#------------------------------------------------------------------------------
#$Date: 2024-12-07 18:07:11 +0100 (Sat, 07 Dec 2024) $
#$Revision: 296764 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/32/2023274.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_2023274
loop_
_publ_author_name
'Książkiewicz, Olga'
_publ_section_title
;
A salt from biologically active compounds pyridine-2,3-dicarboxylic
(quinolinic) acid and cytosine.
;
_journal_coeditor_code WV3015
_journal_issue 'Pt 11'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first 742
_journal_page_last 747
_journal_paper_doi 10.1107/S2053229624009598
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C4 H6 N3 O +, C7 H4 N O4 -'
_chemical_formula_moiety 'C4 H6 N3 O +, C7 H4 N O4 -'
_chemical_formula_sum 'C11 H10 N4 O5'
_chemical_formula_weight 278.23
_chemical_name_systematic
;
6-Amino-2-oxo-2,3-dihydropyrimidin-1-ium 3-carboxypyridine-2-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 92.162(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 3.63740(10)
_cell_length_b 11.3412(4)
_cell_length_c 26.7510(8)
_cell_measurement_reflns_used 6170
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 76.0410
_cell_measurement_theta_min 4.2120
_cell_volume 1102.76(6)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy Dualflex diffractometer with a HyPix detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0446
_diffrn_reflns_av_unetI/netI 0.0264
_diffrn_reflns_limit_h_max 4
_diffrn_reflns_limit_h_min -4
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_number 10377
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 76.498
_diffrn_reflns_theta_min 3.307
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 1.163
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.49806
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2021)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.676
_exptl_crystal_description needle
_exptl_crystal_F_000 576
_exptl_crystal_size_max 0.448
_exptl_crystal_size_mid 0.030
_exptl_crystal_size_min 0.019
_refine_diff_density_max 0.384
_refine_diff_density_min -0.263
_refine_ls_extinction_coef 0.0024(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.137
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 198
_refine_ls_number_reflns 2181
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.137
_refine_ls_R_factor_all 0.0532
_refine_ls_R_factor_gt 0.0499
_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^)+(0.0427P)^2^+1.7012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1251
_refine_ls_wR_factor_ref 0.1268
_reflns_number_gt 2021
_reflns_number_total 2181
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wv3015sup1.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2023274.cif.'
_cod_database_code 2023274
_cod_database_fobs_code 2023274
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 2 0.59 0.39
0 0 -2 0.70 0.41
0 0 -2 0.15 0.31
0 0 -3 0.83 0.46
0 0 3 1.25 0.49
0 0 3 1.45 0.64
0 0 4 61.48 2.68
0 0 -4 61.44 2.73
0 0 4 63.02 2.84
0 0 -5 0.29 0.68
0 0 5 0.10 0.81
0 0 5 1.24 0.99
0 0 -6 291.72 10.82
0 0 6 309.79 11.03
0 0 -7 0.67 0.94
0 0 7 -0.10 1.07
0 0 7 1.30 1.30
0 0 8 1666.77 62.59
0 0 -8 1821.65 62.69
0 0 -9 1.52 1.41
0 0 -9 0.74 1.00
0 0 9 0.42 1.25
0 0 -10 201.73 9.00
0 0 -10 202.61 8.54
0 0 10 202.28 8.67
0 0 -11 0.24 1.71
0 0 11 0.10 1.41
0 0 -12 991.31 36.86
0 0 12 954.66 36.37
0 0 12 974.32 37.86
0 0 13 0.64 2.31
0 0 13 0.52 1.63
0 0 13 0.87 0.76
0 0 -13 -0.76 2.16
0 0 13 0.28 0.69
0 0 14 409.06 15.77
0 0 14 377.19 17.12
0 0 14 353.02 13.65
0 0 14 358.38 13.74
0 0 -14 386.01 16.07
0 0 15 0.27 2.32
0 0 15 -0.17 1.88
0 0 15 -0.05 0.81
0 0 15 0.57 0.85
0 0 -15 -0.58 2.22
0 0 16 87.78 4.21
0 0 -16 102.02 6.58
0 0 16 98.48 7.34
