HTAB 2.00000
BOND $H
CONF
L.S. 10
TEMP -100.00
WGHT 0.063700 0.022100
FVAR 0.57818
O1 4 0.147681 0.542392 0.668165 11.00000 0.05145 0.06063 =
0.03279 -0.00791 0.01394 -0.01278
O2 4 0.307183 0.118821 0.398778 11.00000 0.06054 0.03069 =
0.03206 -0.00153 0.01013 0.00111
O3 4 0.719459 0.395524 0.043326 11.00000 0.07618 0.16798 =
0.04893 -0.00696 0.01990 0.03970
O4 4 0.596553 0.747704 0.009094 11.00000 0.11305 0.08647 =
0.04187 0.00316 0.03236 -0.01466
N1 3 0.361090 0.554177 0.388305 11.00000 0.05715 0.02884 =
0.02594 -0.00166 0.01049 0.00004
H1 2 0.354036 0.723977 0.401070 11.00000 -1.20000
N2 3 0.417304 0.510156 0.330795 11.00000 0.04923 0.03217 =
0.02737 -0.00200 0.00870 0.00073
N3 3 0.637900 0.585966 0.051050 11.00000 0.05938 0.09384 =
0.03846 -0.00849 0.01416 -0.01054
C1 1 -0.101065 0.882275 0.930305 11.00000 0.06526 0.10996 =
0.04341 -0.01756 0.02320 -0.00846
AFIX 137
H1A 2 -0.136189 1.063016 0.920871 11.00000 -1.20000
H1B 2 -0.010078 0.886972 0.961152 11.00000 -1.20000
H1C 2 -0.179652 0.782238 0.948641 11.00000 -1.20000
AFIX 0
C2 1 -0.066037 0.750637 0.869037 11.00000 0.04119 0.06818 =
0.03488 -0.00433 0.01558 -0.01355
C3 1 0.029005 0.542487 0.869826 11.00000 0.09245 0.06924 =
0.03073 0.00802 -0.00159 0.01125
AFIX 43
H3 2 0.074131 0.476727 0.909949 11.00000 -1.20000
AFIX 0
C4 1 0.062152 0.423189 0.813966 11.00000 0.08265 0.06952 =
0.04403 0.00172 -0.00144 0.03372
AFIX 43
H4 2 0.130000 0.278228 0.816291 11.00000 -1.20000
AFIX 0
C5 1 -0.001895 0.511489 0.754704 11.00000 0.03854 0.04921 =
0.03370 -0.00032 0.00898 -0.00542
C6 1 -0.097421 0.718857 0.753526 11.00000 0.06390 0.06500 =
0.03547 0.00061 -0.00241 0.01517
AFIX 43
H6 2 -0.143298 0.783136 0.713380 11.00000 -1.20000
AFIX 0
C7 1 -0.129526 0.838719 0.809362 11.00000 0.05507 0.09375 =
0.04625 -0.01503 0.00020 0.02457
AFIX 43
H7 2 -0.196585 0.984825 0.806939 11.00000 -1.20000
AFIX 0
C8 1 0.034856 0.384644 0.693681 11.00000 0.04810 0.05574 =
0.03659 -0.00222 0.01260 -0.00794
AFIX 23
H8A 2 0.072933 0.203070 0.702463 11.00000 -1.20000
H8B 2 -0.056490 0.374539 0.662284 11.00000 -1.20000
AFIX 0
C9 1 0.182260 0.483962 0.608089 11.00000 0.03845 0.04171 =
0.02816 -0.00031 0.00490 0.00013
C10 1 0.122197 0.273523 0.570520 11.00000 0.04099 0.03738 =
0.03959 -0.00153 0.01214 -0.00525
AFIX 43
H10 2 0.052049 0.156850 0.586470 11.00000 -1.20000
AFIX 0
C11 1 0.165172 0.236204 0.510327 11.00000 0.04729 0.03257 =
0.03491 -0.00688 0.00509 -0.00439
AFIX 43
H11 2 0.123802 0.092481 0.485007 11.00000 -1.20000
AFIX 0
C12 1 0.267869 0.403377 0.485302 11.00000 0.03951 0.02791 =
0.02591 -0.00162 0.00349 0.00448
