#------------------------------------------------------------------------------
#$Date: 2023-03-14 03:14:51 +0000 (Tue, 14 Mar 2023) $
#$Revision: 281864 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/42/2244231.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_2244231
loop_
_publ_author_name
'Ismail, Ahmad Zaidi'
'Gunasekharan, Mohanapriya'
'Karunakaran, Thiruventhan'
'Mohd Faudzi, Siti Munirah'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of
3-(3-hydroxyphenyl)-1-(1H-pyrrol-2-yl)prop-2-en-1-one hemihydrate
;
_journal_coeditor_code YZ2023
_journal_issue 4
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2056989023001925
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac '2C13 H11 N O2, H2 O'
_chemical_formula_moiety '2(C13 H11 N O2), H2 O'
_chemical_formula_sum 'C26 H24 N2 O5'
_chemical_formula_weight 444.47
_chemical_name_systematic
;
3-(3-Hydroxyphenyl)-1-(1H-pyrrol-2-yl)prop-2-en-1-one hemihydrate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 13
_space_group_name_Hall '-P 2yc'
_space_group_name_H-M_alt 'P 1 2/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 105.3560(10)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 11.90960(10)
_cell_length_b 5.58360(10)
_cell_length_c 16.8121(2)
_cell_measurement_reflns_used 9119
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 76.0860
_cell_measurement_theta_min 3.8270
_cell_volume 1078.07(3)
_computing_cell_refinement
;
CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_publication_material
;
PublCif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0279
_diffrn_reflns_av_unetI/netI 0.0169
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 13888
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 75.232
_diffrn_reflns_theta_min 3.849
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.783
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.676
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.369
_exptl_crystal_description prism
_exptl_crystal_F_000 468
_exptl_crystal_size_max 0.180
_exptl_crystal_size_mid 0.170
_exptl_crystal_size_min 0.130
_refine_diff_density_max 0.303
_refine_diff_density_min -0.188
_refine_ls_extinction_coef 0.0039(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.040
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 163
_refine_ls_number_reflns 2221
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.040
_refine_ls_R_factor_all 0.0364
_refine_ls_R_factor_gt 0.0344
_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^)+(0.0512P)^2^+0.3933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0926
_refine_ls_wR_factor_ref 0.0947
_reflns_number_gt 2067
_reflns_number_total 2221
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2023sup1.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 2/c'
_cod_database_code 2244231
_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 0.872
_shelx_estimated_absorpt_t_max 0.905
_shelx_hkl_file
;
0 0 2 1.33 0.20
0 0 3 -0.02 0.16
0 0 4 1256.27 21.93
0 0 5 0.19 0.28
0 0 6 9.15 0.85
0 0 6 8.47 0.84
0 0 7 0.25 0.35
0 0 7 0.23 0.27
0 0 7 -0.02 0.25
0 0 -8 264.94 4.93
0 0 8 244.30 6.61
0 0 8 255.80 6.67
0 0 9 0.97 0.49
0 0 9 -0.04 0.30
0 0 10 1885.23 34.93
0 0 10 1946.10 34.93
0 0 10 1924.33 34.96
0 0 10 1829.65 35.12
0 0 10 1874.47 35.11
0 0 10 1968.77 34.79
0 0 10 1977.70 35.30
0 0 10 1959.36 34.76
0 0 10 1866.03 35.04
0 0 10 1750.51 34.93
0 0 11 -0.23 0.38
0 0 11 -0.10 0.33
0 0 11 0.74 0.42
0 0 11 0.21 0.46
0 0 -11 0.16 0.24
0 0 11 0.74 0.55
0 0 11 0.06 0.39
0 0 11 0.43 0.48
0 0 11 0.62 0.63
0 0 11 0.22 0.36
0 0 11 0.39 0.44
0 0 11 0.22 0.36
0 0 11 -0.59 0.41
0 0 12 148.98 5.76
0 0 12 155.04 5.89