0 0 -16 102.53 7.42
0 0 16 92.83 4.32
0 0 17 0.92 1.03
0 0 17 0.66 1.11
0 0 -17 -0.95 2.62
0 0 17 -0.96 2.55
0 0 -17 -0.64 2.37
0 0 17 1.96 0.99
0 0 18 55.26 3.13
0 0 18 57.73 3.00
0 0 18 51.64 3.14
0 0 18 56.23 3.28
0 0 -18 54.95 5.40
0 0 18 54.69 5.95
0 0 -18 55.02 6.09
0 0 18 48.67 3.05
0 0 19 -0.16 1.09
0 0 19 0.26 1.13
0 0 19 0.09 1.22
0 0 19 -0.84 1.32
0 0 -19 1.16 2.56
0 0 19 -1.90 2.76
0 0 -19 -1.17 2.79
0 0 19 -0.08 1.11
0 0 20 131.95 6.16
0 0 20 128.11 5.88
0 0 20 125.95 6.23
0 0 20 131.24 6.10
0 0 -20 129.53 9.00
0 0 20 136.05 10.07
0 0 20 134.02 6.22
0 0 -20 130.89 10.05
0 0 21 -0.19 1.26
0 0 21 0.23 1.41
0 0 21 0.41 1.46
0 0 21 -0.09 1.28
0 0 -21 3.09 3.21
0 0 21 -0.87 2.57
0 0 -21 4.99 3.46
0 0 21 -0.37 1.37
0 0 22 567.44 22.16
0 0 22 604.56 22.76
0 0 22 606.14 22.46
0 0 -22 595.25 26.83
0 0 22 610.75 28.38
0 0 -22 619.11 28.75
0 0 22 554.43 22.49
0 0 23 0.48 2.83
0 0 -23 -1.56 3.10
0 0 -23 2.03 2.76
0 0 23 -0.68 1.51
0 0 23 -0.34 1.57
0 0 24 484.60 25.57
0 0 -24 473.88 24.39
0 0 24 525.66 20.08
0 0 24 521.75 20.40
0 0 -24 523.62 26.48
0 0 -25 -0.42 3.37
0 0 -25 -1.61 2.98
0 0 25 -0.30 1.61
0 0 25 -0.60 1.78
0 0 26 1337.74 49.30
0 0 26 1324.88 48.88
0 0 27 0.23 1.77
0 0 27 1.43 1.57
0 0 28 28.49 2.55
0 0 29 -0.08 1.39
0 0 30 40.42 2.70
0 0 31 1.05 1.13
0 1 0 2.24 0.56
0 1 -1 261.02 9.93
0 -1 1 274.79 9.91
0 -1 -2 495.82 19.10
0 1 -2 532.87 19.11
0 -1 2 556.28 19.09
0 1 2 503.92 19.06
0 1 -2 537.56 19.41
0 -1 3 385.46 15.18
0 -1 3 393.08 14.61
0 1 -3 412.14 15.13
0 -1 3 407.44 15.23
0 -1 3 430.08 14.87
0 1 3 406.66 14.85
0 -1 -3 415.00 14.92
0 1 -3 422.55 14.92
0 -1 4 1148.00 44.02
0 -1 4 1240.76 44.76
0 1 -4 1224.52 44.53
0 -1 4 1334.07 44.37
0 1 4 1268.75 44.31
0 -1 4 1314.78 44.79
0 1 -4 1250.77 44.38
0 -1 5 0.46 0.71
0 -1 5 1.13 1.37
0 1 -5 0.21 1.09
0 -1 5 0.06 1.22
0 1 5 -0.12 0.93
0 -1 5 0.55 1.02
0 1 -5 1.09 1.20
0 1 -6 1091.04 39.26
0 -1 6 1032.79 38.92
0 -1 6 1122.19 39.95
0 1 -6 1089.29 39.41
0 -1 6 1138.01 39.77
0 1 6 1094.74 39.29
0 1 -6 1085.79 39.35
0 1 -7 602.21 21.18
0 -1 7 535.81 20.82
0 -1 7 586.88 21.96
0 1 -7 568.48 21.25
0 -1 -7 548.74 21.91
0 1 -7 576.68 21.33
0 -1 8 136.55 5.76
0 -1 8 138.96 6.82
0 1 8 121.62 5.68
0 1 -8 139.85 5.90
0 1 -8 133.71 6.03
0 -1 -8 130.92 6.76
0 1 -8 135.98 6.24
0 1 9 3.01 1.03
0 1 -9 2.10 1.02
0 -1 9 0.70 1.19
0 -1 9 2.65 1.86
0 1 -9 2.73 1.33
0 -1 -9 4.63 1.91
0 1 -9 1.63 1.70
0 1 10 145.00 6.60
0 1 -10 150.26 6.27
0 -1 10 128.25 7.28
0 1 10 125.11 5.92
0 -1 10 135.81 6.22
0 1 -10 135.11 6.73
0 -1 -10 158.74 7.72
0 -1 11 3021.28 110.65
0 1 -11 3054.41 109.08
0 -1 11 3022.28 109.16
0 1 11 3086.30 109.55
0 1 -11 2960.08 109.74
0 -1 -11 3140.19 111.00
0 1 -12 652.06 24.65
0 1 12 661.76 25.32
0 -1 12 641.75 24.88
0 -1 12 621.85 26.25
0 1 -12 664.66 25.55
0 -1 -12 669.75 26.67
0 1 13 16.43 1.38
0 1 13 13.06 1.22
0 1 13 17.38 2.62
0 -1 13 14.54 2.99
0 1 -13 16.76 1.87
0 -1 13 13.36 2.20
0 1 -13 15.20 2.74
0 -1 -13 14.13 2.89
0 1 14 14.87 1.37
0 1 14 13.96 1.31
0 1 14 15.43 2.67
0 -1 14 15.90 3.14
0 -1 -14 16.07 3.34
0 1 -14 17.70 3.14
0 -1 -15 83.58 6.55
0 -1 15 72.04 6.01
0 1 15 80.34 5.44
0 1 15 72.68 3.59
0 1 15 70.37 3.48
0 1 -15 76.52 5.53
0 1 16 85.65 4.17
0 1 16 95.32 4.37
0 -1 16 90.82 6.99
0 1 16 101.78 6.44
0 -1 -16 105.74 7.74
0 -1 -16 85.74 3.96
0 1 -16 104.49 6.66
0 1 17 1.54 1.03
0 1 17 1.90 1.08
0 -1 17 1.24 0.99
0 -1 17 1.20 1.16
0 -1 17 1.75 1.08
0 1 17 2.02 2.88
0 -1 17 3.11 2.64
0 -1 -17 1.70 2.72
0 -1 -17 1.38 0.83
0 1 -17 1.21 2.47
0 1 18 52.69 3.15
0 1 18 56.71 3.04
0 -1 18 54.83 3.07
0 -1 18 54.78 3.20
0 -1 18 54.13 3.28
0 1 18 56.16 3.26
0 -1 18 61.86 6.04
0 1 18 57.81 6.28
0 -1 -18 56.81 6.22
0 1 -18 54.10 5.44
0 -1 -18 58.37 2.90
0 1 -19 462.12 21.92
0 -1 -19 496.02 22.60
