#------------------------------------------------------------------------------
#$Date: 2025-04-25 04:08:57 +0200 (Fri, 25 Apr 2025) $
#$Revision: 299399 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023480.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_2023480
loop_
_publ_author_name
'Shaposhnyk, Anna M.'
'Rudiuk, Vitalii V.'
'Baumer, Vyacheslav N.'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of ketorolac
tromethamine
;
_journal_coeditor_code EX2090
_journal_issue 5
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989025003226
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac 'C15 H12 N O3 +, C4 H12 N O3 -'
_chemical_formula_moiety 'C15 H12 N O3 +, C4 H12 N O3 -'
_chemical_formula_sum 'C19 H24 N2 O6'
_chemical_formula_weight 376.40
_chemical_name_common
;
Ketorolac tromethamine
;
_chemical_name_systematic
;
1,3-Dihydroxy-2-(hydroxymethyl)propan-2-aminium
5-benzoyl-2,3-dihydro-1H-pyrrolizine-1-carboxylate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-I 2ya'
_space_group_name_H-M_alt 'I 1 2/a 1'
_atom_sites_solution_hydrogens geom
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 90
_cell_angle_beta 96.389(6)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 20.3154(13)
_cell_length_b 6.6466(4)
_cell_length_c 28.0770(15)
_cell_measurement_reflns_used 2134
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 22.6880
_cell_measurement_theta_min 3.3670
_cell_volume 3767.6(4)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 293.15
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Rigaku Xcalibur Sapphire3'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0847
_diffrn_reflns_av_unetI/netI 0.0592
_diffrn_reflns_limit_h_max 25
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_limit_l_min -34
_diffrn_reflns_number 14262
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.084
_diffrn_reflns_theta_min 3.151
_exptl_absorpt_coefficient_mu 0.099
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.58393
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2018)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.327
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1600
_exptl_crystal_size_max 0.56
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.07
_refine_diff_density_max 0.163
_refine_diff_density_min -0.187
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.044
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 249
_refine_ls_number_reflns 3734
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.044