0 0 12 155.57 5.48
0 0 12 147.98 5.10
0 0 12 156.81 5.65
0 0 12 139.17 5.63
0 0 12 146.91 5.69
0 0 12 151.68 5.73
0 0 12 154.89 5.45
0 0 12 149.42 5.36
0 0 12 145.66 5.51
0 0 12 147.16 5.50
0 0 13 0.29 0.52
0 0 13 0.55 0.60
0 0 13 0.69 0.45
0 0 13 0.68 0.60
0 0 13 -0.30 0.49
0 0 13 -0.21 0.53
0 0 13 -0.17 0.50
0 0 13 -0.20 0.49
0 0 13 0.48 0.52
0 0 13 0.08 0.43
0 0 13 0.27 0.44
0 0 14 27.82 2.53
0 0 14 31.93 2.37
0 0 14 33.24 2.59
0 0 14 28.96 2.12
0 0 14 14.94 1.90
0 0 14 18.43 2.10
0 0 14 27.78 2.33
0 0 14 31.86 2.60
0 0 14 31.88 2.43
0 0 14 20.56 2.05
0 0 14 14.35 1.81
0 0 15 0.14 0.50
0 0 15 -0.24 0.52
0 0 15 0.06 0.48
0 0 15 -0.43 0.58
0 0 15 0.34 0.53
0 0 15 -0.09 0.61
0 0 15 -0.37 0.56
0 0 15 0.38 0.43
0 0 15 -0.48 0.68
0 0 16 99.57 5.02
0 0 16 86.05 3.86
0 0 16 90.27 4.26
0 0 16 92.60 4.59
0 0 16 94.18 4.63
0 0 16 88.24 4.41
0 0 16 92.07 4.24
0 0 16 99.43 4.39
0 0 16 93.97 4.43
0 0 17 0.04 0.35
0 0 17 0.27 0.42
0 0 17 0.35 0.45
0 0 17 0.91 0.60
0 0 17 -0.30 0.52
0 0 17 0.37 0.43
0 0 18 40.26 2.28
0 0 18 41.30 2.53
0 0 18 39.18 2.56
0 0 18 40.83 2.60
0 0 19 0.60 0.36
0 -1 0 61.86 1.71
0 -1 0 60.87 1.54
0 -1 0 59.14 1.57
0 -1 1 680.99 11.65
0 -1 -1 646.68 11.80
0 -1 1 666.85 12.05
0 -1 -1 654.91 11.96
0 1 1 677.06 11.44
0 -1 1 696.02 11.44
0 1 1 667.85 11.43
0 -1 1 696.04 11.41
0 -1 2 2835.49 45.79
0 -1 -2 2772.87 46.07
0 -1 2 2812.49 46.38
0 -1 -2 2849.61 46.24
0 1 2 2838.35 46.06
0 1 2 2779.89 46.05
0 -1 2 2768.30 46.05
0 -1 -3 29.46 0.99
0 1 3 30.25 0.76
0 -1 -3 29.73 1.02
0 -1 3 30.76 1.15
0 -1 3 30.02 1.13
0 1 3 29.30 1.13
0 1 3 30.20 1.15
0 -1 3 33.96 1.20
0 -1 -4 161.32 3.40
0 -1 -4 161.74 3.30
0 -1 4 173.65 3.66
0 -1 4 165.63 3.83
0 1 4 158.63 3.83
0 -1 4 166.19 3.86
0 1 4 158.52 3.82
0 -1 -5 9.94 0.58
0 -1 5 11.39 0.68
0 -1 -5 10.44 0.46
0 -1 5 12.86 0.91
0 -1 5 11.86 0.86
0 1 5 9.13 0.79
0 1 5 9.40 0.79
0 -1 -6 476.16 8.82
0 -1 6 488.31 8.96
0 1 6 479.05 9.88
0 -1 6 486.85 9.81
0 -1 6 492.40 9.90
0 1 6 462.22 9.85
0 1 7 13.48 1.15
0 -1 7 11.77 1.08
0 -1 7 11.79 1.04
0 1 7 10.83 1.03
0 -1 -8 623.49 11.35
0 1 8 619.22 13.07
0 1 8 585.40 12.91
0 -1 8 622.76 12.98
0 -1 9 89.64 3.63
0 -1 9 82.65 3.41
0 1 9 89.69 3.67
0 1 9 87.71 3.58
0 -1 10 3.03 0.70
0 1 10 3.34 0.69
0 1 10 3.55 0.73
0 -1 10 1.96 0.59
0 1 10 3.43 0.74
0 1 10 3.18 0.75
0 -1 10 3.85 0.79
0 -1 10 2.84 0.70
0 -1 -10 2.63 0.62
0 1 10 2.28 0.57
0 -1 10 3.95 0.85
0 1 10 3.24 0.67
0 -1 10 2.89 0.77
0 1 10 3.12 0.76
0 1 -10 3.18 0.54
0 1 10 3.21 0.64
0 -1 10 3.08 0.70
0 -1 10 2.67 0.60
0 1 10 2.12 0.56
0 -1 10 2.53 0.62
0 1 10 3.34 0.65
0 1 10 1.67 0.54
0 1 10 4.60 0.86
0 1 11 44.24 2.66
0 -1 11 41.73 2.61
0 1 11 40.26 2.55
0 -1 11 40.03 2.57
0 1 11 40.54 2.74
0 -1 11 42.32 2.77
0 -1 11 41.62 2.63
0 1 11 44.83 2.79
0 -1 -11 45.30 2.53
0 1 11 41.25 2.45
0 -1 11 41.99 2.74
0 1 11 44.17 2.35
0 1 11 41.65 2.45
0 1 11 44.36 2.75
0 -1 11 36.47 2.52
0 -1 11 42.09 2.72
0 1 11 41.91 2.74
0 -1 11 39.22 2.48
0 1 11 41.61 2.57
0 1 11 38.94 2.67
0 -1 11 44.19 2.68
0 1 11 44.71 2.58
0 -1 11 39.92 2.53
0 1 11 47.58 2.90
0 -1 12 276.16 8.01
0 -1 12 270.96 8.03
0 1 12 275.99 8.02
0 1 12 270.52 8.02
0 -1 12 279.65 8.47
0 1 12 260.87 8.36
0 -1 -12 278.33 7.65
0 1 12 276.24 7.77
0 1 12 279.07 7.76
0 -1 12 268.97 8.32
0 1 12 280.93 8.29
0 -1 12 284.37 8.43
0 -1 12 261.44 8.11
0 1 12 260.61 8.24
0 -1 12 276.63 8.10
0 1 12 289.53 8.21
0 1 12 263.85 8.35
0 -1 12 278.51 7.84
0 1 12 267.05 7.76
0 -1 12 255.69 7.86
0 1 12 279.28 8.37
0 -1 13 37.56 2.64
0 1 13 31.42 2.41
0 -1 13 33.47 2.52
0 1 13 32.72 2.47
0 1 13 34.45 2.76
0 -1 13 34.02 2.73
0 -1 -13 37.59 2.41
0 -1 13 32.34 2.65
0 1 13 36.00 2.47
0 1 13 33.59 2.34
