#------------------------------------------------------------------------------
#$Date: 2024-12-24 05:04:14 +0200 (Tue, 24 Dec 2024) $
#$Revision: 296961 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/35/1573531.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_1573531
loop_
_publ_author_name
'Abdul Rashid, Fatin Nur Ain'
'Mohammat, Mohd Fazli'
'Abdul Manan, Mohd Abdul Fatah'
'Bakhtiar Afendy, Ayisy Amirul Afti'
'Cordes, David B.'
'McKay, Aidan P.'
_publ_section_title
;
Ethyl
4-[(2-hydroxyethyl)amino]-2-(4-methoxyphenyl)-1-methyl-5-oxo-2,5-dihydro-1H-pyrrole-3-carboxylate
;
_journal_coeditor_code HB4500
_journal_issue 12
_journal_name_full IUCrData
_journal_paper_doi 10.1107/S2414314624012227
_journal_volume 9
_journal_year 2024
_chemical_formula_iupac 'C17 H22 N2 O5'
_chemical_formula_moiety 'C17 H22 N2 O5'
_chemical_formula_sum 'C17 H22 N2 O5'
_chemical_formula_weight 334.36
_chemical_name_systematic
;Ethyl
4-[(2-hydroxyethyl)amino]-2-(4-methoxyphenyl)-1-methyl-5-oxo-2,5-dihydro-1H-pyrrole-3-carboxylate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 90
_cell_angle_beta 101.5111(8)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.17216(8)
_cell_length_b 9.24320(6)
_cell_length_c 17.64603(14)
_cell_measurement_reflns_used 26738
_cell_measurement_temperature 100
_cell_measurement_theta_max 75.2450
_cell_measurement_theta_min 4.6300
_cell_volume 1625.77(2)
_computing_cell_refinement
;
CrysAlisPro 1.171.43.109a (Rigaku OD, 2024)
;
_computing_data_collection
;
CrysAlisPro 1.171.43.109a (Rigaku OD, 2024)
;
_computing_data_reduction
;
CrysAlisPro 1.171.43.109a (Rigaku OD, 2024)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al., 2009), publCIF (Westrip,
2010)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100
_diffrn_detector 'hybrid photon counting detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device 'AFC11: Quarter \c 4 circle'
_diffrn_measurement_device_type 'Rigaku XtaLAB P200K'
_diffrn_measurement_method 'shutterless scans'
_diffrn_measurement_specimen_support Loop
_diffrn_radiation_monochromator 'Rigaku Osmic Confocal Optical System'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0706
_diffrn_reflns_av_unetI/netI 0.0224
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 57922
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 75.636
_diffrn_reflns_theta_min 4.658
_diffrn_source 'Rotating Anode'
_exptl_absorpt_coefficient_mu 0.839
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.73497
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2024)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.366
_exptl_crystal_description plate
_exptl_crystal_F_000 712
_exptl_crystal_size_max 0.09
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.01
_refine_diff_density_max 0.277
_refine_diff_density_min -0.273
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.057
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 230
_refine_ls_number_reflns 3336
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.058
_refine_ls_R_factor_all 0.0436
_refine_ls_R_factor_gt 0.0400
_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^)+(0.0505P)^2^+0.7868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1040
_refine_ls_wR_factor_ref 0.1064
_reflns_number_gt 3074
_reflns_number_total 3336
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb4500.cif
_cod_data_source_block I
_cod_database_code 1573531
_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 0.928
_shelx_estimated_absorpt_t_max 0.992
_shelx_hkl_file
;
0 0 1 0.03 0.14
0 0 1 -0.07 0.14
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0 0 -1 -0.01 0.08
0 0 -1 0.01 0.05
0 0 -2 284.61 21.16
0 0 -2 296.39 21.16
0 0 2 292.27 21.17
0 0 -2 303.11 21.15
0 0 2 293.40 21.22
0 0 2 290.11 21.18
0 0 -2 297.21 21.23
0 0 2 282.03 21.23
0 0 -2 298.55 21.19
0 0 2 286.83 21.17
0 0 2 281.65 21.23
0 0 -2 300.04 21.24
0 0 2 287.01 21.16
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0 0 3 -0.26 0.26
0 0 -4 2331.55 176.79
0 0 -4 2469.66 176.80
0 0 -4 2420.61 176.78
0 0 -4 2662.17 176.77
0 0 4 2421.71 176.79
0 0 4 2360.04 176.90
0 0 -4 2586.87 176.85
0 0 -4 2318.26 176.93
0 0 -4 2651.69 176.81
0 0 4 2394.59 176.78
0 0 4 2350.04 176.81
0 0 -4 2336.22 176.93