C13 1 0.328917 0.610331 0.523947 11.00000 0.04674 0.03909 =
0.03110 -0.00010 0.00732 -0.00662
AFIX 43
H13 2 0.399403 0.727021 0.508241 11.00000 -1.20000
AFIX 0
C14 1 0.287577 0.646457 0.584755 11.00000 0.04889 0.04282 =
0.03325 -0.00744 0.00193 -0.00723
AFIX 43
H14 2 0.332136 0.785035 0.610979 11.00000 -1.20000
AFIX 0
C15 1 0.312639 0.345369 0.421051 11.00000 0.03730 0.02969 =
0.02761 -0.00061 0.00059 0.00407
C16 1 0.431653 0.714285 0.296006 11.00000 0.06055 0.03178 =
0.03198 -0.00541 0.01079 -0.00142
AFIX 43
H16 2 0.404496 0.884332 0.310034 11.00000 -1.20000
AFIX 0
C17 1 0.491034 0.680704 0.233834 11.00000 0.05589 0.03589 =
0.03117 -0.00506 0.01137 -0.01373
C18 1 0.587564 0.475403 0.223223 11.00000 0.05438 0.04826 =
0.03757 -0.00138 0.01045 -0.00849
AFIX 43
H18 2 0.620600 0.356662 0.257043 11.00000 -1.20000
AFIX 0
C19 1 0.635783 0.443696 0.163192 11.00000 0.05117 0.05720 =
0.04686 -0.00952 0.01696 -0.00942
AFIX 43
H19 2 0.702781 0.304857 0.155381 11.00000 -1.20000
AFIX 0
C20 1 0.584324 0.618460 0.114853 11.00000 0.05145 0.06758 =
0.03058 -0.00732 0.01442 -0.01931
C21 1 0.489381 0.821679 0.123566 11.00000 0.07911 0.05423 =
0.03170 0.00224 0.01332 -0.01812
AFIX 43
H21 2 0.455193 0.937239 0.089234 11.00000 -1.20000
AFIX 0
C22 1 0.444465 0.854552 0.183620 11.00000 0.08196 0.04018 =
0.03899 0.00251 0.02100 -0.00585
AFIX 43
H22 2 0.380496 0.998273 0.191162 11.00000 -1.20000
AFIX 0
HKLF 4
REM SH197
REM wR2 = 0.1255, GooF = S = 1.035, Restrained GooF = 1.035 for all data
REM R1 = 0.0528 for 2635 Fo > 4sig(Fo) and 0.0867 for all 3799 data
REM 266 parameters refined using 1 restraints
END
WGHT 0.0635 0.0400
REM Instructions for potential hydrogen bonds
HTAB N1 O2_$2
HTAB C14 N2_$1
HTAB C16 O2_$2
HTAB C21 O4_$3
REM Highest difference peak 0.189, deepest hole -0.156, 1-sigma level 0.040
Q1 1 0.1146 0.4702 0.5771 11.00000 0.05 0.19
Q2 1 0.7657 0.5403 0.0578 11.00000 0.05 0.17
Q3 1 0.5198 0.4261 0.3290 11.00000 0.05 0.16
Q4 1 -0.2546 0.9636 0.9159 11.00000 0.05 0.16
Q5 1 0.1780 0.3408 0.5938 11.00000 0.05 0.16
Q6 1 0.5197 0.6213 0.3279 11.00000 0.05 0.15
Q7 1 0.4972 0.7129 0.2702 11.00000 0.05 0.15
Q8 1 0.6962 0.5846 0.1462 11.00000 0.05 0.15
Q9 1 0.1668 0.6359 0.5808 11.00000 0.05 0.15
Q10 1 0.3190 0.5714 0.2936 11.00000 0.05 0.14
;
_shelx_res_checksum 31355
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.1477(3) 0.5424(5) 0.66816(11) 0.0476(7) Uani d 1 . .
O O2 0.3072(3) 0.1188(5) 0.39878(10) 0.0407(6) Uani d 1 . .
O O3 0.7195(4) 0.3955(11) 0.04333(15) 0.0967(14) Uani d 1 . .
O O4 0.5966(4) 0.7477(8) 0.00909(14) 0.0786(10) Uani d 1 . .
N N1 0.3611(4) 0.5542(5) 0.38830(13) 0.0369(7) Uani d 1 . .