0 1 13 32.94 2.64
0 1 13 32.04 2.56
0 -1 13 32.36 2.57
0 -1 13 32.57 2.60
0 1 13 30.26 2.42
0 1 13 34.45 2.75
0 -1 13 36.92 2.64
0 -1 13 32.85 2.37
0 -1 13 35.48 2.57
0 1 13 36.63 2.53
0 1 13 32.63 2.60
0 -1 14 41.40 3.10
0 1 14 39.90 3.06
0 1 14 41.85 3.00
0 1 14 39.13 2.62
0 -1 14 42.32 3.08
0 1 14 42.75 2.68
0 1 14 41.24 3.02
0 1 14 40.75 2.94
0 -1 14 40.53 2.93
0 -1 14 41.73 3.03
0 1 14 45.31 3.19
0 -1 14 41.09 2.84
0 -1 14 37.29 2.61
0 1 14 40.51 2.86
0 1 14 42.14 2.79
0 -1 14 43.69 2.91
0 1 14 44.05 2.93
0 -1 14 41.46 2.87
0 -1 15 7.28 1.38
0 1 15 4.46 1.09
0 1 15 5.70 1.15
0 1 15 4.21 0.87
0 -1 15 5.61 1.12
0 1 15 5.70 1.21
0 -1 15 6.00 1.17
0 -1 15 7.57 1.33
0 1 15 6.14 1.17
0 -1 15 5.00 0.96
0 -1 15 5.58 1.01
0 1 15 4.74 1.15
0 1 15 4.68 1.08
0 -1 15 3.58 0.87
0 1 15 6.00 1.10
0 1 15 5.64 1.10
0 -1 15 7.56 1.24
0 1 16 1.85 0.72
0 -1 16 2.67 0.86
0 1 16 3.22 0.77
0 -1 16 2.43 0.72
0 1 16 1.90 0.66
0 -1 16 2.32 0.83
0 1 16 1.53 0.74
0 1 16 1.84 0.73
0 -1 16 3.95 0.89
0 1 16 3.83 1.06
0 -1 16 2.23 0.70
0 -1 16 1.62 0.60
0 -1 16 2.01 0.72
0 -1 17 15.22 1.64
0 1 17 13.35 1.30
0 -1 17 14.84 1.65
0 -1 17 16.63 1.75
0 1 17 13.40 1.60
0 1 17 15.82 1.69
0 1 17 14.67 1.71
0 -1 17 14.02 1.45
0 1 17 13.62 1.53
0 -1 17 14.68 1.56
0 1 17 12.85 1.45
0 -1 18 69.10 3.23
0 1 18 73.81 3.51
0 1 18 69.86 3.20
0 1 18 65.47 2.97
0 1 18 68.83 3.35
0 -1 18 66.90 3.29
0 -1 18 74.74 3.24
0 1 19 0.39 0.32
0 1 19 0.92 0.37
0 -2 0 41.71 1.77
0 -2 0 38.01 1.60
0 -2 0 42.07 1.57
0 -2 1 11.16 0.90
0 -2 -1 10.69 0.85
0 -2 1 10.63 0.70
0 -2 -1 10.16 0.77
0 -2 -1 11.52 0.82
0 -2 -2 302.87 6.67
0 -2 2 311.29 6.86
0 -2 -2 313.88 6.49
0 -2 -2 315.41 6.77
0 -2 2 309.61 6.06
0 -2 -3 140.46 3.51
0 -2 3 140.03 3.01
0 -2 -3 137.47 3.89
0 -2 3 145.59 3.92
0 -2 -3 140.35 3.70
0 2 3 133.71 3.02
0 -2 3 136.05 3.01
0 -2 -4 41.23 1.61
0 -2 -4 44.60 2.01
0 -2 4 39.26 1.15
0 -2 4 36.65 1.75
0 2 4 43.69 1.35
0 -2 -4 41.16 1.70
0 2 4 40.71 1.51
0 -2 4 38.83 1.47
0 -2 -5 210.91 4.72
0 -2 5 216.48 5.22
0 2 5 206.03 3.90
0 -2 -5 210.43 4.81
0 2 5 207.34 4.87
0 2 5 216.10 4.97
0 -2 5 211.10 4.78
0 -2 -6 80.23 2.44
0 -2 -6 83.46 3.19
0 -2 6 80.23 2.80
0 -2 -6 83.38 2.44
0 -2 6 79.71 2.66
0 -2 6 81.92 2.80
0 2 6 77.54 2.73
0 2 6 77.54 2.77
0 -2 -7 729.66 13.26
0 -2 -7 683.87 14.68
0 -2 7 718.59 13.89
0 2 7 711.93 14.31
0 2 7 732.05 14.25
0 -2 7 706.94 14.23
0 -2 7 724.92 14.04
0 2 8 5.41 0.84
0 -2 8 2.84 0.57
0 -2 -8 3.70 0.75
0 2 8 5.53 0.91
0 -2 8 3.60 0.82
0 2 8 4.96 0.85
0 -2 8 3.70 0.74
0 2 8 5.09 0.96
0 -2 8 3.96 0.58
0 2 9 0.59 0.54
0 -2 9 -0.09 0.36
0 2 9 0.34 0.39
0 -2 9 -0.05 0.44
0 -2 9 1.54 0.56
0 2 9 0.55 0.44
0 -2 -9 0.60 0.47
0 2 9 0.57 0.41
0 -2 9 0.27 0.39
0 2 9 0.89 0.47
0 2 9 0.17 0.44
0 -2 9 -0.26 0.37
0 -2 9 1.17 0.57
0 2 9 -0.14 0.36
0 2 9 1.25 0.52
0 -2 9 1.21 0.55
0 2 9 0.65 0.50
0 -2 10 4.55 0.88
0 -2 10 4.18 0.83
0 2 10 3.72 0.80
0 2 10 4.21 0.76
0 2 10 4.39 0.87
0 -2 10 4.46 0.84
0 -2 -10 3.37 0.77
0 2 10 4.41 0.88
0 -2 10 4.15 0.86
0 2 10 1.81 0.65
0 -2 10 4.76 0.88
0 2 10 3.52 0.83
0 -2 10 4.89 0.90
0 2 10 4.39 0.84
0 2 10 3.69 0.87
0 -2 10 4.90 0.90
0 2 10 3.19 0.80
0 2 11 250.43 7.34
0 -2 11 250.43 7.24
0 -2 11 260.03 7.39
0 2 11 255.18 7.26
0 -2 11 244.63 7.57
0 2 11 245.07 7.68
0 2 11 256.13 7.51
0 -2 -11 290.21 8.20
0 2 11 263.60 7.66
0 -2 11 242.77 7.99
0 2 11 256.80 7.50
0 -2 11 260.19 7.68
0 2 11 232.59 7.46
0 -2 11 246.06 7.42
0 2 11 242.85 7.87
0 2 11 266.56 7.83
0 -2 11 248.18 7.64
0 2 -11 263.34 6.98
0 2 11 249.48 8.12
0 -2 12 14.82 1.55
0 2 12 14.28 1.49
0 2 12 15.97 1.79
0 -2 12 13.68 1.65
0 2 12 15.50 1.63
0 -2 -12 14.22 1.68
0 2 12 16.65 1.73
0 2 12 17.16 1.64
0 -2 12 13.74 1.73