0 0 4 2301.03 176.79
0 0 -5 0.01 0.34
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0 0 5 -0.22 0.56
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0 0 -6 485.28 32.60
0 0 -6 436.41 32.57
0 0 -6 443.45 32.55
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0 0 -6 455.66 32.81
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0 0 -7 0.29 0.27
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0 0 -8 37.02 3.18
0 0 -8 40.18 2.76
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0 0 -8 40.67 2.81
0 0 -8 37.75 2.73
0 0 -8 36.73 2.76
0 0 -8 39.28 2.75
0 0 -8 36.28 2.76
0 0 8 36.88 2.76
0 0 -8 25.36 2.64
0 0 8 36.24 2.98
0 0 8 40.03 2.76
0 0 8 39.29 2.77
0 0 -8 38.15 3.15
0 0 8 36.40 2.74
0 0 9 0.30 0.41
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0 0 -9 -0.06 0.23
0 0 9 0.06 0.49
0 0 -9 0.39 0.93
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0 0 -9 0.07 0.55
0 0 -9 0.47 0.86
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0 0 10 11.31 1.17
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0 0 -10 8.69 1.04
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0 0 -10 11.59 1.15
0 0 -10 13.39 1.16
0 0 -10 14.11 1.21
0 0 -10 12.81 1.12
0 0 -10 12.23 1.64
0 0 -11 0.77 1.01
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0 0 -11 0.08 0.45
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0 0 11 0.31 0.53
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0 0 -12 -0.12 0.81
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0 0 16 46.34 3.59
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0 0 16 50.22 3.64
0 0 16 46.67 3.57
0 0 -16 52.98 3.71
0 0 -16 49.33 3.65
0 0 -16 53.21 3.82
0 0 -16 54.94 3.80
0 0 -16 47.21 3.64
0 0 -16 44.61 4.45
0 0 16 28.47 3.43
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10 -2 -6 -0.30 0.72
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10 -2 -5 0.20 0.66
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10 -2 -5 1.51 0.80
10 2 -5 0.79 0.76
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-10 -2 4 10.15 1.21
-10 -2 4 9.16 1.15
-10 -2 4 10.47 1.22
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10 -2 -4 11.06 1.24
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-10 -2 4 10.51 1.11
10 2 -4 13.17 1.40
10 2 -4 11.05 1.43
10 -2 -4 10.18 1.27
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10 2 -4 10.35 1.29
-10 -2 4 9.93 1.10
10 -2 -4 10.55 1.31
10 2 -4 9.99 1.31
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-10 -2 3 24.39 2.09
-10 -2 3 25.75 2.15
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-10 2 3 26.32 2.13
-10 -2 3 25.37 2.07
10 2 -3 23.14 2.27
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-10 -2 3 19.87 2.00
10 2 -3 22.25 2.18
10 -2 -3 26.38 2.25
10 2 -3 23.47 2.22
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-10 -2 3 22.68 2.04
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-10 -2 2 15.70 1.49
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-10 -2 2 16.68 1.48
10 2 -2 15.95 1.67
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-10 -2 2 14.36 1.42
10 2 -2 17.39 1.66
10 -2 -2 11.78 1.53
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-10 -2 -1 207.87 14.48
-10 -2 -1 160.78 14.38
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-10 -2 -1 226.70 14.51
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-10 -2 -1 214.21 14.49
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-10 -2 -5 36.18 2.60
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-10 -2 -6 20.27 1.49
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-10 5 6 10.27 1.03
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10 5 -6 6.02 0.83
-10 -5 5 1.92 0.48
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-11 3 8 0.51 0.46
11 3 -8 0.16 0.53
11 -3 -8 0.15 0.70
-11 -3 8 0.20 0.42
-11 3 8 0.94 0.49
-11 3 8 0.68 0.32
11 3 -8 0.46 0.32
-11 -3 8 1.09 0.47
11 -3 -7 7.85 0.93
-11 3 7 8.88 0.87
-11 3 7 8.56 0.87
11 3 -7 8.01 0.96
11 -3 -7 8.56 1.10
-11 3 7 4.69 0.69
-11 3 7 9.14 0.89
-11 -3 7 8.88 0.83
11 3 -7 4.65 0.75
-11 -3 7 9.51 0.87
11 -3 -6 1.33 0.80
-11 3 6 1.61 0.53
-11 3 6 0.64 0.51
-11 3 6 0.90 0.38
-11 -3 6 0.74 0.46
11 3 -6 1.28 0.49
-11 3 6 1.74 0.56
11 -3 -5 2.62 0.82
11 3 -5 0.86 0.62
-11 3 5 1.55 0.55
-11 3 5 1.26 0.41