0 1 19 435.76 17.07
0 -1 19 431.56 16.73
0 1 19 452.39 16.72
0 1 19 429.35 16.96
0 -1 19 438.35 17.14
0 -1 19 430.44 16.93
0 -1 19 472.23 21.75
0 1 19 486.24 22.40
0 1 19 417.82 16.90
0 1 -19 472.17 20.68
0 1 -20 77.44 7.49
0 -1 -20 87.04 8.14
0 1 20 73.02 4.19
0 -1 20 75.06 4.04
0 1 20 80.51 4.03
0 -1 20 76.49 4.16
0 -1 20 76.97 4.35
0 1 20 76.06 4.17
0 1 20 81.23 7.79
0 -1 20 75.89 7.26
0 1 20 81.42 4.37
0 1 -20 77.16 6.95
0 1 20 69.31 4.08
0 1 21 30.29 2.41
0 -1 21 27.89 2.58
0 -1 21 31.93 2.59
0 1 21 27.39 2.47
0 1 21 35.09 5.60
0 -1 21 31.30 4.99
0 1 21 32.36 2.76
0 1 -21 31.18 5.28
0 -1 -21 36.68 5.72
0 -1 -21 28.70 4.75
0 1 -21 22.40 4.67
0 1 22 20.11 2.11
0 1 22 24.51 2.38
0 -1 22 18.99 2.26
0 -1 22 23.29 2.48
0 1 22 18.20 4.48
0 -1 22 17.94 4.36
0 -1 22 24.83 2.44
0 1 22 19.89 2.40
0 -1 -22 21.12 4.75
0 1 -22 17.34 4.57
0 -1 -22 16.11 4.24
0 1 -22 21.04 4.51
0 1 23 182.88 8.07
0 -1 23 194.52 8.42
0 1 23 183.59 8.28
0 -1 23 193.65 8.69
0 1 23 194.92 13.41
0 1 23 180.18 8.52
0 -1 23 186.85 8.47
0 1 -23 195.52 13.53
0 -1 -23 176.05 13.10
0 1 -23 182.63 12.28
0 -1 -23 157.40 11.66
0 -1 24 22.13 2.43
0 -1 24 20.25 2.59
0 1 24 18.98 2.31
0 1 24 17.27 4.52
0 1 24 19.56 2.51
0 -1 24 23.45 2.50
0 -1 -24 20.60 5.10
0 1 -24 20.01 4.94
0 1 -24 15.71 4.65
0 -1 -24 14.50 4.37
0 -1 25 79.67 4.61
0 1 25 86.34 4.60
0 1 25 73.68 4.77
0 -1 25 83.20 4.85
0 1 25 68.19 8.09
0 1 25 88.16 4.99
0 -1 25 80.75 4.79
0 1 -25 77.62 8.59
0 -1 -25 73.76 8.31
0 -1 -25 59.15 7.28
0 1 -25 59.02 7.25
0 -1 26 42.80 3.24
0 1 26 37.03 3.35
0 -1 26 38.99 3.26
0 1 26 45.09 3.55
0 1 26 43.66 3.18
0 -1 27 33.66 2.84
0 -1 27 31.12 2.87
0 1 27 27.47 2.90
0 1 27 29.98 2.98
0 1 27 29.88 2.64
0 1 28 127.02 6.12
0 -1 28 135.69 6.31
0 1 28 142.53 6.65
0 1 28 124.93 6.53
0 -1 28 125.35 6.51
0 -1 29 15.54 1.95
0 1 29 15.08 1.84
0 1 29 14.28 2.18
0 1 29 10.52 2.07
0 -1 29 13.53 2.10
0 -1 30 12.80 1.75
0 1 30 11.29 1.56
0 -1 30 11.39 1.88
0 1 30 8.91 1.77
0 1 31 1.01 1.03
0 -1 31 -0.24 1.22
0 -2 0 2989.42 116.99
0 2 0 3336.51 116.08
0 2 0 3306.14 116.45
0 -2 1 1499.22 58.19
0 -2 -1 1442.60 58.15
0 2 -1 1580.23 57.17
0 2 -1 1467.57 57.69
0 2 -2 107.63 5.08
0 2 2 107.22 4.57
0 2 -2 105.84 4.33
0 2 -2 96.07 4.75
0 2 -3 82.22 4.15
0 2 3 76.07 3.65
0 2 -3 82.19 3.54
0 -2 -3 91.95 3.62
0 2 -3 84.86 4.06
0 2 -4 437.31 15.80
0 2 -4 406.40 16.02
0 2 4 402.27 15.51
0 2 -4 426.48 15.41
0 -2 -4 417.42 15.44
0 -2 4 393.99 16.02
0 2 -5 117.57 5.04
0 2 5 95.34 4.61
0 2 -5 105.52 4.64
0 -2 -5 107.21 4.71
0 -2 5 101.22 5.17
0 2 -5 103.04 5.13
0 2 6 572.15 21.17
0 2 -6 560.61 21.12
0 -2 -6 566.83 21.18
0 -2 6 575.32 21.78
0 2 -6 565.24 21.57
0 2 7 148.62 6.43
0 2 -7 145.08 6.45
0 -2 -7 145.29 6.49
0 -2 7 145.03 6.91
0 2 -7 141.44 6.74
0 -2 8 390.13 16.29
0 2 8 411.00 15.61
0 -2 -8 408.36 15.72
0 2 -8 379.07 15.58
0 -2 8 410.90 16.17
0 2 -8 400.49 15.86
0 2 -9 583.35 22.86
0 2 -9 605.82 22.83
0 -2 -9 617.00 22.91
0 -2 9 593.88 23.56
0 2 -9 590.31 22.54
0 2 9 588.72 22.72
0 2 -10 141.61 6.82
0 2 -10 135.67 6.93
0 -2 -10 139.86 6.98
0 -2 10 144.67 7.66
0 2 -10 151.40 6.57
0 2 -11 331.67 14.08
0 -2 -11 357.79 14.54
0 2 -11 337.49 14.41
0 2 11 325.59 13.78
0 -2 11 354.35 15.28
0 2 -11 374.76 13.90
0 2 -12 197.85 8.85
0 2 -12 200.05 9.37
0 -2 -12 199.16 9.40
0 -2 12 192.74 9.97
0 2 -12 209.83 8.56
0 2 12 177.20 8.33
0 2 13 58.84 2.91
0 2 13 52.64 3.32
0 2 -13 63.49 3.53
0 -2 13 62.83 5.03
0 2 13 52.85 2.70
0 -2 13 51.53 2.62
0 -2 13 55.72 2.89
0 2 -13 60.91 4.57
0 -2 -13 58.85 4.49
0 2 14 518.32 18.69
0 2 14 557.74 21.05
0 -2 14 506.35 21.72
0 2 -14 541.88 19.50
0 2 14 469.96 18.45
0 -2 14 502.23 18.42
0 -2 14 474.14 18.62
0 -2 14 498.53 18.46
0 -2 -14 518.67 20.86
0 -2 -14 486.35 18.35
0 2 -14 510.10 20.87
0 2 15 420.57 15.91