H H1 0.354(4) 0.724(8) 0.4011(17) 0.044 Uiso d 1 . .
N N2 0.4173(3) 0.5102(5) 0.33080(12) 0.0359(7) Uani d 1 . .
N N3 0.6379(4) 0.5860(10) 0.05105(16) 0.0632(11) Uani d 1 . .
C C1 -0.1011(5) 0.8823(12) 0.93031(19) 0.0716(14) Uani d 1 . .
H H1A -0.136189 1.063016 0.920871 0.086 Uiso calc 1 . .
H H1B -0.010078 0.886972 0.961152 0.086 Uiso calc 1 . .
H H1C -0.179652 0.782238 0.948641 0.086 Uiso calc 1 . .
C C2 -0.0660(4) 0.7506(9) 0.86904(16) 0.0472(10) Uani d 1 . .
C C3 0.0290(5) 0.5425(10) 0.86983(18) 0.0648(13) Uani d 1 . .
H H3 0.074131 0.476727 0.909949 0.078 Uiso calc 1 . .
C C4 0.0622(5) 0.4232(10) 0.81397(18) 0.0661(13) Uani d 1 . .
H H4 0.130000 0.278228 0.816291 0.079 Uiso calc 1 . .
C C5 -0.0019(4) 0.5115(8) 0.75470(16) 0.0401(8) Uani d 1 . .
C C6 -0.0974(5) 0.7189(9) 0.75353(18) 0.0554(11) Uani d 1 . .
H H6 -0.143298 0.783136 0.713380 0.067 Uiso calc 1 . .
C C7 -0.1295(5) 0.8387(11) 0.80936(19) 0.0655(13) Uani d 1 . .
H H7 -0.196585 0.984825 0.806939 0.079 Uiso calc 1 . .
C C8 0.0349(4) 0.3846(8) 0.69368(16) 0.0462(9) Uani d 1 . .
H H8A 0.072933 0.203070 0.702463 0.055 Uiso calc 1 . .
H H8B -0.056490 0.374539 0.662284 0.055 Uiso calc 1 . .
C C9 0.1823(4) 0.4840(7) 0.60809(15) 0.0360(8) Uani d 1 . .
C C10 0.1222(4) 0.2735(7) 0.57052(15) 0.0387(9) Uani d 1 . .
H H10 0.052049 0.156850 0.586470 0.046 Uiso calc 1 . .
C C11 0.1652(4) 0.2362(7) 0.51033(15) 0.0382(8) Uani d 1 . .
H H11 0.123802 0.092481 0.485007 0.046 Uiso calc 1 . .
C C12 0.2679(4) 0.4034(6) 0.48530(15) 0.0311(8) Uani d 1 . .
C C13 0.3289(4) 0.6103(7) 0.52395(15) 0.0388(8) Uani d 1 . .
H H13 0.399403 0.727021 0.508241 0.047 Uiso calc 1 . .
C C14 0.2876(4) 0.6465(7) 0.58475(16) 0.0419(9) Uani d 1 . .
H H14 0.332136 0.785035 0.610979 0.050 Uiso calc 1 . .
C C15 0.3126(4) 0.3454(7) 0.42105(15) 0.0318(8) Uani d 1 . .
C C16 0.4317(4) 0.7143(7) 0.29601(16) 0.0410(8) Uani d 1 . .
H H16 0.404496 0.884332 0.310034 0.049 Uiso calc 1 . .
C C17 0.4910(4) 0.6807(7) 0.23383(16) 0.0405(9) Uani d 1 . .
C C18 0.5876(5) 0.4754(8) 0.22322(18) 0.0463(9) Uani d 1 . .
H H18 0.620600 0.356662 0.257043 0.056 Uiso calc 1 . .
C C19 0.6358(5) 0.4437(9) 0.16319(18) 0.0509(10) Uani d 1 . .
H H19 0.702781 0.304857 0.155381 0.061 Uiso calc 1 . .
C C20 0.5843(4) 0.6185(9) 0.11485(17) 0.0491(10) Uani d 1 . .
C C21 0.4894(5) 0.8217(8) 0.12357(17) 0.0545(11) Uani d 1 . .
H H21 0.455193 0.937239 0.089234 0.065 Uiso calc 1 . .