-11 3 5 1.44 0.57
11 3 -5 0.88 0.53
-11 -3 5 2.33 0.53
11 -3 -4 46.21 3.24
11 3 -4 42.67 3.19
11 3 -4 33.76 3.09
-11 3 4 49.31 3.16
-11 -3 4 46.88 3.09
-11 3 4 28.13 2.95
-11 3 4 45.29 3.13
-11 -3 3 12.40 1.04
11 -3 -3 13.16 1.26
11 3 -3 9.79 1.15
11 3 -3 13.29 1.21
-11 -3 3 13.07 1.09
11 3 -3 11.63 1.17
-11 3 2 -0.08 0.50
-11 -3 2 -0.21 0.40
11 -3 -2 1.00 0.69
-11 3 2 -0.68 0.37
11 3 -2 0.05 0.56
-11 -3 2 0.46 0.45
11 3 -2 0.09 0.57
-11 -3 1 0.48 0.46
-11 3 1 0.14 0.32
-11 3 1 0.48 0.49
-11 -3 1 0.66 0.45
11 -3 -1 0.70 0.63
11 3 -1 0.79 0.57
-11 -3 1 0.34 0.33
-11 3 1 -0.34 0.54
11 3 -1 0.86 0.59
11 3 -1 0.84 0.57
-11 -3 0 0.36 0.43
-11 -3 0 -0.32 0.33
11 3 0 -0.04 0.49
-11 3 0 0.28 0.49
11 3 0 0.41 0.53
-11 -3 0 0.50 0.36
-11 3 0 0.17 0.48
-11 -3 0 -0.19 0.42
-11 -3 -1 0.40 0.40
-11 -3 -1 0.41 0.34
11 3 1 0.29 0.42
-11 3 -1 0.58 0.46
11 3 1 0.46 0.52
-11 -3 -1 0.03 0.33
-11 3 -1 0.89 0.44
-11 -3 -1 0.79 0.45
-11 -3 -2 20.01 1.53
-11 -3 -2 15.56 1.45
11 3 2 17.96 1.50
-11 3 -2 16.43 1.48
11 3 2 20.02 1.60
-11 3 -2 13.60 1.44
-11 -3 -2 21.97 1.50
-11 3 -2 23.77 1.55
-11 -3 -3 0.29 0.31
11 3 3 -0.27 0.42
-11 3 -3 -0.06 0.26
-11 -3 -3 -0.17 0.29
-11 -3 -3 0.05 0.33
-11 3 -3 -0.29 0.32
11 3 3 0.19 0.43
11 3 4 0.66 0.37
-11 -3 -4 0.54 0.28
-11 -3 -4 0.75 0.30
-11 -3 -4 0.81 0.32
-11 -3 -5 8.08 0.73
-11 4 11 0.27 0.45
-11 4 10 2.43 0.46
-11 4 10 1.55 0.38
-11 4 10 1.99 0.40
-11 4 9 28.39 2.12
11 4 -9 24.52 2.10
-11 4 9 29.59 2.12
-11 4 9 30.34 2.12
-11 -4 9 23.49 2.03
11 4 -8 1.43 0.46
11 -4 -8 2.49 0.72
11 -4 -8 1.55 0.57
-11 4 8 1.34 0.46
-11 -4 8 1.09 0.35
-11 4 8 1.98 0.49
11 4 -7 11.82 1.18
11 -4 -7 14.38 1.33
-11 4 7 13.14 1.15
11 -4 -7 11.89 1.19
-11 4 7 12.45 1.15
-11 -4 7 11.47 1.05
-11 4 6 3.77 0.60
11 -4 -6 3.47 0.78
-11 4 6 2.72 0.57
-11 4 6 2.46 0.56
-11 -4 6 3.12 0.47
11 4 -6 1.58 0.43
11 -4 -5 1.36 0.73
-11 4 5 1.85 0.56
-11 -4 5 0.40 0.36
11 4 -5 0.28 0.40
-11 4 5 1.21 0.48
11 4 -5 1.98 0.60
-11 4 4 11.14 1.06
11 4 -4 10.14 1.11
-11 -4 4 10.95 0.98
11 4 -4 9.90 1.05
-11 4 4 10.98 1.08
11 -4 -4 11.42 1.21
-11 -4 3 0.55 0.38
11 -4 -3 0.12 0.65
-11 -4 3 0.38 0.29
11 4 -3 -0.25 0.47
11 4 -3 0.51 0.57
-11 4 3 0.23 0.45
-11 -4 2 25.11 2.41
11 4 -2 36.17 2.59
-11 4 2 43.99 2.60
11 4 -2 37.60 2.59
-11 -4 2 39.72 2.49
11 4 -2 21.36 2.41
-11 4 2 42.76 2.58
-11 -4 1 5.04 0.56
-11 -4 1 3.18 0.51
-11 4 1 6.12 0.70
11 4 -1 4.68 0.69
-11 4 1 7.37 0.67
11 4 -1 3.42 0.54
-11 -4 0 0.48 0.33
11 4 0 1.12 0.44
-11 4 0 0.55 0.43
11 4 0 0.13 0.46
-11 4 0 0.37 0.38
11 4 0 0.18 0.33
-11 -4 -1 9.62 0.86
-11 -4 -1 10.09 0.87
11 4 1 9.60 0.92
-11 4 -1 9.07 0.88
11 4 1 10.63 0.97
11 4 1 11.28 0.92
-11 4 -1 7.61 0.86
-11 -4 -2 3.20 0.43
11 4 2 2.68 0.52
-11 -4 -2 2.66 0.39
11 4 2 3.85 0.48
11 4 3 0.81 0.39
-11 5 9 6.49 0.65
-11 5 9 4.89 0.67
-11 5 8 4.81 0.59
-11 5 8 3.63 0.58
11 5 -8 3.61 0.49
-11 5 8 4.42 0.54
-11 5 7 2.92 0.49
11 5 -7 1.82 0.44
-11 5 7 1.83 0.38
-11 5 6 0.25 0.40
-11 5 6 0.49 0.36
11 5 -6 0.75 0.44
-11 5 6 0.15 0.31
-11 5 5 1.70 0.49
-11 5 5 2.66 0.46
11 5 -4 3.75 0.50
-11 5 4 4.57 0.55
11 5 -4 3.56 0.60
-11 5 3 28.77 2.08
11 5 -3 23.48 2.02
-11 5 3 26.89 2.03
11 5 -3 24.38 2.07
-11 5 2 5.18 0.56
-11 -5 2 4.32 0.51
11 5 -2 4.15 0.63
11 5 -2 5.13 0.60
-11 -5 1 0.19 0.25
11 5 -1 0.15 0.36
-11 5 1 0.53 0.35
11 5 -1 0.23 0.37
11 5 0 2.30 0.41
11 5 1 4.99 0.68
11 5 2 0.34 0.46
-12 0 11 -0.12 0.46
12 0 -10 1.18 0.35
-12 0 10 1.31 0.42
12 0 -9 0.22 0.39
12 0 -8 13.18 1.29
-12 0 8 14.24 1.21
12 0 -8 16.98 1.41
-12 0 7 -0.27 0.39
-12 0 7 -0.02 0.32
12 0 -7 0.24 0.63
-12 0 6 9.99 0.94
-12 0 6 8.79 0.88
12 0 -6 10.20 1.09
-12 0 5 0.47 0.46
-12 0 5 -0.37 0.38
12 0 -5 0.36 0.63
-12 0 4 64.50 4.69
12 0 -4 53.63 4.72
-12 0 4 64.88 4.71
12 0 -4 66.79 4.79
-12 0 3 -0.03 0.40
12 0 -3 0.11 0.47
-12 0 3 0.03 0.46
12 0 -3 -0.07 0.58
12 0 -2 1.72 0.53
-12 0 2 1.99 0.53
-12 0 2 2.16 0.47
-12 0 1 -0.35 0.42
12 0 -1 0.84 0.44
-12 0 1 0.06 0.38
-12 0 0 2.16 0.45
-12 0 0 1.99 0.42
12 0 0 1.57 0.42
-12 0 0 2.45 0.47
-12 0 -1 -0.04 0.32
-12 0 -1 -0.05 0.31
-12 0 -1 0.29 0.36
12 0 2 1.81 0.38
-12 0 -2 2.13 0.43
-12 0 -2 1.90 0.41
-12 0 -3 0.56 0.44
-12 -1 11 6.37 0.71
-12 -1 10 -0.25 0.42
-12 1 10 0.29 0.29
12 1 -9 1.01 0.41
-12 1 9 0.26 0.29
-12 -1 9 0.73 0.37
-12 1 9 0.63 0.33