0 2 -15 423.27 18.23
0 -2 -15 419.29 15.57
0 -2 -15 418.18 18.15
0 -2 15 423.00 15.69
0 2 15 476.78 18.60
0 -2 15 430.91 19.14
0 -2 15 394.60 15.83
0 -2 15 424.19 15.71
0 2 15 402.50 15.70
0 2 -16 53.97 5.07
0 -2 -16 53.88 4.91
0 -2 -16 54.62 2.77
0 -2 16 56.50 2.91
0 2 16 57.60 4.98
0 -2 16 44.71 4.93
0 -2 16 51.47 2.83
0 2 16 50.26 2.88
0 2 17 295.69 12.36
0 -2 17 331.29 12.42
0 -2 17 295.82 12.20
0 -2 17 311.63 12.65
0 -2 17 312.11 12.45
0 -2 17 321.10 16.06
0 2 17 359.96 15.75
0 2 17 336.86 12.62
0 -2 17 317.62 12.35
0 2 -17 338.46 15.47
0 -2 -17 319.97 12.17
0 -2 -17 334.77 15.36
0 2 18 204.84 7.57
0 -2 18 171.94 7.52
0 -2 18 171.69 7.91
0 -2 18 172.08 7.70
0 2 -18 200.47 11.01
0 -2 -18 187.74 7.46
0 -2 -18 164.50 10.24
0 2 18 187.16 7.90
0 -2 18 172.83 7.61
0 2 18 169.93 7.65
0 -2 18 192.87 7.77
0 2 19 10.26 1.55
0 -2 19 7.52 1.53
0 -2 19 9.27 1.69
0 -2 -19 5.89 3.12
0 -2 -19 8.51 1.29
0 2 -19 9.76 3.53
0 2 19 7.96 1.70
0 -2 19 10.22 1.57
0 -2 19 9.59 1.48
0 2 20 390.53 15.03
0 -2 20 366.05 15.29
0 -2 20 387.75 15.60
0 -2 -20 391.81 14.94
0 2 -20 413.04 19.31
0 -2 -20 376.52 18.82
0 2 20 406.87 15.61
0 -2 20 402.60 15.43
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3 8 11 3.40 1.01
3 8 11 3.63 1.09
3 8 12 74.39 3.59
3 8 12 69.68 3.39
3 8 13 3.94 0.88
3 8 13 4.21 1.01
3 8 14 1.18 0.70
3 8 15 8.17 0.81
3 -9 -15 10.15 1.14
3 -9 -14 27.00 1.88
3 -9 -11 22.57 2.11
3 -9 -10 3.22 1.53
3 -9 -9 0.44 0.93
3 -9 -9 1.55 1.54
3 -9 -8 4.23 1.09
-3 -9 8 3.04 0.80
3 -9 -8 3.29 1.65
3 -9 -7 28.86 1.97
-3 -9 7 30.32 1.90
3 -9 -7 29.12 2.57
-3 -9 6 2.95 0.89
3 -9 -6 4.95 1.16
3 -9 -6 2.11 1.66
3 -9 -5 4.05 1.16
3 -9 -5 1.12 1.58
3 -9 -4 1.36 1.27
3 -9 -4 2.10 1.13
3 -9 -4 -0.66 1.57
3 -9 -3 8.10 1.59
3 -9 -3 10.38 1.41
3 -9 -3 5.32 1.66
3 -9 -2 53.95 3.18
3 -9 -1 16.28 2.22
3 -9 0 99.04 4.86
3 -9 1 20.37 1.81
3 -9 1 11.51 2.37
3 9 2 2.99 0.98
3 -9 2 4.64 1.74
3 -9 2 5.04 1.29
3 9 3 3.04 0.99
3 -9 3 4.60 1.69
3 -9 3 3.09 1.23
3 9 4 2.88 1.01
3 -9 4 1.50 1.62
3 -9 4 3.43 1.20
3 9 5 14.30 1.44
3 -9 5 15.52 2.02
3 -9 5 13.23 1.53
3 9 6 4.13 1.08
3 -9 6 4.37 1.68
3 -9 6 3.14 1.11
3 -9 7 1.58 1.56
3 9 7 0.94 0.94
3 -9 8 1.37 1.48
3 9 8 0.25 0.89
3 -9 9 8.92 1.62
3 9 9 5.64 1.04
3 9 11 27.25 1.46
3 -10 -9 3.76 0.97
3 -10 -8 24.22 1.70
3 -10 -7 4.50 1.07
3 -10 -4 13.42 1.31
3 -10 -3 28.11 1.80
3 -10 -3 22.86 1.65
3 -10 -2 17.47 1.61
3 -10 -1 39.30 2.34
3 -10 0 30.37 2.19
3 -10 1 263.76 9.92
3 -10 1 252.54 10.03
3 -10 2 21.83 2.05
3 -10 3 16.11 1.63
3 -10 4 3.97 1.28
3 -10 5 3.14 1.14
3 -10 6 2.23 1.07
3 -10 7 2.58 1.02
4 0 -14 19.02 1.41
4 0 -13 0.20 0.95
4 0 -12 1.88 1.01
4 0 -11 -0.79 1.12
-4 0 11 -0.03 0.49
-4 0 10 10.25 0.94
-4 0 9 0.31 0.58
-4 0 8 10.53 1.05
-4 0 7 -0.67 0.71
4 0 -7 -0.45 1.33
-4 0 6 27.53 1.90
4 0 -6 39.05 2.45
-4 0 5 3.59 0.94
4 0 -5 3.36 1.46
4 0 -4 291.89 10.33
-4 0 4 234.86 10.01
-4 0 3 29.81 1.75
4 0 -3 8.12 1.67
4 0 -2 10.35 1.52
4 0 -1 1.16 1.20
4 0 0 10.34 1.38
4 0 1 0.86 1.22
4 0 2 53.89 2.92
4 0 2 51.91 3.22
4 0 3 5.56 1.37
4 0 3 2.21 1.26
4 0 4 212.48 8.55
4 0 4 224.45 9.06
4 0 5 7.57 1.33
4 0 6 6.79 1.24
4 0 7 1.51 1.05
4 0 8 185.06 7.28
4 0 8 185.37 7.72
4 0 9 1.96 0.98
4 0 9 1.77 1.07
4 0 10 69.90 3.21
4 0 10 74.64 3.59
4 0 11 1.57 0.83
4 0 11 1.12 0.95
4 0 12 3.37 0.79
4 1 -14 1.22 0.85
4 -1 -14 1.27 0.78
4 1 -13 6.21 1.12
4 -1 -13 6.12 1.03
-4 -1 12 1.53 0.56
4 1 -12 1.32 1.01
4 -1 -12 2.09 0.97
4 -1 -11 27.42 1.80
4 1 -11 29.85 1.94
-4 -1 10 4.88 0.81
4 -1 -10 8.33 1.29
-4 -1 9 1.49 0.70
-4 -1 8 17.80 1.46
4 1 -8 24.80 1.96
4 -1 -7 39.48 2.45
4 1 -7 43.16 2.59
4 -1 -6 60.27 2.98
4 1 -6 53.73 3.00
4 1 -5 3.10 1.45
4 -1 -5 4.54 1.36
-4 -1 5 0.89 0.95
4 1 -4 8.23 1.56
4 -1 -4 7.90 1.46
-4 -1 4 4.25 1.12
4 -1 -3 48.58 2.77
4 1 -3 48.84 2.86