0 2 12 17.48 1.83
0 -2 12 14.33 1.62
0 2 12 15.53 1.64
0 -2 12 12.96 1.51
0 2 12 16.39 1.73
0 2 12 15.28 1.78
0 -2 12 14.00 1.63
0 2 12 15.45 1.87
0 -2 13 168.35 5.82
0 2 13 171.32 5.81
0 2 13 152.13 6.16
0 -2 13 167.71 6.30
0 -2 -13 165.00 6.12
0 -2 13 168.39 6.61
0 2 13 172.52 5.66
0 2 13 161.23 5.89
0 2 13 160.39 6.09
0 -2 13 165.83 6.01
0 -2 13 167.85 6.13
0 2 13 170.39 6.01
0 2 13 170.56 6.53
0 2 13 167.87 6.21
0 -2 13 157.73 6.00
0 2 13 164.14 6.52
0 -2 14 7.13 1.14
0 2 14 9.83 1.28
0 -2 -14 9.57 1.46
0 -2 14 5.06 1.16
0 2 14 6.16 0.98
0 2 14 9.15 1.34
0 -2 14 8.22 1.25
0 -2 14 6.21 1.08
0 2 14 7.37 1.19
0 2 14 7.12 1.21
0 2 14 6.87 1.28
0 2 14 7.45 1.35
0 -2 14 5.68 1.10
0 2 14 8.65 1.46
0 -2 15 31.97 2.64
0 2 15 38.07 2.55
0 -2 15 30.99 2.40
0 2 15 35.05 2.46
0 2 15 34.76 2.58
0 -2 15 27.39 2.24
0 2 15 34.63 2.75
0 2 15 33.42 2.55
0 -2 15 30.38 2.39
0 2 15 33.14 2.73
0 2 16 0.82 0.49
0 -2 16 2.15 0.83
0 2 16 1.45 0.63
0 -2 16 0.69 0.50
0 -2 16 0.70 0.46
0 2 16 1.15 0.45
0 2 16 1.02 0.51
0 2 16 0.99 0.62
0 -2 16 1.05 0.52
0 2 16 1.23 0.59
0 2 17 9.26 1.21
0 2 17 8.17 1.21
0 -2 17 9.45 1.26
0 2 17 8.14 1.00
0 -2 17 7.86 1.08
0 2 17 9.45 1.26
0 -2 18 10.75 1.11
0 2 18 9.47 1.09
0 2 18 8.95 1.10
0 2 18 9.72 1.11
0 -2 19 1.64 0.38
0 2 19 2.14 0.46
0 2 19 2.49 0.53
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13 1 -3 441.27 10.83
13 -1 -3 454.03 10.82
-13 -1 3 428.12 10.03
-13 1 2 525.25 11.79
-13 1 2 491.25 11.91
-13 -1 2 513.35 11.97
13 1 -2 504.65 11.85
13 -1 -2 521.16 11.86
-13 -1 2 493.95 10.71
-13 1 1 96.52 4.05
-13 -1 1 97.88 4.03
13 1 -1 94.81 3.93
13 -1 -1 96.86 3.92
-13 1 1 100.05 3.86
13 1 0 17.26 1.54
13 -1 0 16.55 1.52
-13 1 0 17.07 1.42
-13 1 0 16.27 1.56
-13 -1 0 18.09 1.61
13 1 0 17.60 1.56
13 -1 0 17.07 1.51
13 1 1 0.34 0.30
13 -1 1 0.57 0.37
-13 1 -1 0.58 0.40
-13 -1 -1 1.52 0.56
-13 1 -1 0.71 0.33
13 1 1 0.26 0.35
13 -1 1 0.19 0.39
-13 1 -2 4.11 0.63
13 1 2 4.43 0.72
13 1 2 3.37 0.67
13 -1 2 3.96 0.69
13 1 2 4.33 0.74
13 -1 2 3.37 0.66
13 1 3 1.08 0.39
13 1 3 2.32 0.53
13 -1 3 1.19 0.38
13 1 3 1.11 0.40
13 -1 3 1.83 0.46
13 1 4 -0.42 0.35
13 1 4 -0.13 0.27
13 -1 4 -0.04 0.28
13 1 4 -0.05 0.23
13 1 4 0.29 0.26
13 -1 4 -0.09 0.24
-13 2 13 17.55 1.09
-13 2 12 7.35 0.81
13 2 -12 7.38 0.71
-13 2 11 94.62 3.28
13 2 -11 92.20 2.96
-13 2 11 92.55 2.89
-13 -2 11 87.15 2.80
-13 2 10 53.15 2.45
13 2 -10 54.49 2.22
-13 -2 10 48.36 2.06
-13 2 10 53.89 2.29
-13 -2 10 51.31 2.17
13 2 -10 45.30 1.98
-13 -2 9 6.70 0.79
-13 2 9 8.26 0.86
-13 2 9 7.49 0.89
13 2 -9 7.53 0.80
-13 -2 9 7.79 0.88
13 2 -9 6.61 0.77
13 -2 -9 7.01 0.82
-13 2 8 -0.36 0.40
13 2 -8 -0.56 0.37
13 -2 -8 -0.25 0.36
-13 -2 8 -0.20 0.36
-13 -2 8 -0.72 0.36
-13 2 8 0.25 0.30
-13 -2 7 33.76 1.95
-13 2 7 34.90 2.11
-13 2 7 34.84 1.86
-13 -2 7 35.78 1.99
13 2 -7 30.56 1.81
13 -2 -7 32.94 1.85
-13 -2 7 33.20 1.87
-13 2 7 32.83 1.82
-13 -2 6 0.25 0.32
-13 2 6 0.39 0.44
13 2 -6 0.20 0.30
13 -2 -6 0.66 0.43
-13 2 6 0.02 0.35
-13 -2 6 0.39 0.36
-13 -2 6 -0.52 0.41
-13 2 6 -0.05 0.34
-13 -2 5 11.42 1.03
-13 2 5 11.12 1.06
-13 -2 5 11.96 1.16
13 2 -5 11.31 1.11
13 -2 -5 10.42 1.06
-13 2 5 12.64 1.31
-13 2 5 10.74 1.21
-13 2 4 5.45 0.86
13 2 -4 5.55 0.79
13 -2 -4 5.23 0.74
-13 2 4 5.70 0.80
-13 -2 4 6.32 0.87
-13 2 4 5.16 0.97
13 2 -3 62.99 2.68
13 -2 -3 66.67 2.72
-13 2 3 62.92 2.62
-13 -2 3 64.99 2.80
-13 2 3 69.06 3.10
13 2 -2 34.66 1.89
13 -2 -2 35.25 1.91
13 2 -2 38.24 1.98
13 -2 -2 37.72 1.94
-13 -2 2 35.21 1.96
-13 2 2 37.52 2.20
13 2 -1 17.79 1.27
13 -2 -1 20.55 1.37
13 2 -1 17.19 1.25
13 -2 -1 17.43 1.26
-13 -2 1 16.05 1.25
-13 2 1 17.15 1.43
13 2 0 184.07 4.80
13 -2 0 198.43 4.97