-12 1 8 2.18 0.38
12 1 -8 1.96 0.50
-12 1 8 2.14 0.44
-12 -1 8 2.09 0.44
-12 1 8 1.89 0.42
12 -1 -8 1.60 0.64
12 1 -8 1.03 0.58
-12 1 7 26.17 2.07
-12 -1 7 27.62 2.08
-12 1 7 24.90 2.05
-12 1 7 25.37 2.05
12 -1 -7 25.76 2.19
12 1 -7 27.53 2.20
-12 1 6 0.57 0.37
-12 -1 6 0.50 0.32
12 1 -6 0.40 0.51
-12 -1 6 0.22 0.42
-12 1 6 0.88 0.47
-12 1 6 0.43 0.38
12 -1 -6 1.00 0.65
12 1 -6 1.02 0.63
-12 1 5 0.14 0.38
-12 -1 5 -0.27 0.35
12 1 -5 -0.33 0.51
-12 1 5 0.05 0.39
-12 1 5 0.20 0.42
-12 -1 5 -0.39 0.42
12 -1 -5 0.52 0.59
12 1 -5 -0.12 0.59
-12 1 4 6.35 0.76
-12 -1 4 6.59 0.73
-12 1 4 7.74 0.82
-12 -1 4 8.00 0.79
-12 1 4 7.42 0.77
12 1 -4 5.96 0.85
12 -1 -4 7.29 0.91
12 1 -4 8.51 0.94
12 1 -3 4.67 0.74
-12 1 3 6.70 0.70
-12 -1 3 4.94 0.63
-12 1 3 5.54 0.67
-12 -1 3 4.89 0.67
-12 1 3 6.42 0.74
12 -1 -3 6.05 0.81
12 1 -3 5.93 0.80
-12 -1 2 0.82 0.44
-12 1 2 0.84 0.40
12 1 -2 0.65 0.44
-12 1 2 0.43 0.41
-12 -1 2 0.65 0.38
-12 -1 1 4.69 0.58
-12 1 1 4.73 0.56
-12 1 1 3.62 0.50
12 -1 -1 3.64 0.58
12 1 -1 3.85 0.59
-12 1 1 4.27 0.58
-12 -1 1 4.30 0.56
12 -1 0 1.07 0.37
12 1 0 0.53 0.36
-12 -1 0 1.44 0.41
-12 1 0 0.93 0.34
-12 1 0 1.80 0.44
-12 -1 0 1.27 0.34
-12 -1 0 1.75 0.40
-12 1 -1 0.07 0.26
-12 -1 -1 0.27 0.35
12 1 1 -0.18 0.39
-12 -1 -1 0.19 0.30
-12 -1 -2 0.04 0.43
12 1 2 0.61 0.34
-12 1 -2 -0.27 0.38
-12 -1 -2 0.28 0.37
-12 -1 -3 7.34 0.72
-12 -2 10 4.79 0.60
-12 -2 9 0.44 0.36
12 2 -9 -0.17 0.32
-12 2 8 15.09 1.26
12 2 -8 13.15 1.30
-12 2 8 16.71 1.27
-12 -2 8 15.95 1.27
-12 2 7 81.73 5.34
12 2 -7 73.21 5.37
-12 2 7 87.33 5.35
-12 -2 7 85.85 5.34
-12 2 7 63.17 5.27
12 2 -7 51.24 5.27
12 -2 -7 91.79 5.47
-12 2 6 1.70 0.39
-12 2 6 1.29 0.45
-12 -2 6 1.36 0.39
-12 2 6 0.31 0.29
12 2 -6 1.23 0.40
12 -2 -6 1.10 0.61
12 2 -5 3.22 0.58
-12 2 5 2.93 0.49
-12 2 5 1.98 0.41
-12 2 5 4.19 0.56
-12 -2 5 3.49 0.50
12 2 -5 3.13 0.53
12 -2 -5 4.00 0.70
12 2 -4 0.92 0.47
-12 2 4 -0.38 0.31
-12 2 4 -0.08 0.41
12 2 -4 0.39 0.43
-12 -2 4 -0.07 0.37
-12 2 4 0.32 0.38
12 2 -3 66.68 5.00
-12 2 3 73.34 4.99
-12 -2 3 75.16 4.96
-12 2 3 73.71 4.98
-12 -2 3 70.16 4.92
12 2 -2 0.32 0.41
-12 -2 2 0.97 0.40
-12 2 2 0.36 0.29
-12 -2 2 0.41 0.28
-12 -2 2 0.34 0.34
12 2 -1 1.94 0.45
-12 -2 1 2.07 0.42
-12 2 1 1.52 0.45
12 2 -1 1.64 0.50
-12 -2 1 1.55 0.33
-12 -2 1 1.97 0.40
12 2 0 0.28 0.30
-12 -2 0 0.65 0.36
-12 -2 0 0.93 0.36
-12 2 0 0.04 0.35
12 2 0 0.79 0.44
-12 -2 0 0.14 0.25
-12 2 0 0.39 0.35
-12 -2 0 0.78 0.33
-12 -2 -1 -0.58 0.42
12 2 1 -0.05 0.46
-12 2 -1 0.11 0.27
-12 -2 -1 0.08 0.23
-12 -2 -2 8.32 0.81
12 3 -8 27.88 2.42
-12 3 8 34.74 2.41
12 3 -7 7.90 0.92
-12 3 7 10.30 0.87
-12 -3 7 8.34 0.77
-12 3 7 9.66 0.86
-12 3 6 19.15 1.49
-12 -3 6 16.37 1.41
-12 3 6 19.10 1.47
12 3 -5 2.91 0.58
-12 -3 5 3.68 0.47
-12 3 5 4.67 0.59
12 3 -5 3.59 0.48
-12 3 5 4.38 0.54
12 3 -4 16.35 1.52
-12 3 4 21.36 1.53
12 3 -4 16.94 1.47
-12 -3 4 18.09 1.44
-12 -3 3 1.44 0.33
12 3 -3 0.98 0.43
12 3 -3 0.80 0.40
12 3 -2 0.58 0.38
-12 -3 2 0.05 0.28
-12 3 2 0.33 0.44
-12 3 2 0.02 0.37
12 3 -1 0.27 0.32
-12 3 1 1.29 0.43
-12 -3 1 0.86 0.33
12 3 0 0.23 0.50
-12 -3 0 0.19 0.34
0 0 0 0.00 0.00
TITL fatah6 in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 1.54184 10.172163 9.243196 17.646027 90.0000 101.5111 90.0000
ZERR 4.00 0.000084 0.000063 0.000141 0.0000 0.0008 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N O
UNIT 68.00 88.00 8.00 20.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 9299
_shelx_res_file
;
TITL fatah6_a.res in P2(1)/n
fatah6.res
created by SHELXL-2019/3 at 15:27:20 on 15-Oct-2024
REM Old TITL fatah6 in P21/n #14
REM SHELXT solution in P2(1)/n: R1 0.128, Rweak 0.021, Alpha 0.023
REM 0.727 for 220 systematic absences, Orientation as input
REM Formula found by SHELXT: C17 N3 O4
CELL 1.54184 10.172163 9.243196 17.646027 90 101.5111 90
ZERR 4 0.000084 0.000063 0.000141 0 0.0008 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 68 88 8 20
EQIV $1 1-X,-Y,1-Z
DFIX 0.98 N19 H19
DFIX 0.98 0.005 O22 H22A
DFIX 0.98 O22 H22B
L.S. 10 0 0
PLAN 5
SIZE 0.01 0.07 0.09
TEMP -173.15
CONF
HTAB O22 O22_$1
HTAB N19 O15
HTAB O22 O15_$1
list 4
MORE -1
BOND $H
fmap 2
acta
REM
REM
REM
WGHT 0.050500 0.786800
FVAR 0.36099
O5 4 0.341086 0.328285 0.291960 11.00000 0.02696 0.02453 =