_refine_ls_R_factor_all 0.0904
_refine_ls_R_factor_gt 0.0566
_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^)+(0.0717P)^2^+0.7854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1430
_refine_ls_wR_factor_ref 0.1787
_reflns_number_gt 2314
_reflns_number_total 3734
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ex2090.cif
_cod_data_source_block I
_cod_database_code 2023480
_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 0.946
_shelx_estimated_absorpt_t_max 0.993
_shelx_hkl_file
;
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0 0 -662029.03 2332.00 4
0 0 666423.89 2416.85 2
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0 0 -656028.55 2395.84 2
0 0 -8 850.86 95.18 2
0 0 -8 870.11 86.36 1
0 0 -8 1055.55 83.86 5
0 0 8 997.00 109.66 1
0 0 -8 1045.94 78.41 4
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0 0 10 6352.78 300.91 4
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0 0 -10 5570.60 312.07 1
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22 1 1 23.88 35.08 4
22 -1 1 42.58 20.96 8
22 1 3 59.07 43.88 4
22 -1 3 150.84 82.42 8
22 1 5 24.93 35.55 4
22 -1 5 8.76 21.42 8
22 1 7 37.97 30.74 4
22 -1 7 -24.11 48.69 8
22 1 9 32.04 39.78 4
22 -1 9 84.95 66.50 8
22 1 11 27.45 38.87 4
22 -1 11 11.78 21.11 8
22 -2 -16 1.76 1.80 8
22 2 -16 43.80 35.20 3
22 -2 -14 8.60 13.69 8
22 2 -14 27.17 18.69 3
22 -2 -12 -27.63 40.09 8
22 2 -12 -35.32 18.12 3
22 2 -10 83.53 54.90 4
22 -2 -10 214.03 82.07 8
22 2 -10 125.10 78.84 8
22 2 -10 204.71 77.15 3
22 2 -8 36.96 38.79 4
22 -2 -8 114.01 71.04 8
22 2 -8 45.52 52.07 8
22 2 -8 125.76 60.23 3
22 2 -6 88.74 48.03 4
22 -2 -6 265.09 104.41 8
22 2 -6 220.05 73.67 3
22 2 -4 2.15 13.13 4
22 -2 -4 -38.19 37.15 8
22 2 -2 191.82 75.60 4
22 -2 -2 282.61 100.68 8
22 2 0 70.45 46.63 4
22 -2 0 47.86 40.71 8
22 2 2 -5.71 33.09 4
22 -2 2 9.69 34.36 8
22 2 4 143.80 66.87 4
22 -2 4 100.12 56.50 8
22 2 6 -20.56 18.69 4
22 -2 6 8.07 32.41 8
22 2 8 13.47 14.74 4
22 -2 8 6.96 27.50 8
22 2 10 42.02 34.23 4
22 -2 10 67.80 67.65 8
22 -3 -13 32.49 34.74 8
22 3 -13 63.66 50.01 3
22 -3 -11 -8.24 3.73 8
22 3 -11 4.49 22.02 3
22 3 -9 15.17 20.58 4
22 -3 -9 -14.99 33.89 8
22 3 -9 5.23 27.02 3
22 3 -7 -11.68 27.25 4
22 -3 -7 22.42 51.39 8
22 3 -7 10.93 21.39 3
22 3 -5 1.79 6.45 4
22 -3 -5 25.79 26.81 8
22 3 -5 57.75 39.25 3
22 3 -3 -1.85 15.61 4
22 -3 -3 32.71 42.98 8
22 3 -1 12.53 14.43 4
22 -3 -1 10.32 22.59 8
22 3 1 66.73 56.15 4
22 -3 1 19.34 32.74 8
22 3 3 4.69 6.26 4
22 -3 3 82.14 59.49 8
22 3 5 -18.95 38.91 4