13 2 0 182.91 4.80
-13 -2 0 181.93 4.90
-13 2 0 204.18 5.43
13 2 1 3.45 0.51
-13 -2 -1 2.55 0.50
-13 2 -1 3.24 0.58
13 2 2 14.64 1.15
-13 2 -2 11.52 0.89
13 2 2 11.78 1.01
13 2 3 69.29 2.41
13 2 3 63.11 2.28
-13 3 9 30.19 1.50
13 3 -8 7.02 0.65
-13 3 8 6.46 0.63
13 3 -7 23.37 1.21
-13 3 7 27.29 1.41
-13 3 6 -0.34 0.29
-13 3 5 14.09 1.10
-13 3 4 1.33 0.38
-13 3 3 20.35 1.34
-13 3 2 20.44 1.31
13 3 -1 11.46 0.92
-13 3 1 10.57 0.89
-13 3 0 0.11 0.21
-14 0 12 23.64 1.29
-14 0 12 21.90 1.27
-14 0 12 23.36 1.31
-14 0 11 0.20 0.24
-14 0 11 0.07 0.29
-14 0 11 0.47 0.34
-14 0 10 11.57 1.07
-14 0 10 10.49 1.02
-14 0 10 11.80 1.07
-14 0 9 -0.01 0.33
-14 0 9 -0.21 0.27
-14 0 9 0.17 0.29
-14 0 8 13.80 1.26
-14 0 8 12.37 1.18
-14 0 8 14.58 1.28
14 0 -8 12.94 1.22
-14 0 7 -0.26 0.31
-14 0 7 -0.38 0.44
14 0 -7 -0.47 0.44
-14 0 7 0.15 0.30
-14 0 7 -0.15 0.35
-14 0 6 18.23 1.46
-14 0 6 18.91 1.50
14 0 -6 17.16 1.45
-14 0 6 16.89 1.50
-14 0 5 -0.45 0.43
14 0 -5 -0.09 0.44
-14 0 5 -0.24 0.39
-14 0 5 0.25 0.35
-14 0 4 148.47 4.53
-14 0 4 149.36 4.72
14 0 -4 151.87 4.80
-14 0 4 148.68 4.88
-14 0 3 0.36 0.28
14 0 -3 0.08 0.34
-14 0 3 0.08 0.30
-14 0 3 -0.37 0.36
14 0 -2 3.36 0.65
-14 0 2 3.16 0.63
-14 0 2 2.42 0.49
14 0 -1 -0.18 0.34
-14 0 1 -0.07 0.27
14 0 -1 0.22 0.27
14 0 0 7.55 0.85
-14 0 0 7.63 0.84
14 0 0 8.30 0.90
14 0 1 0.01 0.22
-14 0 -1 -0.13 0.26
14 0 1 -0.11 0.23
-14 -1 11 0.29 0.23
-14 1 11 -0.18 0.28
-14 1 11 0.53 0.31
-14 1 11 0.24 0.25
14 1 -11 0.26 0.28
14 -1 -11 0.77 0.29
-14 1 11 -0.27 0.21
-14 -1 11 0.42 0.27
-14 -1 10 18.75 1.25
-14 1 10 19.72 1.25
-14 1 10 19.41 1.22
-14 -1 10 19.10 1.29
-14 1 10 19.67 1.28
-14 1 10 19.90 1.25
-14 -1 10 18.61 1.26
14 1 -10 18.97 1.26
14 -1 -10 18.35 1.23
-14 -1 9 46.12 2.11
-14 1 9 44.67 2.05
-14 1 9 42.83 1.96
-14 1 9 44.71 2.13
-14 -1 9 47.95 2.17
-14 1 9 46.20 2.07
-14 -1 9 46.86 2.14
14 1 -9 44.51 2.09
14 -1 -9 41.38 2.00
-14 -1 8 0.02 0.29
-14 1 8 0.01 0.31
-14 1 8 0.67 0.32
-14 -1 8 0.04 0.27
-14 1 8 0.58 0.38
14 1 -8 0.01 0.29
14 -1 -8 -0.07 0.28
-14 1 8 -0.11 0.34
-14 -1 8 0.67 0.37
-14 -1 7 8.71 0.95
-14 1 7 9.73 0.98
-14 1 7 8.91 0.88
-14 -1 7 10.52 1.01
-14 1 7 8.53 0.96
-14 -1 7 8.39 0.94
14 1 -7 8.33 0.93
14 -1 -7 8.46 0.94
-14 1 7 7.35 0.86
-14 -1 6 2.20 0.51
-14 1 6 1.09 0.45
14 1 -6 1.46 0.45
14 -1 -6 0.82 0.32
-14 1 6 1.39 0.45
-14 -1 6 1.68 0.51
-14 -1 6 1.26 0.44
-14 1 6 1.36 0.43
-14 1 5 175.80 4.94
-14 -1 5 166.68 4.98
14 1 -5 170.16 5.00
14 -1 -5 173.98 4.99
-14 1 5 177.29 5.11
-14 -1 5 173.50 4.63
-14 1 4 63.98 2.66
-14 -1 4 60.68 2.66
14 1 -4 64.93 2.73
14 -1 -4 64.68 2.71
-14 1 4 65.14 2.74
-14 -1 4 59.24 2.21
14 1 -3 39.67 2.06
14 -1 -3 44.38 2.14
-14 1 3 42.15 2.05
-14 -1 3 36.78 2.00
-14 1 3 41.42 2.07
14 1 -2 16.44 1.27
14 -1 -2 19.96 1.39
14 1 -2 15.39 1.24
14 -1 -2 18.54 1.31
-14 1 2 15.88 1.20
-14 -1 2 14.89 1.23
-14 1 2 18.07 1.26
14 1 -1 31.71 1.70
14 -1 -1 34.80 1.77
-14 1 1 30.28 1.51
14 1 -1 28.80 1.62
14 -1 -1 32.66 1.71
-14 1 1 27.74 1.54
-14 -1 1 28.50 1.62
14 1 0 12.62 0.96
14 1 0 13.96 1.04
14 -1 0 13.34 1.01
14 1 0 12.09 0.96
14 -1 0 12.90 0.98
-14 1 0 9.64 0.85
-14 -1 0 10.57 0.92
14 -1 1 -0.29 0.25
14 -1 1 -0.21 0.22
-14 -1 -1 -0.49 0.29
-14 2 9 -0.23 0.24
-14 2 8 5.44 0.63
-14 2 8 6.05 0.67
-14 2 7 8.72 0.84
-14 2 6 43.20 1.96
-14 2 5 3.26 0.55
-14 2 4 28.04 1.55
-14 2 3 4.55 0.63
-14 2 2 63.14 2.26
0 0 0 0.00 0.00
TITL exp_2027 in P2/c
REM P2/c (#13 in standard setting)
CELL 1.54184 11.909560 5.583570 16.812115 90.0000 105.3559 90.0000
ZERR 4.00 0.000123 0.000061 0.000160 0.0000 0.0010 0.0000
LATT 1
SYMM -x, y,-z+1/2
SFAC C H N O
UNIT 52.00 44.00 4.00 10.00
REM CrysAlisPro recorded range (K): Min=99.9; max=100.1; aver:100.0