C C22 0.4445(5) 0.8546(8) 0.18362(17) 0.0526(10) Uani d 1 . .
H H22 0.380496 0.998273 0.191162 0.063 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 0.0515(15) 0.0606(18) 0.0328(13) -0.0128(14) 0.0139(11) -0.0079(12)
O2 0.0605(16) 0.0307(12) 0.0321(12) 0.0011(13) 0.0101(11) -0.0015(11)
O3 0.076(2) 0.168(4) 0.0489(19) 0.040(3) 0.0199(16) -0.007(2)
O4 0.113(3) 0.086(2) 0.0419(17) -0.015(2) 0.0324(17) 0.0032(17)
N1 0.0571(18) 0.0288(16) 0.0259(14) 0.0000(15) 0.0105(12) -0.0017(12)
N2 0.0492(17) 0.0322(15) 0.0274(15) 0.0007(14) 0.0087(12) -0.0020(12)
N3 0.059(2) 0.094(3) 0.038(2) -0.011(2) 0.0142(17) -0.008(2)
C1 0.065(3) 0.110(4) 0.043(2) -0.008(3) 0.023(2) -0.018(2)
C2 0.0412(19) 0.068(3) 0.035(2) -0.014(2) 0.0156(15) -0.0043(19)
C3 0.092(3) 0.069(3) 0.031(2) 0.011(3) -0.002(2) 0.0080(19)
C4 0.083(3) 0.070(3) 0.044(2) 0.034(3) -0.001(2) 0.002(2)
C5 0.0385(19) 0.049(2) 0.0337(18) -0.0054(19) 0.0090(15) -0.0003(16)
C6 0.064(2) 0.065(3) 0.035(2) 0.015(2) -0.0024(18) 0.0006(19)
C7 0.055(2) 0.094(4) 0.046(2) 0.025(3) 0.0002(19) -0.015(2)
C8 0.048(2) 0.056(2) 0.037(2) -0.008(2) 0.0126(16) -0.0022(18)
C9 0.0385(19) 0.042(2) 0.0282(17) 0.0001(17) 0.0049(14) -0.0003(15)
C10 0.0410(19) 0.037(2) 0.0396(19) -0.0052(17) 0.0121(16) -0.0015(16)
C11 0.0473(19) 0.0326(17) 0.0349(19) -0.0044(17) 0.0051(15) -0.0069(15)
C12 0.0395(19) 0.0279(17) 0.0259(16) 0.0045(16) 0.0035(14) -0.0016(13)
C13 0.0467(19) 0.039(2) 0.0311(17) -0.0066(18) 0.0073(15) -0.0001(16)
C14 0.049(2) 0.043(2) 0.0333(19) -0.0072(19) 0.0019(15) -0.0074(16)
C15 0.0373(19) 0.0297(18) 0.0276(16) 0.0041(16) 0.0006(14) -0.0006(14)
C16 0.061(2) 0.0318(18) 0.0320(18) -0.0014(18) 0.0108(16) -0.0054(15)
C17 0.056(2) 0.036(2) 0.0312(18) -0.0137(18) 0.0114(16) -0.0051(15)
C18 0.054(2) 0.048(2) 0.038(2) -0.008(2) 0.0104(17) -0.0014(17)
C19 0.051(2) 0.057(2) 0.047(2) -0.009(2) 0.0170(18) -0.010(2)
C20 0.051(2) 0.068(3) 0.0306(19) -0.019(2) 0.0144(16) -0.007(2)
C21 0.079(3) 0.054(3) 0.032(2) -0.018(2) 0.0133(19) 0.0022(18)
C22 0.082(3) 0.040(2) 0.039(2) -0.006(2) 0.021(2) 0.0025(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
C9 O1 C8 . . 117.8(3) ?
C15 N1 N2 . . 119.1(3) ?
C15 N1 H1 . . 124(2) ?
N2 N1 H1 . . 117(2) ?
C16 N2 N1 . . 116.0(3) ?
O4 N3 O3 . . 124.3(4) ?
O4 N3 C20 . . 118.1(4) ?
O3 N3 C20 . . 117.7(4) ?
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
C3 C2 C7 . . 117.0(4) ?
C3 C2 C1 . . 121.6(4) ?