22 -3 5 44.61 45.85 8
22 3 7 31.07 35.21 4
22 -3 7 48.47 35.90 8
23 0 -17 30.35 31.44 3
23 0 -15 -36.78 47.61 8
23 0 -15 -0.66 15.51 3
23 0 -13 -2.10 26.14 8
23 0 -13 -5.98 4.46 3
23 0 -11 15.67 27.50 8
23 0 -11 -11.36 23.83 3
23 0 -9 42.28 42.05 8
23 0 -7 4.94 21.49 8
23 0 -5 -61.94 72.90 8
23 0 -3 -67.13 67.05 8
23 0 -1 -14.26 13.06 8
23 0 1 -2.82 26.63 8
23 0 3 -16.11 38.84 8
23 0 5 13.21 28.37 4
23 0 5 0.92 18.27 8
23 0 7 -7.91 37.34 4
23 0 7 -21.13 33.06 8
23 0 9 -4.97 42.31 4
23 0 9 72.71 53.95 8
-23 1 16 8.79 24.27 2
23 -1 -16 -0.26 19.45 8
23 -1 -16 33.47 33.45 3
23 1 -16 30.02 23.50 3
-23 1 14 -0.95 7.43 2
23 -1 -14 1.78 13.54 8
23 -1 -14 16.06 29.10 3
23 1 -14 -14.19 21.49 3
23 -1 -12 22.21 30.39 8
23 1 -12 101.58 73.35 8
23 1 -12 60.91 40.34 3
23 -1 -10 -10.24 22.48 8
23 1 -10 18.16 24.42 8
23 1 -10 -24.36 17.12 3
23 -1 -8 -20.25 23.70 8
23 1 -8 -23.33 26.74 8
23 1 -8 9.54 24.96 3
23 1 -6 11.49 13.82 4
23 -1 -6 -7.83 27.16 8
23 1 -6 12.21 7.92 8
23 1 -4 25.72 37.74 4
23 -1 -4 48.63 62.18 8
23 1 -4 83.04 63.47 8
23 1 -2 109.02 58.02 4
23 -1 -2 329.27 114.23 8
23 1 -2 298.58 115.78 8
23 1 0 55.66 12.95 4
23 -1 0 -27.56 58.11 8
23 1 2 86.84 58.49 4
23 -1 2 12.51 32.45 8
23 1 4 187.46 77.67 4
23 -1 4 86.05 66.67 8
23 1 6 122.96 71.32 4
23 -1 6 64.79 55.37 8
23 1 8 -21.89 20.23 4
23 -1 8 10.67 45.49 8
23 -2 -13 49.15 39.00 8
23 2 -13 89.37 54.18 3
23 -2 -11 1.22 6.01 8
23 2 -11 65.58 55.34 3
23 2 -9 24.56 34.63 4
23 -2 -9 35.07 11.87 8
23 2 -9 13.88 41.76 8
23 2 -9 58.86 41.75 3
23 2 -7 -0.52 9.44 4
23 -2 -7 30.19 38.69 8
23 2 -7 -7.36 13.05 8
23 2 -7 17.97 14.85 3
23 2 -5 13.47 26.82 4
23 -2 -5 150.00 76.64 8
23 2 -3 35.93 37.52 4
23 -2 -3 213.74 79.31 8
23 2 -1 0.83 22.38 4
23 -2 -1 -25.04 44.73 8
23 2 1 33.88 35.92 4
23 -2 1 14.09 27.24 8
23 2 3 40.93 43.56 4
23 -2 3 2.29 16.96 8
23 2 5 -16.66 27.73 4
23 -2 5 -47.81 56.07 8
23 2 7 -17.06 28.73 4
23 -2 7 39.79 29.52 8
23 3 -8 17.82 26.04 4
23 -3 -8 -19.44 28.92 8
23 3 -8 23.86 24.03 3
23 3 -6 -5.30 22.51 4
23 -3 -6 16.72 14.71 8
23 3 -6 17.45 36.13 3
23 3 -4 6.90 16.28 4
23 -3 -4 3.48 15.82 8
23 3 -2 -4.69 10.70 4
23 -3 -2 37.52 41.54 8
23 3 0 6.17 22.23 4
23 -3 0 11.28 17.89 8
23 3 2 1.45 16.18 4
24 0 -12 8.41 19.24 8
24 0 -12 31.38 24.27 3
24 0 -10 61.78 60.36 8
24 0 -8 20.12 17.80 8
24 0 -6 -12.15 34.54 8
24 0 -4 66.26 59.30 8
24 0 -2 93.92 39.76 8
24 0 0 48.27 46.49 8
24 0 2 38.87 42.52 8
24 0 4 16.78 37.67 8
24 0 6 5.14 13.33 8
24 1 -13 70.33 48.28 3
24 -1 -11 11.42 24.92 8
24 1 -11 -6.09 2.84 8