TEMP -173
SIZE 0.13 0.17 0.18
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 76341
_shelx_res_file
;
TITL exp_2027_a.res in P2/c
shelx.res
created by SHELXL-2018/3 at 20:18:00 on 14-Jan-2023
CELL 1.54184 11.9096 5.5836 16.8121 90.000 105.356 90.000
ZERR 2.00 0.0001 0.0001 0.0002 0.000 0.001 0.000
LATT 1
SYMM - X, Y, 1/2 - Z
SFAC C H N O
UNIT 52 48 4 10
MERG 2
EQIV $2 -x+1, -y+1, -z+1
EQIV $3 x-1, -y+1, z-1/2
HTAB O2 O1_$2
HTAB N1 O3
HTAB C13 O1_$2
HTAB O3 O2_$3
FMAP 2 53 53
PLAN 5
SIZE 0.130 0.170 0.180
ACTA
BOND $H
CONF
LIST 4
L.S. 20
TEMP -173.00
WGHT 0.051200 0.393300
EXTI 0.003851
FVAR 0.73128
O1 4 0.279001 0.421893 0.339505 11.00000 0.02509 0.02722 =
0.02275 0.00892 -0.00315 -0.00808
O2 4 0.812843 0.953692 0.595331 11.00000 0.01779 0.02385 =
0.01939 0.00320 -0.00124 -0.00436
O3 4 0.000000 0.052586 0.250000 10.50000 0.02175 0.01926 =
0.02077 0.00000 0.00463 0.00000
N1 3 0.105655 0.455476 0.191882 11.00000 0.01705 0.01990 =
0.01764 0.00101 0.00246 -0.00254
C1 1 0.177377 0.792468 0.154083 11.00000 0.01760 0.01871 =
0.01705 0.00113 0.00445 0.00147
AFIX 43
H1A 2 0.225141 0.928386 0.153517 11.00000 -1.20000
AFIX 0
C2 1 0.076949 0.727796 0.092549 11.00000 0.02136 0.02561 =
0.01670 0.00254 0.00004 0.00244
AFIX 43
H2A 2 0.044033 0.812012 0.042726 11.00000 -1.20000
AFIX 0
C3 1 0.035124 0.518959 0.118094 11.00000 0.01721 0.02773 =
0.01816 -0.00082 -0.00147 -0.00107
AFIX 43
H3 2 -0.032172 0.434067 0.088590 11.00000 -1.20000
AFIX 0
C4 1 0.193819 0.620517 0.215942 11.00000 0.01450 0.01729 =
0.01627 -0.00098 0.00447 -0.00063
C5 1 0.282026 0.592933 0.292912 11.00000 0.01728 0.01889 =
0.01672 0.00130 0.00430 0.00017
C6 1 0.375553 0.773644 0.313813 11.00000 0.01825 0.01847 =
0.01663 0.00193 0.00398 -0.00085
AFIX 43
H6 2 0.376212 0.901776 0.276763 11.00000 -1.20000
AFIX 0
C7 1 0.459372 0.758640 0.384434 11.00000 0.01764 0.01700 =
0.01761 0.00144 0.00505 0.00026
AFIX 43
H7 2 0.455306 0.624717 0.418413 11.00000 -1.20000
AFIX 0
C8 1 0.556715 0.923259 0.415878 11.00000 0.01535 0.01649 =
0.01560 -0.00161 0.00564 0.00107
C9 1 0.569279 1.140196 0.377188 11.00000 0.01900 0.01796 =
0.01501 0.00018 0.00432 0.00173
AFIX 43
H9 2 0.513693 1.186081 0.327786 11.00000 -1.20000
AFIX 0
C10 1 0.663503 1.287521 0.411555 11.00000 0.02319 0.01444 =
0.01911 0.00071 0.00833 -0.00015
AFIX 43
H10 2 0.672229 1.433834 0.384975 11.00000 -1.20000
AFIX 0
C11 1 0.745518 1.224717 0.484326 11.00000 0.01758 0.01763 =
0.01952 -0.00300 0.00547 -0.00385
AFIX 43
H11 2 0.809769 1.326921 0.507080 11.00000 -1.20000
AFIX 0
C12 1 0.732382 1.010964 0.523309 11.00000 0.01501 0.01964 =
0.01470 -0.00138 0.00339 0.00173
C13 1 0.638912 0.861017 0.488988 11.00000 0.01720 0.01473 =
0.01705 0.00083 0.00593 0.00047
AFIX 43
H13 2 0.630823 0.714363 0.515581 11.00000 -1.20000
AFIX 0
H2O 2 0.785566 0.832462 0.620242 11.00000 0.05001
H1N 2 0.094819 0.323892 0.218562 11.00000 0.03361
H3O 2 -0.033501 -0.038749 0.209137 11.00000 0.06186
HKLF 4
REM exp_2027_a.res in P2/c
REM wR2 = 0.0947, GooF = S = 1.040, Restrained GooF = 1.040 for all data
REM R1 = 0.0344 for 2067 Fo > 4sig(Fo) and 0.0364 for all 2221 data
REM 163 parameters refined using 0 restraints
END
WGHT 0.0512 0.3933
REM Highest difference peak 0.303, deepest hole -0.188, 1-sigma level 0.045
Q1 1 0.2279 0.6265 0.2565 11.00000 0.05 0.30
Q2 1 0.3294 0.6881 0.3018 11.00000 0.05 0.28
Q3 1 0.5891 0.9202 0.4599 11.00000 0.05 0.27
Q4 1 0.6879 0.9401 0.5054 11.00000 0.05 0.25
Q5 1 0.5094 0.8587 0.4012 11.00000 0.05 0.23
;
_shelx_res_checksum 73562
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.27900(7) 0.42189(15) 0.33951(5) 0.0268(2) Uani d 1 . .