C7 C2 C1 . . 121.4(4) ?
C2 C3 C4 . . 121.8(4) ?
C2 C3 H3 . . 119.1 ?
C4 C3 H3 . . 119.1 ?
C3 C4 C5 . . 120.9(4) ?
C3 C4 H4 . . 119.5 ?
C5 C4 H4 . . 119.5 ?
C6 C5 C4 . . 117.6(4) ?
C6 C5 C8 . . 121.1(3) ?
C4 C5 C8 . . 121.2(4) ?
C5 C6 C7 . . 121.3(4) ?
C5 C6 H6 . . 119.3 ?
C7 C6 H6 . . 119.3 ?
C6 C7 C2 . . 121.4(4) ?
C6 C7 H7 . . 119.3 ?
C2 C7 H7 . . 119.3 ?
O1 C8 C5 . . 108.1(3) ?
O1 C8 H8A . . 110.1 ?
C5 C8 H8A . . 110.1 ?
O1 C8 H8B . . 110.1 ?
C5 C8 H8B . . 110.1 ?
H8A C8 H8B . . 108.4 ?
O1 C9 C14 . . 115.7(3) ?
O1 C9 C10 . . 125.0(3) ?
C14 C9 C10 . . 119.3(3) ?
C11 C10 C9 . . 119.5(3) ?
C11 C10 H10 . . 120.2 ?
C9 C10 H10 . . 120.2 ?
C10 C11 C12 . . 121.9(3) ?
C10 C11 H11 . . 119.1 ?
C12 C11 H11 . . 119.1 ?
C11 C12 C13 . . 117.9(3) ?
C11 C12 C15 . . 118.8(3) ?
C13 C12 C15 . . 123.3(3) ?
C14 C13 C12 . . 120.4(3) ?
C14 C13 H13 . . 119.8 ?
C12 C13 H13 . . 119.8 ?
C13 C14 C9 . . 120.9(3) ?
C13 C14 H14 . . 119.5 ?
C9 C14 H14 . . 119.5 ?
O2 C15 N1 . . 122.1(3) ?
O2 C15 C12 . . 121.7(3) ?
N1 C15 C12 . . 116.2(3) ?
N2 C16 C17 . . 118.7(3) ?
N2 C16 H16 . . 120.6 ?
C17 C16 H16 . . 120.6 ?
C18 C17 C22 . . 119.3(3) ?
C18 C17 C16 . . 121.6(3) ?
C22 C17 C16 . . 119.1(3) ?
C19 C18 C17 . . 119.8(4) ?
C19 C18 H18 . . 120.1 ?
C17 C18 H18 . . 120.1 ?
C20 C19 C18 . . 118.6(4) ?
C20 C19 H19 . . 120.7 ?
C18 C19 H19 . . 120.7 ?
C21 C20 C19 . . 123.1(3) ?
C21 C20 N3 . . 118.5(4) ?
C19 C20 N3 . . 118.4(4) ?
C20 C21 C22 . . 117.9(4) ?
C20 C21 H21 . . 121.1 ?
C22 C21 H21 . . 121.1 ?
C21 C22 C17 . . 121.3(4) ?
C21 C22 H22 . . 119.3 ?
C17 C22 H22 . . 119.3 ?
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 C9 . 1.363(4) ?
O1 C8 . 1.437(4) ?
O2 C15 . 1.237(4) ?
O3 N3 . 1.231(6) ?
O4 N3 . 1.227(5) ?
N1 C15 . 1.358(4) ?
N1 N2 . 1.376(4) ?
N1 H1 . 0.90(4) ?
N2 C16 . 1.279(4) ?
N3 C20 . 1.480(5) ?
C1 C2 . 1.511(5) ?
C1 H1A . 0.9800 ?
C1 H1B . 0.9800 ?
C1 H1C . 0.9800 ?
C2 C3 . 1.353(6) ?
C2 C7 . 1.386(5) ?
C3 C4 . 1.379(6) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.381(5) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.352(6) ?
C5 C8 . 1.500(5) ?
C6 C7 . 1.377(5) ?
C6 H6 . 0.9500 ?
C7 H7 . 0.9500 ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 C14 . 1.382(5) ?
C9 C10 . 1.395(5) ?
C10 C11 . 1.373(4) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.395(5) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.396(5) ?