24 1 -11 0.17 17.48 3
24 -1 -9 5.30 17.88 8
24 1 -9 13.72 35.15 8
24 1 -9 -11.73 13.83 3
24 -1 -7 68.47 56.98 8
24 1 -7 3.17 32.10 8
24 1 -5 13.60 21.18 4
24 -1 -5 -9.15 23.06 8
24 1 -5 -14.19 33.08 8
24 1 -3 49.66 44.81 4
24 -1 -3 58.14 47.93 8
24 1 -3 136.96 64.45 8
24 1 -1 27.69 36.96 4
24 -1 -1 -2.22 35.44 8
24 1 -1 115.93 82.28 8
24 1 1 -21.31 48.50 4
24 -1 1 2.14 3.07 8
24 1 1 -20.40 9.74 8
24 1 3 -6.96 26.58 4
24 -1 3 9.54 8.19 8
24 1 5 61.51 34.65 4
24 -1 5 152.35 85.61 8
24 2 -8 18.92 17.52 4
24 2 -8 -11.38 39.15 8
24 2 -8 37.08 32.80 3
24 2 -6 16.45 27.81 4
24 -2 -6 58.75 49.29 8
24 2 -6 33.36 49.62 8
24 2 -4 20.89 30.90 4
24 -2 -4 1.69 15.56 8
24 2 -2 35.60 38.45 4
24 -2 -2 124.85 78.09 8
24 2 0 4.78 3.73 4
24 -2 0 -14.96 33.83 8
24 2 2 3.22 15.89 4
25 0 -5 39.10 45.30 8
25 0 -3 7.84 12.14 8
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 68060
_shelx_res_file
;
TITL 0sa in I2/a
kt.res
created by SHELXL-2018/3 at 19:49:33 on 27-Mar-2025
REM I2/a (#15 in standard setting)
CELL 0.71073 20.315353 6.646624 28.077001 90 96.3891 90
ZERR 8 0.001308 0.000432 0.001491 0 0.0056 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H N O
UNIT 152 192 16 48
EQIV $1 +X,0.5-Y,0.5+Z
EQIV $2 +X,1+Y,+Z
EQIV $3 1-X,1-Y,1-Z
EQIV $4 1-X,-Y,1-Z
L.S. 22
PLAN 1
SIZE 0.56 0.22 0.07
TEMP 20
CONF
HTAB O4 O3_$1
HTAB O5 O6_$2
HTAB O6 O2
HTAB N1 O1
HTAB N1 O1_$3
HTAB N1 O2_$4
htab
BOND $H
MORE -1
fmap 2
acta
REM
REM
REM
WGHT 0.071700 0.785400
FVAR 1.02214 0.08514
O1 4 0.485933 0.330328 0.440783 11.00000 0.07804 0.06797 =
0.04992 -0.00460 0.00416 -0.01431
O2 4 0.465223 0.008461 0.424050 11.00000 0.06465 0.06026 =
0.06546 0.00657 0.00447 -0.00261
O3 4 0.356415 0.143619 0.206824 11.00000 0.11046 0.06151 =
0.05212 -0.00724 -0.00870 0.00287
O4 4 0.401043 0.353064 0.618615 11.00000 0.09139 0.09121 =
0.05418 -0.00060 0.01108 -0.01372
AFIX 147
H4 2 0.384403 0.347567 0.643885 11.00000 -1.50000
AFIX 0
O5 4 0.355010 0.573013 0.481592 11.00000 0.12786 0.06460 =
0.06343 0.00967 -0.01052 0.00497
AFIX 147
H5 2 0.364973 0.692435 0.483945 11.00000 -1.50000
AFIX 0
O6 4 0.391500 -0.029632 0.496430 11.00000 0.07193 0.05681 =
0.07155 -0.00078 0.00808 -0.00447
AFIX 147
H6A 2 0.415208 -0.019853 0.474738 11.00000 -1.50000
AFIX 0
N1 3 0.450025 0.314470 0.533066 11.00000 0.05419 0.05640 =
0.04351 0.00075 -0.00042 -0.00567
AFIX 137
H1A 2 0.457862 0.325858 0.502620 11.00000 -1.20000
H1B 2 0.470895 0.206582 0.546029 11.00000 -1.20000
H1C 2 0.464673 0.423879 0.549180 11.00000 -1.20000
AFIX 0