0.02874 -0.00001 -0.00582 -0.00311
O13 4 0.939885 0.928480 0.319840 11.00000 0.02917 0.02951 =
0.02762 0.00768 0.00466 -0.00532
O15 4 0.802937 0.226641 0.491824 11.00000 0.03211 0.02069 =
0.03610 -0.00202 -0.00756 0.00338
O16 4 0.809049 0.460535 0.529442 11.00000 0.02467 0.02082 =
0.02224 0.00020 -0.00281 -0.00094
O22 4 0.404439 -0.063923 0.441639 11.00000 0.04705 0.04091 =
0.02768 0.00507 0.00155 -0.01622
H22A 2 0.321168 -0.096019 0.456678 10.50000 -1.50000
PART -1
H22B 2 0.479711 -0.017177 0.476627 10.50000 -1.50000
PART 0
N1 3 0.455734 0.515250 0.362002 11.00000 0.02006 0.01982 =
0.02508 0.00059 -0.00003 -0.00004
N19 3 0.572067 0.150142 0.377819 11.00000 0.02431 0.01806 =
0.02398 0.00025 -0.00070 -0.00111
H19 2 0.647368 0.113265 0.409830 11.00000 0.03523
C2 1 0.578050 0.540349 0.420037 11.00000 0.02113 0.01922 =
0.01885 -0.00039 0.00150 -0.00054
AFIX 13
H2 2 0.553384 0.575074 0.469032 11.00000 -1.20000
AFIX 0
C3 1 0.634224 0.388697 0.431898 11.00000 0.02284 0.01905 =
0.01885 0.00071 0.00375 -0.00161
C4 1 0.553603 0.293141 0.385039 11.00000 0.02193 0.02072 =
0.01797 0.00190 0.00426 -0.00153
C5 1 0.436109 0.376088 0.339291 11.00000 0.02240 0.02055 =
0.02200 0.00194 0.00342 -0.00104
C6 1 0.367250 0.632251 0.329252 11.00000 0.02435 0.02233 =
0.03274 0.00261 0.00003 0.00311
AFIX 137
H6A 2 0.410681 0.690047 0.294676 11.00000 -1.50000
H6B 2 0.348131 0.693750 0.370983 11.00000 -1.50000
H6C 2 0.283186 0.591964 0.299979 11.00000 -1.50000
AFIX 0
C7 1 0.670474 0.649845 0.393455 11.00000 0.02023 0.01836 =
0.01984 0.00185 0.00043 0.00178
C8 1 0.706290 0.635047 0.321517 11.00000 0.02930 0.02340 =
0.02023 -0.00279 0.00201 -0.00248
AFIX 43
H8 2 0.670204 0.557712 0.288350 11.00000 -1.20000
AFIX 0
C9 1 0.793744 0.731813 0.298067 11.00000 0.03049 0.03069 =
0.01912 0.00201 0.00593 -0.00085
AFIX 43
H9 2 0.816202 0.721865 0.248590 11.00000 -1.20000
AFIX 0
C10 1 0.848929 0.843824 0.346897 11.00000 0.02167 0.02078 =
0.02374 0.00747 0.00079 0.00099
C11 1 0.811914 0.862077 0.417853 11.00000 0.02593 0.01882 =
0.02373 -0.00126 -0.00001 -0.00160
AFIX 43
H11 2 0.847341 0.940002 0.450770 11.00000 -1.20000
AFIX 0
C12 1 0.722137 0.764744 0.440282 11.00000 0.02472 0.02108 =
0.02001 -0.00060 0.00330 0.00056
AFIX 43
H12 2 0.695973 0.777571 0.488603 11.00000 -1.20000
AFIX 0
C14 1 1.003159 1.039760 0.369320 11.00000 0.04089 0.03820 =
0.04596 -0.00303 0.01294 -0.01943
AFIX 137
H14A 2 1.062776 1.095104 0.342862 11.00000 -1.50000
H14B 2 1.055617 0.996804 0.416585 11.00000 -1.50000
H14C 2 0.934820 1.104289 0.382711 11.00000 -1.50000
AFIX 0
C15 1 0.754999 0.348571 0.485600 11.00000 0.02350 0.01993 =
0.02026 0.00120 0.00422 -0.00353
C17 1 0.931780 0.432523 0.585711 11.00000 0.02221 0.02609 =
0.02236 0.00208 -0.00202 -0.00034
AFIX 23
H17A 2 1.003709 0.398723 0.559586 11.00000 -1.20000
H17B 2 0.916399 0.357827 0.623200 11.00000 -1.20000
AFIX 0
C18 1 0.969736 0.574573 0.626072 11.00000 0.03090 0.02904 =
0.02683 -0.00176 -0.00261 -0.00327
AFIX 137
H18A 2 0.982430 0.647720 0.587974 11.00000 -1.50000
H18B 2 1.053341 0.562775 0.664254 11.00000 -1.50000
H18C 2 0.898122 0.605610 0.652238 11.00000 -1.50000
AFIX 0
C20 1 0.477147 0.048453 0.333048 11.00000 0.03159 0.02220 =
0.02394 -0.00296 -0.00038 -0.00219
AFIX 23
H20A 2 0.525209 -0.041922 0.325556 11.00000 -1.20000
H20B 2 0.441995 0.090415 0.281357 11.00000 -1.20000
AFIX 0
C21 1 0.360723 0.012275 0.370989 11.00000 0.03555 0.02591 =
0.02854 -0.00167 0.00366 -0.00563
AFIX 23
H21A 2 0.315223 0.102708 0.381347 11.00000 -1.20000
H21B 2 0.295103 -0.047698 0.335390 11.00000 -1.20000
AFIX 0
HKLF 4
REM fatah6_a.res in P2(1)/n
REM wR2 = 0.1064, GooF = S = 1.057, Restrained GooF = 1.058 for all data
REM R1 = 0.0400 for 3074 Fo > 4sig(Fo) and 0.0436 for all 3336 data
REM 230 parameters refined using 3 restraints
END
WGHT 0.0505 0.7868
REM Highest difference peak 0.277, deepest hole -0.273, 1-sigma level 0.043
Q1 1 0.6131 0.4691 0.4303 11.00000 0.05 0.28
Q2 1 0.8005 0.7795 0.4349 11.00000 0.05 0.25
Q3 1 0.7210 0.6813 0.4252 11.00000 0.05 0.25
Q4 1 0.6771 0.3704 0.4594 11.00000 0.05 0.25
Q5 1 0.6113 0.3410 0.4035 11.00000 0.05 0.24
;
_shelx_res_checksum 83479
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O5 0.34109(10) 0.32829(11) 0.29196(6) 0.0283(2) Uani d 1 . .