C12 C15 . 1.477(4) ?
C13 C14 . 1.379(5) ?
C13 H13 . 0.9500 ?
C14 H14 . 0.9500 ?
C16 C17 . 1.472(5) ?
C16 H16 . 0.9500 ?
C17 C18 . 1.385(5) ?
C17 C22 . 1.398(5) ?
C18 C19 . 1.385(5) ?
C18 H18 . 0.9500 ?
C19 C20 . 1.383(6) ?
C19 H19 . 0.9500 ?
C20 C21 . 1.360(6) ?
C21 C22 . 1.374(5) ?
C21 H21 . 0.9500 ?
C22 H22 . 0.9500 ?
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
C14 H14 N2 2_656 0.95 2.68 3.524(5) 148.3 yes
C16 H16 O2 1_565 0.95 2.45 3.259(4) 143.1 yes
C21 H21 O4 2_655 0.95 2.59 3.532(5) 171.2 yes
N1 H1 O2 1_565 0.90(4) 2.04(4) 2.911(4) 161(3) 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 N1 N2 C16 . . . . 166.0(3) ?
C7 C2 C3 C4 . . . . 0.3(7) ?
C1 C2 C3 C4 . . . . -179.5(5) ?
C2 C3 C4 C5 . . . . -0.5(8) ?
C3 C4 C5 C6 . . . . 0.2(7) ?
C3 C4 C5 C8 . . . . 179.3(4) ?
C4 C5 C6 C7 . . . . 0.2(6) ?
C8 C5 C6 C7 . . . . -178.9(4) ?
C5 C6 C7 C2 . . . . -0.4(7) ?
C3 C2 C7 C6 . . . . 0.2(7) ?
C1 C2 C7 C6 . . . . 179.9(4) ?
C9 O1 C8 C5 . . . . -170.9(3) ?
C6 C5 C8 O1 . . . . 80.9(4) ?
C4 C5 C8 O1 . . . . -98.2(5) ?
C8 O1 C9 C14 . . . . 177.9(3) ?
C8 O1 C9 C10 . . . . -3.5(5) ?
O1 C9 C10 C11 . . . . 179.5(3) ?
C14 C9 C10 C11 . . . . -2.0(5) ?
C9 C10 C11 C12 . . . . 0.0(5) ?
C10 C11 C12 C13 . . . . 1.1(5) ?
C10 C11 C12 C15 . . . . 177.9(3) ?
C11 C12 C13 C14 . . . . -0.2(5) ?
C15 C12 C13 C14 . . . . -176.9(3) ?
C12 C13 C14 C9 . . . . -1.8(5) ?
O1 C9 C14 C13 . . . . -178.5(3) ?
C10 C9 C14 C13 . . . . 2.9(5) ?
N2 N1 C15 O2 . . . . -5.3(5) ?
N2 N1 C15 C12 . . . . 174.1(3) ?
C11 C12 C15 O2 . . . . -25.7(5) ?
C13 C12 C15 O2 . . . . 151.0(3) ?
C11 C12 C15 N1 . . . . 154.8(3) ?
C13 C12 C15 N1 . . . . -28.5(5) ?
N1 N2 C16 C17 . . . . -179.9(3) ?
N2 C16 C17 C18 . . . . -27.8(5) ?
N2 C16 C17 C22 . . . . 149.9(4) ?
C22 C17 C18 C19 . . . . -0.4(5) ?
C16 C17 C18 C19 . . . . 177.2(4) ?
C17 C18 C19 C20 . . . . -0.6(5) ?
C18 C19 C20 C21 . . . . 0.5(6) ?
C18 C19 C20 N3 . . . . 179.1(4) ?
O4 N3 C20 C21 . . . . 1.5(5) ?
O3 N3 C20 C21 . . . . -177.5(4) ?
O4 N3 C20 C19 . . . . -177.2(4) ?
O3 N3 C20 C19 . . . . 3.9(5) ?
C19 C20 C21 C22 . . . . 0.7(6) ?
N3 C20 C21 C22 . . . . -177.9(3) ?
C20 C21 C22 C17 . . . . -1.8(6) ?
C18 C17 C22 C21 . . . . 1.7(6) ?
C16 C17 C22 C21 . . . . -176.0(3) ?