N4 3 0.427647 0.261879 0.292609 11.00000 0.06046 0.05460 =
0.04246 -0.00233 0.00140 -0.00050
C1 1 0.500579 0.223046 0.362625 11.00000 0.05183 0.06413 =
0.04949 0.00045 0.00140 -0.00020
AFIX 13
H1 2 0.542985 0.294588 0.364741 11.00000 21.00000
AFIX 0
C2 1 0.504422 0.035847 0.330415 11.00000 0.07692 0.07264 =
0.05560 -0.00417 0.00145 0.01658
AFIX 23
H2A 2 0.549840 0.012643 0.324234 11.00000 21.00000
H2B 2 0.488949 -0.082141 0.346188 11.00000 21.00000
AFIX 0
C3 1 0.461170 0.074013 0.283779 11.00000 0.09348 0.06506 =
0.06010 -0.00886 -0.00381 0.01770
AFIX 23
H3A 2 0.487734 0.087891 0.257319 11.00000 21.00000
H3B 2 0.429569 -0.034252 0.276724 11.00000 21.00000
AFIX 0
C4 1 0.482861 0.182675 0.413330 11.00000 0.04599 0.06197 =
0.04999 0.00208 -0.00586 0.00017
C5 1 0.380283 0.380295 0.267214 11.00000 0.05403 0.05901 =
0.04248 0.00091 -0.00029 -0.00180
C6 1 0.372199 0.544503 0.296378 11.00000 0.06997 0.05716 =
0.05137 -0.00323 -0.00213 0.00529
AFIX 43
H6 2 0.343025 0.650623 0.288933 11.00000 -1.20000
AFIX 0
C7 1 0.414366 0.525640 0.338303 11.00000 0.07787 0.06246 =
0.04827 -0.00949 -0.00687 0.00643
AFIX 43
H7 2 0.418692 0.615070 0.363935 11.00000 -1.20000
AFIX 0
C7A 1 0.448855 0.347992 0.334719 11.00000 0.05828 0.05368 =
0.04653 -0.00219 0.00019 -0.00263
C8 1 0.346372 0.315344 0.222334 11.00000 0.06244 0.06085 =
0.04497 0.00042 0.00428 -0.00789
C9 1 0.300137 0.450699 0.192760 11.00000 0.05259 0.06801 =
0.04208 -0.00448 0.00201 -0.00095
C10 1 0.314451 0.648977 0.183684 11.00000 0.06497 0.06669 =
0.05879 -0.00278 -0.00676 -0.00267
AFIX 43
H10 2 0.351325 0.709561 0.200381 11.00000 -1.20000
AFIX 0
C11 1 0.274767 0.757846 0.150219 11.00000 0.09572 0.07665 =
0.06900 0.00170 -0.01281 0.02072
AFIX 43
H11 2 0.285832 0.889880 0.143567 11.00000 -1.20000
AFIX 0
C12 1 0.218975 0.672778 0.126607 11.00000 0.07696 0.11557 =
0.06418 -0.00756 -0.01360 0.03340
AFIX 43
H12 2 0.192488 0.746515 0.103745 11.00000 -1.20000
AFIX 0
C13 1 0.202221 0.478798 0.136716 11.00000 0.05126 0.13864 =
0.06696 -0.02181 -0.00640 0.00318
AFIX 43
H13 2 0.163240 0.423167 0.121828 11.00000 -1.20000
AFIX 0
C14 1 0.243262 0.365651 0.169060 11.00000 0.05922 0.09530 =
0.05918 -0.01066 0.00479 -0.01653
AFIX 43
H14 2 0.232702 0.232434 0.174914 11.00000 -1.20000
AFIX 0
C15 1 0.377493 0.292872 0.535356 11.00000 0.05098 0.05991 =
0.05251 0.00128 -0.00295 -0.00320
C16 1 0.367426 0.219621 0.585083 11.00000 0.06462 0.07304 =
0.06193 0.00325 0.01018 -0.00598
AFIX 23
H16A 2 0.320578 0.217037 0.588954 11.00000 21.00000