O O13 0.93989(10) 0.92848(11) 0.31984(6) 0.0289(2) Uani d 1 . .
O O15 0.80294(10) 0.22664(11) 0.49182(6) 0.0316(3) Uani d 1 . .
O O16 0.80905(9) 0.46054(10) 0.52944(5) 0.0236(2) Uani d 1 . .
O O22 0.40444(12) -0.06392(13) 0.44164(6) 0.0394(3) Uani d 1 . .
H H22A 0.321(2) -0.096(5) 0.457(2) 0.059 Uiso d 0.5 . .
H H22B 0.480(4) -0.017(5) 0.477(2) 0.059 Uiso d 0.5 A -1
N N1 0.45573(11) 0.51525(12) 0.36200(7) 0.0223(2) Uani d 1 . .
N N19 0.57207(12) 0.15014(12) 0.37782(7) 0.0229(3) Uani d 1 . .
H H19 0.6474(15) 0.1133(19) 0.4098(10) 0.035(5) Uiso d 1 . .
C C2 0.57805(13) 0.54035(14) 0.42004(7) 0.0201(3) Uani d 1 . .
H H2 0.553384 0.575074 0.469032 0.024 Uiso calc 1 . .
C C3 0.63422(13) 0.38870(14) 0.43190(7) 0.0203(3) Uani d 1 . .
C C4 0.55360(13) 0.29314(14) 0.38504(7) 0.0202(3) Uani d 1 . .
C C5 0.43611(13) 0.37609(15) 0.33929(8) 0.0218(3) Uani d 1 . .
C C6 0.36725(14) 0.63225(15) 0.32925(9) 0.0273(3) Uani d 1 . .
H H6A 0.410681 0.690047 0.294676 0.041 Uiso calc 1 . .
H H6B 0.348131 0.693750 0.370983 0.041 Uiso calc 1 . .
H H6C 0.283186 0.591964 0.299979 0.041 Uiso calc 1 . .
C C7 0.67047(13) 0.64984(14) 0.39345(7) 0.0200(3) Uani d 1 . .
C C8 0.70629(14) 0.63505(15) 0.32152(8) 0.0247(3) Uani d 1 . .
H H8 0.670204 0.557712 0.288350 0.030 Uiso calc 1 . .
C C9 0.79374(14) 0.73181(16) 0.29807(8) 0.0266(3) Uani d 1 . .
H H9 0.816202 0.721865 0.248590 0.032 Uiso calc 1 . .
C C10 0.84893(13) 0.84382(14) 0.34690(8) 0.0226(3) Uani d 1 . .
C C11 0.81191(14) 0.86208(14) 0.41785(8) 0.0235(3) Uani d 1 . .
H H11 0.847341 0.940002 0.450770 0.028 Uiso calc 1 . .
C C12 0.72214(13) 0.76474(14) 0.44028(8) 0.0221(3) Uani d 1 . .
H H12 0.695973 0.777571 0.488603 0.027 Uiso calc 1 . .
C C14 1.00316(18) 1.03976(19) 0.36932(11) 0.0411(4) Uani d 1 . .
H H14A 1.062776 1.095104 0.342862 0.062 Uiso calc 1 . .
H H14B 1.055617 0.996804 0.416585 0.062 Uiso calc 1 . .
H H14C 0.934820 1.104289 0.382711 0.062 Uiso calc 1 . .
C C15 0.75500(13) 0.34857(14) 0.48560(7) 0.0212(3) Uani d 1 . .
C C17 0.93178(14) 0.43252(15) 0.58571(8) 0.0245(3) Uani d 1 . .
H H17A 1.003709 0.398723 0.559586 0.029 Uiso calc 1 . .
H H17B 0.916399 0.357827 0.623200 0.029 Uiso calc 1 . .
C C18 0.96974(15) 0.57457(16) 0.62607(8) 0.0301(3) Uani d 1 . .
H H18A 0.982430 0.647720 0.587974 0.045 Uiso calc 1 . .
H H18B 1.053341 0.562775 0.664254 0.045 Uiso calc 1 . .
H H18C 0.898122 0.605610 0.652238 0.045 Uiso calc 1 . .
C C20 0.47715(15) 0.04845(15) 0.33305(8) 0.0267(3) Uani d 1 . .
H H20A 0.525209 -0.041922 0.325556 0.032 Uiso calc 1 . .
H H20B 0.441995 0.090415 0.281357 0.032 Uiso calc 1 . .
C C21 0.36072(16) 0.01227(17) 0.37099(8) 0.0304(3) Uani d 1 . .
H H21A 0.315223 0.102708 0.381347 0.036 Uiso calc 1 . .