4 1 -2 1.12 1.24
4 -1 -2 1.46 1.20
4 1 -1 1.82 1.25
4 -1 -1 1.58 1.16
4 1 0 2.49 1.25
4 -1 0 0.93 1.03
4 1 1 11.71 1.66
4 1 2 34.73 2.41
4 1 2 36.89 2.57
4 1 3 4.37 1.40
4 1 3 1.19 1.19
4 1 4 4.80 1.33
4 1 4 5.40 1.37
4 1 5 10.45 1.48
4 1 5 11.56 1.62
4 1 6 1.42 1.18
4 1 6 0.71 1.11
4 -1 6 0.07 1.08
4 1 7 -0.31 1.05
4 -1 7 0.78 1.09
4 1 8 -0.21 1.04
4 -1 8 0.98 1.05
4 1 9 2.18 1.03
4 1 10 0.85 0.93
4 1 10 -0.23 0.93
4 1 11 92.79 3.92
4 1 11 89.96 4.18
4 1 12 1.26 0.81
4 1 13 11.14 1.06
4 1 14 35.81 1.77
4 -2 -13 4.37 0.91
-4 -2 13 4.88 0.67
4 2 -12 7.32 1.17
4 -2 -12 7.34 1.03
-4 -2 12 6.48 0.79
-4 -2 11 4.04 0.75
4 -2 -11 6.52 1.09
-4 -2 10 9.89 1.03
4 -2 -10 15.81 1.40
-4 -2 9 1.00 0.71
4 2 -8 -0.32 1.23
-4 -2 8 0.65 0.74
4 2 -7 5.71 1.39
-4 -2 7 3.68 0.92
4 2 -6 8.21 1.52
4 -2 -6 8.14 1.31
-4 -2 6 6.80 1.13
4 2 -5 6.82 1.46
4 -2 -5 7.62 1.30
-4 -2 5 3.82 1.07
4 2 -4 7.55 1.49
4 -2 -4 9.06 1.43
4 -2 -3 58.41 3.05
4 2 -3 59.93 3.17
4 2 -2 3.20 1.29
4 -2 -2 5.66 1.23
4 -2 -1 1.49 1.05
4 2 -1 1.26 1.20
4 -2 0 8.48 1.21
4 2 0 6.50 1.39
4 2 1 17.16 1.87
4 -2 1 18.71 1.51
4 2 2 9.59 1.59
4 2 2 8.52 1.48
4 2 3 18.54 1.84
4 2 3 17.17 1.81
4 2 4 49.98 2.84
4 2 4 46.49 2.91
4 2 5 3.37 1.30
4 2 5 2.21 1.16
4 2 6 10.00 1.45
4 2 6 9.97 1.47
4 2 7 43.02 2.42
4 2 7 40.30 2.61
4 2 8 15.12 1.51
4 2 8 14.63 1.60
4 2 9 1.99 1.04
4 2 9 2.04 1.03
4 2 10 7.08 1.13
4 2 11 16.13 1.32
4 2 12 11.12 1.11
4 2 13 -0.54 0.70
4 2 14 5.02 0.74
4 3 -13 0.21 0.81
-4 -3 12 13.31 1.02
4 -3 -12 15.91 1.20
-4 -3 11 1.56 0.57
4 -3 -11 3.75 0.90
-4 -3 10 68.78 3.25
4 -3 -10 83.36 3.42
-4 -3 9 14.54 1.23
4 -3 -9 19.73 1.49
4 3 -9 18.14 1.61
-4 -3 8 99.40 4.50
4 3 -8 117.63 4.79
-4 -3 7 20.16 1.56
4 3 -7 23.45 1.87
-4 -3 6 203.19 8.42
4 -3 -6 221.29 8.37
4 3 -6 214.44 8.50
-4 -3 5 23.88 1.89
4 3 -5 28.04 2.10
-4 -3 4 7.75 1.21
4 3 -4 8.09 1.43
4 3 -3 8.21 1.39
4 -3 -3 7.68 1.20
4 -3 -2 20.03 1.66
4 -3 -1 108.72 4.61
4 3 0 35.38 2.39
4 -3 0 40.89 2.18
4 3 1 10.99 1.49
4 -3 1 10.71 1.17
4 3 2 12.96 1.54
4 3 3 43.82 2.66
4 3 4 17.15 1.72
4 3 5 2.64 1.07
4 3 6 2.59 1.08
4 3 7 1.52 0.96
4 3 8 29.02 2.06
4 3 9 0.74 0.91
4 3 10 0.10 0.80
-4 -4 11 0.51 0.44
-4 -4 10 1.12 0.53
4 4 -10 0.70 0.91
4 -4 -10 1.91 0.77
-4 -4 9 115.95 4.83
4 -4 -9 128.26 4.90
4 4 -9 116.91 5.01
-4 -4 8 33.59 1.84
4 4 -8 34.18 2.07
-4 -4 7 24.43 1.56
4 4 -7 24.62 1.80
4 4 -6 13.18 1.44
-4 -4 6 13.18 1.21
4 4 -5 18.52 1.66
-4 -4 5 18.00 1.46
4 4 -4 76.29 3.73
-4 -4 4 75.11 3.70
4 -4 -3 91.40 3.79
-4 -4 3 80.94 3.90
4 -4 -2 45.40 2.11
-4 -4 2 25.70 1.96
4 -4 -1 151.70 6.00
4 -4 0 64.27 2.77
4 4 0 50.27 2.90
4 4 1 67.47 3.14
4 -4 1 58.52 2.69
4 4 2 20.83 1.68
4 4 2 9.78 1.34
4 4 3 21.59 1.76
4 4 3 20.08 1.66
4 4 4 2.69 1.15
4 4 4 1.32 0.91
4 4 5 4.12 1.12
4 4 5 2.83 0.97
4 4 6 6.55 1.15
4 4 6 3.89 0.99
4 4 7 35.05 1.96
4 4 7 29.25 1.98
4 4 8 15.84 1.31
4 4 8 12.79 1.29
4 4 9 11.98 1.14
4 4 10 0.36 0.73
4 4 11 0.12 0.62
4 4 12 1.64 0.55
4 -5 -8 12.65 1.05
4 -5 -5 26.08 1.60
4 -5 -4 7.42 0.99
4 -5 -3 27.83 1.66
4 -5 -2 61.23 2.79
4 -5 -1 41.94 2.12
4 5 0 35.27 2.07
4 -5 0 33.46 1.80
-4 -5 0 33.18 1.90
4 5 1 8.64 1.24
4 5 2 19.89 1.57
4 5 3 74.62 3.36
4 5 4 15.29 1.36
4 5 5 246.83 9.34
4 5 6 62.18 2.83
4 5 7 7.21 0.90
4 5 7 6.65 0.92
4 5 8 16.72 1.11
4 5 8 14.07 1.11
4 5 9 0.57 0.58
4 6 -3 1.58 0.81
4 6 -2 1.67 0.82
4 6 -1 3.42 0.89
4 6 0 51.26 2.39
4 6 1 144.81 5.64
4 6 2 36.31 1.83
4 6 3 198.62 7.47
4 6 4 18.30 1.17
4 6 5 8.35 0.80
4 6 6 4.36 0.64
0 0 0 0.00 0.00
TITL exp_602_auto in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 1.54184 3.637398 11.341151 26.750951 90.0000 92.1622 90.0000
ZERR 3.00 0.000126 0.000357 0.000774 0.0000 0.0029 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N O
UNIT 30.00 30.00 15.00 15.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 71063