O O2 0.81284(7) 0.95369(15) 0.59533(5) 0.0215(2) Uani d 1 . .
O O3 0.000000 0.0526(2) 0.250000 0.0208(3) Uani d 1 . .
N N1 0.10566(8) 0.45548(17) 0.19188(5) 0.0186(2) Uani d 1 . .
C C1 0.17738(9) 0.7925(2) 0.15408(6) 0.0178(2) Uani d 1 . .
H H1A 0.225141 0.928386 0.153517 0.021 Uiso calc 1 . .
C C2 0.07695(9) 0.7278(2) 0.09255(6) 0.0222(3) Uani d 1 . .
H H2A 0.044033 0.812012 0.042726 0.027 Uiso calc 1 . .
C C3 0.03512(9) 0.5190(2) 0.11809(6) 0.0222(3) Uani d 1 . .
H H3 -0.032172 0.434067 0.088590 0.027 Uiso calc 1 . .
C C4 0.19382(9) 0.62052(19) 0.21594(6) 0.0159(2) Uani d 1 . .
C C5 0.28203(9) 0.59293(19) 0.29291(6) 0.0177(2) Uani d 1 . .
C C6 0.37555(9) 0.7736(2) 0.31381(6) 0.0179(2) Uani d 1 . .
H H6 0.376212 0.901776 0.276763 0.021 Uiso calc 1 . .
C C7 0.45937(9) 0.75864(19) 0.38443(6) 0.0173(2) Uani d 1 . .
H H7 0.455306 0.624717 0.418413 0.021 Uiso calc 1 . .
C C8 0.55672(9) 0.92326(19) 0.41588(6) 0.0155(2) Uani d 1 . .
C C9 0.56928(9) 1.14020(19) 0.37719(6) 0.0174(2) Uani d 1 . .
H H9 0.513693 1.186081 0.327786 0.021 Uiso calc 1 . .
C C10 0.66350(9) 1.28752(19) 0.41156(6) 0.0184(2) Uani d 1 . .
H H10 0.672229 1.433834 0.384975 0.022 Uiso calc 1 . .
C C11 0.74552(9) 1.22472(19) 0.48433(6) 0.0181(2) Uani d 1 . .
H H11 0.809769 1.326921 0.507080 0.022 Uiso calc 1 . .
C C12 0.73238(9) 1.0110(2) 0.52331(6) 0.0166(2) Uani d 1 . .
C C13 0.63891(9) 0.86102(19) 0.48899(6) 0.0161(2) Uani d 1 . .
H H13 0.630823 0.714363 0.515581 0.019 Uiso calc 1 . .
H H2O 0.7856(15) 0.832(3) 0.6202(11) 0.050(5) Uiso d 1 . .
H H1N 0.0948(13) 0.324(3) 0.2186(9) 0.034(4) Uiso d 1 . .
H H3O -0.0335(16) -0.039(4) 0.2091(11) 0.062(6) Uiso 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
O1 0.0251(4) 0.0272(5) 0.0228(4) -0.0081(3) -0.0032(3) 0.0089(3)
O2 0.0178(4) 0.0239(4) 0.0194(4) -0.0044(3) -0.0012(3) 0.0032(3)
O3 0.0218(5) 0.0193(6) 0.0208(5) 0.000 0.0046(4) 0.000
N1 0.0170(4) 0.0199(5) 0.0176(4) -0.0025(4) 0.0025(3) 0.0010(4)
C1 0.0176(5) 0.0187(5) 0.0171(5) 0.0015(4) 0.0044(4) 0.0011(4)
C2 0.0214(5) 0.0256(6) 0.0167(5) 0.0024(4) 0.0000(4) 0.0025(4)
C3 0.0172(5) 0.0277(6) 0.0182(5) -0.0011(4) -0.0015(4) -0.0008(4)
C4 0.0145(5) 0.0173(5) 0.0163(5) -0.0006(4) 0.0045(4) -0.0010(4)
C5 0.0173(5) 0.0189(5) 0.0167(5) 0.0002(4) 0.0043(4) 0.0013(4)
C6 0.0183(5) 0.0185(5) 0.0166(5) -0.0009(4) 0.0040(4) 0.0019(4)
C7 0.0176(5) 0.0170(5) 0.0176(5) 0.0003(4) 0.0051(4) 0.0014(4)
C8 0.0153(5) 0.0165(5) 0.0156(5) 0.0011(4) 0.0056(4) -0.0016(4)
C9 0.0190(5) 0.0180(5) 0.0150(5) 0.0017(4) 0.0043(4) 0.0002(4)
C10 0.0232(5) 0.0144(5) 0.0191(5) -0.0002(4) 0.0083(4) 0.0007(4)
C11 0.0176(5) 0.0176(5) 0.0195(5) -0.0038(4) 0.0055(4) -0.0030(4)
C12 0.0150(5) 0.0196(5) 0.0147(5) 0.0017(4) 0.0034(4) -0.0014(4)
C13 0.0172(5) 0.0147(5) 0.0170(5) 0.0005(4) 0.0059(4) 0.0008(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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
C12 O2 H2O . . 109.4(11) ?