H H21B 0.295103 -0.047698 0.335390 0.036 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
O5 0.0270(5) 0.0245(5) 0.0287(5) -0.0031(4) -0.0058(4) 0.0000(4)
O13 0.0292(5) 0.0295(5) 0.0276(5) -0.0053(4) 0.0047(4) 0.0077(4)
O15 0.0321(6) 0.0207(5) 0.0361(6) 0.0034(4) -0.0076(4) -0.0020(4)
O16 0.0247(5) 0.0208(5) 0.0222(5) -0.0009(4) -0.0028(4) 0.0002(4)
O22 0.0470(7) 0.0409(6) 0.0277(6) -0.0162(5) 0.0015(5) 0.0051(5)
N1 0.0201(5) 0.0198(6) 0.0251(6) 0.0000(4) 0.0000(4) 0.0006(4)
N19 0.0243(6) 0.0181(5) 0.0240(6) -0.0011(4) -0.0007(5) 0.0002(4)
C2 0.0211(6) 0.0192(6) 0.0189(6) -0.0005(5) 0.0015(5) -0.0004(5)
C3 0.0228(6) 0.0191(6) 0.0189(6) -0.0016(5) 0.0037(5) 0.0007(5)
C4 0.0219(6) 0.0207(6) 0.0180(6) -0.0015(5) 0.0043(5) 0.0019(5)
C5 0.0224(6) 0.0205(6) 0.0220(6) -0.0010(5) 0.0034(5) 0.0019(5)
C6 0.0244(7) 0.0223(7) 0.0327(7) 0.0031(5) 0.0000(6) 0.0026(6)
C7 0.0202(6) 0.0184(6) 0.0198(6) 0.0018(5) 0.0004(5) 0.0018(5)
C8 0.0293(7) 0.0234(7) 0.0202(6) -0.0025(6) 0.0020(5) -0.0028(5)
C9 0.0305(7) 0.0307(7) 0.0191(6) -0.0009(6) 0.0059(5) 0.0020(5)
C10 0.0217(6) 0.0208(6) 0.0237(6) 0.0010(5) 0.0008(5) 0.0075(5)
C11 0.0259(7) 0.0188(6) 0.0237(6) -0.0016(5) 0.0000(5) -0.0013(5)
C12 0.0247(7) 0.0211(6) 0.0200(6) 0.0006(5) 0.0033(5) -0.0006(5)
C14 0.0409(9) 0.0382(9) 0.0460(9) -0.0194(7) 0.0129(7) -0.0030(7)
C15 0.0235(6) 0.0199(6) 0.0203(6) -0.0035(5) 0.0042(5) 0.0012(5)
C17 0.0222(7) 0.0261(7) 0.0224(6) -0.0003(5) -0.0020(5) 0.0021(5)
C18 0.0309(8) 0.0290(8) 0.0268(7) -0.0033(6) -0.0026(6) -0.0018(6)
C20 0.0316(7) 0.0222(7) 0.0239(7) -0.0022(6) -0.0004(6) -0.0030(5)
C21 0.0356(8) 0.0259(7) 0.0285(7) -0.0056(6) 0.0037(6) -0.0017(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
C10 O13 C14 . . 117.09(11) ?
C15 O16 C17 . . 116.94(10) ?
H22A O22 H22B . . 125(4) ?
C21 O22 H22A . . 105(3) ?
C21 O22 H22B . . 114(3) ?
C5 N1 C2 . . 114.42(11) ?
C5 N1 C6 . . 123.27(11) ?
C6 N1 C2 . . 122.25(11) ?
C4 N19 H19 . . 114.8(12) ?
C4 N19 C20 . . 126.42(12) ?
C20 N19 H19 . . 118.2(12) ?
N1 C2 H2 . . 109.3 ?
N1 C2 C3 . . 101.24(10) ?
N1 C2 C7 . . 112.45(10) ?
C3 C2 H2 . . 109.3 ?
C3 C2 C7 . . 114.87(11) ?
C7 C2 H2 . . 109.3 ?
C4 C3 C2 . . 110.54(11) ?
C4 C3 C15 . . 124.14(12) ?
C15 C3 C2 . . 125.31(11) ?
N19 C4 C3 . . 127.92(13) ?
N19 C4 C5 . . 123.97(12) ?
C3 C4 C5 . . 108.10(11) ?
O5 C5 N1 . . 126.51(13) ?
O5 C5 C4 . . 127.79(12) ?
N1 C5 C4 . . 105.69(11) ?
N1 C6 H6A . . 109.5 ?
N1 C6 H6B . . 109.5 ?
N1 C6 H6C . . 109.5 ?
H6A C6 H6B . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
C8 C7 C2 . . 120.40(12) ?
C12 C7 C2 . . 120.81(11) ?
C12 C7 C8 . . 118.79(12) ?
C7 C8 H8 . . 119.7 ?
C9 C8 C7 . . 120.63(13) ?
C9 C8 H8 . . 119.7 ?
C8 C9 H9 . . 120.0 ?
C8 C9 C10 . . 120.03(12) ?
C10 C9 H9 . . 120.0 ?
O13 C10 C9 . . 115.26(12) ?
O13 C10 C11 . . 124.70(12) ?
C11 C10 C9 . . 120.04(12) ?
C10 C11 H11 . . 120.4 ?
C10 C11 C12 . . 119.25(12) ?
C12 C11 H11 . . 120.4 ?
C7 C12 C11 . . 121.20(12) ?
C7 C12 H12 . . 119.4 ?
C11 C12 H12 . . 119.4 ?
O13 C14 H14A . . 109.5 ?
O13 C14 H14B . . 109.5 ?
O13 C14 H14C . . 109.5 ?
H14A C14 H14B . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
O15 C15 O16 . . 123.23(12) ?
O15 C15 C3 . . 124.58(12) ?
O16 C15 C3 . . 112.19(11) ?
O16 C17 H17A . . 110.6 ?
O16 C17 H17B . . 110.6 ?
O16 C17 C18 . . 105.76(11) ?
H17A C17 H17B . . 108.7 ?
C18 C17 H17A . . 110.6 ?
C18 C17 H17B . . 110.6 ?
C17 C18 H18A . . 109.5 ?