_shelx_res_file
;
TITL exp_602_auto_a.res in P2(1)/n
exp_602_auto.res
created by SHELXL-2018/3 at 14:18:18 on 21-Mar-2024
CELL 1.54184 3.6374 11.3412 26.751 90 92.162 90
ZERR 4 0.0001 0.0004 0.0008 0 0.003 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 44 40 16 20
L.S. 10
PLAN 2
TEMP -173
CONF
HTAB
BOND $H
LIST 4
fmap 2
acta
MORE -1
MERG 2
REM
REM
REM
WGHT 0.042700 1.701200
EXTI 0.002357
FVAR 0.66221
O3A 4 0.491904 0.790639 0.458629 11.00000 0.03565 0.02301 =
0.01323 0.00145 0.00484 0.00386
O2A 4 0.609367 0.600792 0.658198 11.00000 0.03363 0.02154 =
0.01496 0.00277 0.00257 0.00380
O2B 4 0.781009 0.559931 0.581690 11.00000 0.03411 0.01792 =
0.01602 0.00098 0.00440 0.00424
O1 4 0.778164 0.456099 0.768579 11.00000 0.03061 0.02244 =
0.01680 -0.00060 0.00604 0.00481
O3B 4 0.704581 0.632421 0.496956 11.00000 0.03714 0.01988 =
0.01387 0.00046 0.00381 0.00611
AFIX 83
H3B 2 0.724532 0.605880 0.526248 11.00000 -1.50000
AFIX 0
N1 3 0.961528 0.399744 0.691875 11.00000 0.02463 0.01387 =
0.01443 0.00045 0.00244 0.00179
N4 3 0.337068 0.804714 0.634570 11.00000 0.02607 0.01755 =
0.01587 -0.00146 0.00260 -0.00163
N2 3 1.059128 0.277085 0.760822 11.00000 0.02913 0.01883 =
0.01566 0.00291 0.00461 0.00170
N3 3 1.145373 0.348966 0.613511 11.00000 0.03100 0.01928 =
0.01506 -0.00154 0.00348 0.00325
C5 1 0.268020 0.900169 0.540650 11.00000 0.01964 0.01810 =
0.01665 0.00122 0.00019 -0.00249
AFIX 43
H5 2 0.244847 0.933757 0.508151 11.00000 -1.20000
AFIX 0
C1 1 1.122821 0.322235 0.660604 11.00000 0.02142 0.01651 =
0.01676 -0.00267 0.00149 -0.00226
C9 1 0.423954 0.788063 0.546521 11.00000 0.01987 0.01762 =
0.01677 -0.00063 0.00251 -0.00380
C6 1 0.147416 0.962899 0.580902 11.00000 0.02038 0.01627 =
0.02300 -0.00060 0.00170 -0.00112
AFIX 43
H6 2 0.041579 1.039010 0.576732 11.00000 -1.20000
AFIX 0
C11 1 0.544652 0.734293 0.497459 11.00000 0.01977 0.01822 =
0.01570 -0.00094 0.00216 -0.00187
C2 1 0.924349 0.382203 0.742688 11.00000 0.02245 0.01783 =
0.01714 0.00046 0.00260 -0.00124
C10 1 0.624659 0.625125 0.613431 11.00000 0.02180 0.01724 =
0.01707 -0.00136 0.00133 -0.00315
C8 1 0.455558 0.742692 0.595698 11.00000 0.01998 0.01665 =
0.01498 -0.00202 0.00207 -0.00323
C7 1 0.185711 0.911239 0.627639 11.00000 0.02407 0.01863 =
0.02022 -0.00403 0.00533 -0.00217
AFIX 43
H7 2 0.101541 0.952883 0.655820 11.00000 -1.20000
AFIX 0
C4 1 1.260344 0.215067 0.681804 11.00000 0.02337 0.01483 =
0.02339 -0.00234 0.00330 0.00153
AFIX 43
H4 2 1.375181 0.157975 0.661612 11.00000 -1.20000
AFIX 0
C3 1 1.223978 0.196295 0.731301 11.00000 0.02558 0.01555 =
0.02387 0.00195 0.00095 0.00072
AFIX 43
H3 2 1.315415 0.125175 0.745830 11.00000 -1.20000
AFIX 0
H2 2 1.057998 0.268223 0.796040 11.00000 0.03014
H3A 2 1.251531 0.303008 0.592314 11.00000 0.02787
H1 2 0.861230 0.466108 0.679239 11.00000 0.03448
H3C 2 1.036012 0.413837 0.602191 11.00000 0.03448
HKLF 4
REM exp_602_auto_a.res in P2(1)/n
REM wR2 = 0.1268, GooF = S = 1.137, Restrained GooF = 1.137 for all data
REM R1 = 0.0499 for 2021 Fo > 4sig(Fo) and 0.0532 for all 2181 data
REM 198 parameters refined using 0 restraints
END
WGHT 0.0427 1.7012
REM Instructions for potential hydrogen bonds
HTAB O3B O2B
EQIV $1 -x+1/2, y+1/2, -z+3/2
HTAB C7 O1_$1
EQIV $2 -x+5/2, y-1/2, -z+3/2
HTAB C3 O1_$2
EQIV $3 -x+3/2, y-1/2, -z+3/2
HTAB N2 O2A_$3
HTAB N2 N4_$3
EQIV $4 -x+2, -y+1, -z+1
HTAB N3 O3A_$4
HTAB N3 O3B_$4
HTAB N1 O2A
HTAB N3 O2B
REM Highest difference peak 0.384, deepest hole -0.263, 1-sigma level 0.065
Q1 1 0.7863 0.5768 0.5477 11.00000 0.05 0.38
Q2 1 0.3676 0.7381 0.5653 11.00000 0.05 0.33
;
_shelx_res_checksum 38959
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 O3A 0.4919(5) 0.79064(15) 0.45863(6) 0.0239(4) Uani d 1 . .