H3O O3 H3O . 2 108(3) ?
C3 N1 C4 . . 109.61(9) ?
C3 N1 H1N . . 122.9(10) ?
C4 N1 H1N . . 127.4(10) ?
C4 C1 C2 . . 107.27(10) ?
C4 C1 H1A . . 126.4 ?
C2 C1 H1A . . 126.4 ?
C3 C2 C1 . . 107.15(9) ?
C3 C2 H2A . . 126.4 ?
C1 C2 H2A . . 126.4 ?
N1 C3 C2 . . 108.67(10) ?
N1 C3 H3 . . 125.7 ?
C2 C3 H3 . . 125.7 ?
N1 C4 C1 . . 107.30(9) ?
N1 C4 C5 . . 120.68(9) ?
C1 C4 C5 . . 132.01(10) ?
O1 C5 C4 . . 120.80(10) ?
O1 C5 C6 . . 121.48(9) ?
C4 C5 C6 . . 117.73(9) ?
C7 C6 C5 . . 120.54(10) ?
C7 C6 H6 . . 119.7 ?
C5 C6 H6 . . 119.7 ?
C6 C7 C8 . . 127.97(10) ?
C6 C7 H7 . . 116.0 ?
C8 C7 H7 . . 116.0 ?
C13 C8 C9 . . 119.15(9) ?
C13 C8 C7 . . 117.69(9) ?
C9 C8 C7 . . 123.14(9) ?
C10 C9 C8 . . 119.53(9) ?
C10 C9 H9 . . 120.2 ?
C8 C9 H9 . . 120.2 ?
C9 C10 C11 . . 121.19(10) ?
C9 C10 H10 . . 119.4 ?
C11 C10 H10 . . 119.4 ?
C12 C11 C10 . . 119.33(10) ?
C12 C11 H11 . . 120.3 ?
C10 C11 H11 . . 120.3 ?
O2 C12 C11 . . 118.55(9) ?
O2 C12 C13 . . 121.51(10) ?
C11 C12 C13 . . 119.94(9) ?
C12 C13 C8 . . 120.84(10) ?
C12 C13 H13 . . 119.6 ?
C8 C13 H13 . . 119.6 ?
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 C5 . 1.2417(13) ?
O2 C12 . 1.3683(12) ?
O2 H2O . 0.901(19) ?
O3 H3O . 0.864(18) ?
O3 H3O 2 0.864(18) ?
N1 C3 . 1.3484(13) ?
N1 C4 . 1.3749(13) ?
N1 H1N . 0.888(17) ?
C1 C4 . 1.3906(14) ?
C1 C2 . 1.4056(14) ?
C1 H1A . 0.9500 ?
C2 C3 . 1.3804(17) ?
C2 H2A . 0.9500 ?
C3 H3 . 0.9500 ?
C4 C5 . 1.4429(14) ?
C5 C6 . 1.4748(14) ?
C6 C7 . 1.3362(14) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.4642(14) ?
C7 H7 . 0.9500 ?
C8 C13 . 1.3973(14) ?
C8 C9 . 1.4015(15) ?
C9 C10 . 1.3879(15) ?
C9 H9 . 0.9500 ?
C10 C11 . 1.3932(14) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.3902(15) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.3903(15) ?
C13 H13 . 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
O2 H2O O1 3_666 0.901(19) 1.828(19) 2.7257(11) 174.2(16) yes
N1 H1N O3 . 0.888(17) 2.041(17) 2.8722(13) 155.4(14) yes
C13 H13 O1 3_666 0.95 2.51 3.2050(13) 130.4 yes
O3 H3O O2 4_465 0.864(18) 2.320(18) 2.9430(7) 129.2(16) 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
C4 C1 C2 C3 . . . . -0.20(12) ?
C4 N1 C3 C2 . . . . 0.25(13) ?
C1 C2 C3 N1 . . . . -0.03(13) ?
C3 N1 C4 C1 . . . . -0.38(12) ?
C3 N1 C4 C5 . . . . -179.58(9) ?
C2 C1 C4 N1 . . . . 0.35(12) ?
C2 C1 C4 C5 . . . . 179.42(11) ?
N1 C4 C5 O1 . . . . -1.17(16) ?
C1 C4 C5 O1 . . . . 179.86(11) ?
N1 C4 C5 C6 . . . . 178.55(9) ?
C1 C4 C5 C6 . . . . -0.42(17) ?
O1 C5 C6 C7 . . . . -0.66(16) ?
C4 C5 C6 C7 . . . . 179.62(10) ?
C5 C6 C7 C8 . . . . -178.53(9) ?
C6 C7 C8 C13 . . . . -175.38(10) ?
C6 C7 C8 C9 . . . . 6.06(17) ?
C13 C8 C9 C10 . . . . 0.72(14) ?
C7 C8 C9 C10 . . . . 179.26(9) ?
C8 C9 C10 C11 . . . . -0.54(15) ?
C9 C10 C11 C12 . . . . -0.24(16) ?
C10 C11 C12 O2 . . . . -179.10(9) ?
C10 C11 C12 C13 . . . . 0.84(15) ?
O2 C12 C13 C8 . . . . 179.27(9) ?
C11 C12 C13 C8 . . . . -0.67(15) ?
C9 C8 C13 C12 . . . . -0.12(15) ?
C7 C8 C13 C12 . . . . -178.74(9) ?
_cod_database_fobs_code 2244231