C17 C18 H18B . . 109.5 ?
C17 C18 H18C . . 109.5 ?
H18A C18 H18B . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
N19 C20 H20A . . 108.9 ?
N19 C20 H20B . . 108.9 ?
N19 C20 C21 . . 113.26(12) ?
H20A C20 H20B . . 107.7 ?
C21 C20 H20A . . 108.9 ?
C21 C20 H20B . . 108.9 ?
O22 C21 C20 . . 111.24(13) ?
O22 C21 H21A . . 109.4 ?
O22 C21 H21B . . 109.4 ?
C20 C21 H21A . . 109.4 ?
C20 C21 H21B . . 109.4 ?
H21A C21 H21B . . 108.0 ?
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
O5 C5 . 1.2267(16) ?
O13 C10 . 1.3684(16) ?
O13 C14 . 1.4178(19) ?
O15 C15 . 1.2242(17) ?
O16 C15 . 1.3424(16) ?
O16 C17 . 1.4549(15) ?
O22 H22A . 0.983(5) ?
O22 H22B . 0.983(19) ?
O22 C21 . 1.4236(18) ?
N1 C2 . 1.4636(16) ?
N1 C5 . 1.3502(17) ?
N1 C6 . 1.4512(17) ?
N19 H19 . 0.922(14) ?
N19 C4 . 1.3447(17) ?
N19 C20 . 1.4613(17) ?
C2 H2 . 1.0000 ?
C2 C3 . 1.5124(18) ?
C2 C7 . 1.5180(18) ?
C3 C4 . 1.3659(18) ?
C3 C15 . 1.4423(18) ?
C4 C5 . 1.5109(18) ?
C6 H6A . 0.9800 ?
C6 H6B . 0.9800 ?
C6 H6C . 0.9800 ?
C7 C8 . 1.3955(19) ?
C7 C12 . 1.3833(18) ?
C8 H8 . 0.9500 ?
C8 C9 . 1.382(2) ?
C9 H9 . 0.9500 ?
C9 C10 . 1.392(2) ?
C10 C11 . 1.3879(19) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.3944(19) ?
C12 H12 . 0.9500 ?
C14 H14A . 0.9800 ?
C14 H14B . 0.9800 ?
C14 H14C . 0.9800 ?
C17 H17A . 0.9900 ?
C17 H17B . 0.9900 ?
C17 C18 . 1.507(2) ?
C18 H18A . 0.9800 ?
C18 H18B . 0.9800 ?
C18 H18C . 0.9800 ?
C20 H20A . 0.9900 ?
C20 H20B . 0.9900 ?
C20 C21 . 1.510(2) ?
C21 H21A . 0.9900 ?
C21 H21B . 0.9900 ?
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
N19 H19 O15 . 0.922(14) 2.187(17) 2.8595(15) 129.2(15) yes
O22 H22A O15 3_656 0.983(5) 2.082(18) 3.0131(16) 157(4) yes
O22 H22B O22 3_656 0.983(19) 1.83(2) 2.796(2) 167(4) yes
C6 H6B O22 1_565 0.98 2.57 3.4152(18) 144 yes
C8 H8 O13 2_645 0.95 2.34 3.2556(17) 162 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
O13 C10 C11 C12 . . . . -177.32(12) ?
N1 C2 C3 C4 . . . . 0.97(14) ?
N1 C2 C3 C15 . . . . -178.34(12) ?
N1 C2 C7 C8 . . . . -50.65(16) ?
N1 C2 C7 C12 . . . . 130.23(13) ?
N19 C4 C5 O5 . . . . 2.1(2) ?
N19 C4 C5 N1 . . . . -178.77(12) ?
N19 C20 C21 O22 . . . . -65.47(16) ?
C2 N1 C5 O5 . . . . 179.51(13) ?
C2 N1 C5 C4 . . . . 0.36(15) ?
C2 C3 C4 N19 . . . . 178.21(13) ?
C2 C3 C4 C5 . . . . -0.81(14) ?
C2 C3 C15 O15 . . . . -176.13(13) ?
C2 C3 C15 O16 . . . . 4.74(18) ?
C2 C7 C8 C9 . . . . -177.94(12) ?
C2 C7 C12 C11 . . . . 177.04(12) ?
C3 C2 C7 C8 . . . . 64.43(16) ?
C3 C2 C7 C12 . . . . -114.69(14) ?
C3 C4 C5 O5 . . . . -178.84(13) ?
C3 C4 C5 N1 . . . . 0.30(14) ?
C4 N19 C20 C21 . . . . -74.66(17) ?
C4 C3 C15 O15 . . . . 4.7(2) ?
C4 C3 C15 O16 . . . . -174.48(12) ?
C5 N1 C2 C3 . . . . -0.80(14) ?
C5 N1 C2 C7 . . . . 122.29(12) ?
C6 N1 C2 C3 . . . . -177.89(12) ?
C6 N1 C2 C7 . . . . -54.80(16) ?
C6 N1 C5 O5 . . . . -3.4(2) ?
C6 N1 C5 C4 . . . . 177.42(12) ?
C7 C2 C3 C4 . . . . -120.45(12) ?
C7 C2 C3 C15 . . . . 60.24(17) ?
C7 C8 C9 C10 . . . . 1.2(2) ?
C8 C7 C12 C11 . . . . -2.1(2) ?
C8 C9 C10 O13 . . . . 176.51(12) ?
C8 C9 C10 C11 . . . . -2.7(2) ?
C9 C10 C11 C12 . . . . 1.8(2) ?
C10 C11 C12 C7 . . . . 0.6(2) ?
C12 C7 C8 C9 . . . . 1.2(2) ?
C14 O13 C10 C9 . . . . -177.18(14) ?
C14 O13 C10 C11 . . . . 2.0(2) ?
C15 O16 C17 C18 . . . . 179.91(11) ?
C15 C3 C4 N19 . . . . -2.5(2) ?
C15 C3 C4 C5 . . . . 178.51(12) ?
C17 O16 C15 O15 . . . . 1.01(19) ?
C17 O16 C15 C3 . . . . -179.84(10) ?
C20 N19 C4 C3 . . . . 173.28(13) ?
C20 N19 C4 C5 . . . . -7.8(2) ?