O O2A 0.6094(5) 0.60079(14) 0.65820(6) 0.0233(4) Uani d 1 . .
O O2B 0.7810(5) 0.55993(14) 0.58169(6) 0.0226(4) Uani d 1 . .
O O1 0.7782(5) 0.45610(14) 0.76858(6) 0.0232(4) Uani d 1 . .
O O3B 0.7046(5) 0.63242(14) 0.49696(6) 0.0236(4) Uani d 1 . .
H H3B 0.724532 0.605880 0.526248 0.035 Uiso calc 1 . .
N N1 0.9615(5) 0.39974(17) 0.69187(7) 0.0176(4) Uani d 1 . .
N N4 0.3371(5) 0.80471(17) 0.63457(7) 0.0198(4) Uani d 1 . .
N N2 1.0591(6) 0.27708(17) 0.76082(7) 0.0211(4) Uani d 1 . .
N N3 1.1454(6) 0.34897(19) 0.61351(7) 0.0217(4) Uani d 1 . .
C C5 0.2680(6) 0.9002(2) 0.54065(8) 0.0181(5) Uani d 1 . .
H H5 0.244847 0.933757 0.508151 0.022 Uiso calc 1 . .
C C1 1.1228(6) 0.32223(19) 0.66060(8) 0.0182(5) Uani d 1 . .
C C9 0.4240(6) 0.78806(19) 0.54652(8) 0.0180(5) Uani d 1 . .
C C6 0.1474(6) 0.9629(2) 0.58090(8) 0.0199(5) Uani d 1 . .
H H6 0.041579 1.039010 0.576732 0.024 Uiso calc 1 . .
C C11 0.5447(6) 0.7343(2) 0.49746(8) 0.0179(5) Uani d 1 . .
C C2 0.9243(6) 0.3822(2) 0.74269(8) 0.0191(5) Uani d 1 . .
C C10 0.6247(6) 0.6251(2) 0.61343(8) 0.0187(5) Uani d 1 . .
C C8 0.4556(6) 0.7427(2) 0.59570(8) 0.0172(5) Uani d 1 . .
C C7 0.1857(6) 0.9112(2) 0.62764(8) 0.0209(5) Uani d 1 . .
H H7 0.101541 0.952883 0.655820 0.025 Uiso calc 1 . .
C C4 1.2603(6) 0.21507(19) 0.68180(9) 0.0205(5) Uani d 1 . .
H H4 1.375181 0.157975 0.661612 0.025 Uiso calc 1 . .
C C3 1.2240(7) 0.1963(2) 0.73130(9) 0.0217(5) Uani d 1 . .
H H3 1.315415 0.125175 0.745830 0.026 Uiso calc 1 . .
H H2 1.058(8) 0.268(3) 0.7960(12) 0.030(8) Uiso d 1 . .
H H3A 1.252(8) 0.303(3) 0.5923(11) 0.028(8) Uiso d 1 . .
H H1 0.861(9) 0.466(3) 0.6792(11) 0.034(8) Uiso d 1 . .
H H3C 1.036(9) 0.414(3) 0.6022(11) 0.034(8) 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
O3A 0.0356(10) 0.0230(9) 0.0132(8) 0.0039(7) 0.0048(7) 0.0014(6)
O2A 0.0336(9) 0.0215(8) 0.0150(8) 0.0038(7) 0.0026(7) 0.0028(6)
O2B 0.0341(9) 0.0179(8) 0.0160(8) 0.0042(7) 0.0044(7) 0.0010(6)
O1 0.0306(9) 0.0224(8) 0.0168(8) 0.0048(7) 0.0060(7) -0.0006(6)
O3B 0.0371(10) 0.0199(8) 0.0139(8) 0.0061(7) 0.0038(7) 0.0005(6)
N1 0.0246(10) 0.0139(9) 0.0144(9) 0.0018(8) 0.0024(7) 0.0004(7)
N4 0.0261(10) 0.0176(9) 0.0159(9) -0.0016(8) 0.0026(8) -0.0015(7)
N2 0.0291(11) 0.0188(10) 0.0157(10) 0.0017(8) 0.0046(8) 0.0029(7)
N3 0.0310(11) 0.0193(10) 0.0151(10) 0.0033(9) 0.0035(8) -0.0015(8)
C5 0.0196(11) 0.0181(11) 0.0167(11) -0.0025(9) 0.0002(8) 0.0012(8)
C1 0.0214(11) 0.0165(11) 0.0168(11) -0.0023(9) 0.0015(8) -0.0027(8)
C9 0.0199(11) 0.0176(11) 0.0168(11) -0.0038(9) 0.0025(8) -0.0006(8)
C6 0.0204(11) 0.0163(11) 0.0230(11) -0.0011(9) 0.0017(9) -0.0006(9)
C11 0.0198(11) 0.0182(11) 0.0157(10) -0.0019(9) 0.0022(8) -0.0009(8)
C2 0.0224(11) 0.0178(11) 0.0171(11) -0.0012(9) 0.0026(9) 0.0005(8)
C10 0.0218(11) 0.0172(11) 0.0171(11) -0.0031(9) 0.0013(8) -0.0014(8)
C8 0.0200(11) 0.0167(11) 0.0150(10) -0.0032(9) 0.0021(8) -0.0020(8)
C7 0.0241(11) 0.0186(11) 0.0202(11) -0.0022(9) 0.0053(9) -0.0040(9)
C4 0.0234(11) 0.0148(10) 0.0234(12) 0.0015(9) 0.0033(9) -0.0023(9)
C3 0.0256(12) 0.0156(11) 0.0239(12) 0.0007(9) 0.0009(9) 0.0019(9)
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
C11 O3B H3B . . 109.5 ?
C1 N1 C2 . . 124.8(2) ?
C1 N1 H1 . . 119.3(19) ?
C2 N1 H1 . . 115.9(19) ?
C7 N4 C8 . . 120.61(19) ?
C2 N2 H2 . . 115.4(18) ?
C3 N2 C2 . . 122.6(2) ?
C3 N2 H2 . . 121.5(18) ?
C1 N3 H3A . . 122(2) ?
C1 N3 H3C . . 119(2) ?
H3A N3 H3C . . 119(3) ?
C9 C5 H5 . . 119.3 ?
C6 C5 H5 . . 119.3 ?
C6 C5 C9 . . 121.5(2) ?
N1 C1 C4 . . 117.3(2) ?
N3 C1 N1 . . 119.3(2) ?
N3 C1 C4 . . 123.4(2) ?
C5 C9 C11 . . 113.27(19) ?
C5 C9 C8 . . 117.0(2) ?
C8 C9 C11 . . 129.7(2) ?
C5 C6 H6 . . 121.2 ?
C5 C6 C7 . . 117.7(2) ?
C7 C6 H6 . . 121.2 ?
O3A C11 O3B . . 120.8(2) ?
O3A C11 C9 . . 118.6(2) ?
O3B C11 C9 . . 120.64(19) ?
O1 C2 N1 . . 121.2(2) ?
O1 C2 N2 . . 123.6(2) ?
N2 C2 N1 . . 115.17(19) ?
O2A C10 O2B . . 123.7(2) ?
O2A C10 C8 . . 117.54(19) ?
O2B C10 C8 . . 118.75(19) ?
N4 C8 C9 . . 120.9(2) ?
N4 C8 C10 . . 110.66(18) ?
C9 C8 C10 . . 128.40(19) ?
N4 C7 C6 . . 122.3(2) ?
N4 C7 H7 . . 118.8 ?
C6 C7 H7 . . 118.8 ?
C1 C4 H4 . . 120.7 ?
C3 C4 C1 . . 118.6(2) ?
C3 C4 H4 . . 120.7 ?
N2 C3 H3 . . 119.2 ?
C4 C3 N2 . . 121.5(2) ?
C4 C3 H3 . . 119.2 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O3A C11 . 1.228(3) ?
O2A C10 . 1.232(3) ?
O2B C10 . 1.276(3) ?
O1 C2 . 1.222(3) ?
O3B H3B . 0.8400 ?
O3B C11 . 1.294(3) ?
N1 C1 . 1.362(3) ?
N1 C2 . 1.385(3) ?
N1 H1 . 0.90(3) ?
N4 C8 . 1.340(3) ?
N4 C7 . 1.338(3) ?
N2 C2 . 1.371(3) ?
N2 C3 . 1.363(3) ?
N2 H2 . 0.95(3) ?
N3 C1 . 1.301(3) ?
N3 H3A . 0.87(3) ?
N3 H3C . 0.88(3) ?
C5 H5 . 0.9500 ?
C5 C9 . 1.399(3) ?
C5 C6 . 1.376(3) ?
C1 C4 . 1.424(3) ?
C9 C11 . 1.527(3) ?
C9 C8 . 1.413(3) ?
C6 H6 . 0.9500 ?
C6 C7 . 1.383(3) ?
C10 C8 . 1.536(3) ?
C7 H7 . 0.9500 ?
C4 H4 . 0.9500 ?
C4 C3 . 1.353(3) ?
C3 H3 . 0.9500 ?
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
O2A C10 C8 N4 . . . . 4.3(3) ?
O2A C10 C8 C9 . . . . -177.0(2) ?
O2B C10 C8 N4 . . . . -173.8(2) ?
O2B C10 C8 C9 . . . . 4.9(3) ?
N1 C1 C4 C3 . . . . 0.0(3) ?
N3 C1 C4 C3 . . . . 179.7(2) ?
C5 C9 C11 O3A . . . . -1.1(3) ?
C5 C9 C11 O3B . . . . 177.8(2) ?
C5 C9 C8 N4 . . . . 0.6(3) ?
C5 C9 C8 C10 . . . . -177.9(2) ?
C5 C6 C7 N4 . . . . 0.7(3) ?
C1 N1 C2 O1 . . . . 179.5(2) ?
C1 N1 C2 N2 . . . . -1.0(3) ?
C1 C4 C3 N2 . . . . 0.2(4) ?
C9 C5 C6 C7 . . . . 0.0(3) ?
C6 C5 C9 C11 . . . . -179.2(2) ?
C6 C5 C9 C8 . . . . -0.6(3) ?
C11 C9 C8 N4 . . . . 178.9(2) ?
C11 C9 C8 C10 . . . . 0.3(4) ?
C2 N1 C1 N3 . . . . -179.3(2) ?
C2 N1 C1 C4 . . . . 0.5(3) ?
C2 N2 C3 C4 . . . . -0.8(4) ?
C8 N4 C7 C6 . . . . -0.7(3) ?
C8 C9 C11 O3A . . . . -179.4(2) ?
C8 C9 C11 O3B . . . . -0.5(4) ?
C7 N4 C8 C9 . . . . 0.0(3) ?
C7 N4 C8 C10 . . . . 178.8(2) ?
C3 N2 C2 O1 . . . . -179.5(2) ?
C3 N2 C2 N1 . . . . 1.1(3) ?