H16B 2 0.384926 0.084518 0.589999 11.00000 21.00000
AFIX 0
C17 1 0.344618 0.497332 0.527003 11.00000 0.06619 0.06733 =
0.06582 0.00176 -0.00420 0.00853
AFIX 23
H17A 2 0.297458 0.484927 0.529118 11.00000 21.00000
H17B 2 0.362784 0.590435 0.551643 11.00000 21.00000
AFIX 0
C18 1 0.350960 0.143572 0.496942 11.00000 0.05211 0.06783 =
0.07076 -0.00432 -0.00681 -0.00309
AFIX 23
H18A 2 0.306589 0.103162 0.502539 11.00000 21.00000
H18B 2 0.348183 0.208564 0.465850 11.00000 21.00000
AFIX 0
HKLF 4
REM 0sa in I2/a
REM wR2 = 0.1787, GooF = S = 1.044, Restrained GooF = 1.044 for all data
REM R1 = 0.0566 for 2314 Fo > 4sig(Fo) and 0.0904 for all 3734 data
REM 249 parameters refined using 0 restraints
END
WGHT 0.0728 0.7500
REM Instructions for potential hydrogen bonds
HTAB O4 O3_$1
HTAB O5 O6_$2
HTAB O6 O2
HTAB N1 O1
HTAB N1 O2_$4
HTAB N1 O1_$3
HTAB C1 O4_$3
REM Highest difference peak 0.163, deepest hole -0.187, 1-sigma level 0.045
Q1 1 0.4506 -0.0203 0.2509 11.00000 0.05 0.16
;
_shelx_res_checksum 75774
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.48593(10) 0.3303(3) 0.44078(6) 0.0655(5) Uani d 1 . .
O O2 0.46522(9) 0.0085(3) 0.42405(6) 0.0637(5) Uani d 1 . .
O O3 0.35641(11) 0.1436(3) 0.20682(6) 0.0760(6) Uani d 1 . .
O O4 0.40104(11) 0.3531(3) 0.61861(7) 0.0787(6) Uani d 1 . .
H H4 0.384403 0.347567 0.643885 0.118 Uiso calc 1 . .
O O5 0.35501(13) 0.5730(3) 0.48159(7) 0.0869(7) Uani d 1 . .
H H5 0.364973 0.692435 0.483945 0.130 Uiso calc 1 . .
O O6 0.39150(10) -0.0296(3) 0.49643(7) 0.0668(5) Uani d 1 . .
H H6A 0.415208 -0.019853 0.474738 0.100 Uiso calc 1 . .
N N1 0.45003(10) 0.3145(3) 0.53307(6) 0.0518(5) Uani d 1 . .
H H1A 0.457862 0.325858 0.502620 0.062 Uiso calc 1 . .
H H1B 0.470895 0.206582 0.546029 0.062 Uiso calc 1 . .
H H1C 0.464673 0.423879 0.549180 0.062 Uiso calc 1 . .
N N4 0.42765(10) 0.2619(3) 0.29261(6) 0.0528(5) Uani d 1 . .
C C1 0.50058(13) 0.2230(4) 0.36263(8) 0.0555(6) Uani d 1 . .
H H1 0.542985 0.294588 0.364741 0.085(3) Uiso calc 1 . .
C C2 0.50442(16) 0.0358(4) 0.33042(9) 0.0688(8) Uani d 1 . .
H H2A 0.549840 0.012643 0.324234 0.085(3) Uiso calc 1 . .
H H2B 0.488949 -0.082141 0.346188 0.085(3) Uiso calc 1 . .
C C3 0.46117(17) 0.0740(4) 0.28378(10) 0.0738(8) Uani d 1 . .
H H3A 0.487734 0.087891 0.257319 0.085(3) Uiso calc 1 . .
H H3B 0.429569 -0.034252 0.276724 0.085(3) Uiso calc 1 . .
C C4 0.48286(13) 0.1827(4) 0.41333(9) 0.0535(6) Uani d 1 . .
C C5 0.38028(13) 0.3803(4) 0.26721(8) 0.0523(6) Uani d 1 . .
C C6 0.37220(14) 0.5445(4) 0.29638(9) 0.0602(7) Uani d 1 . .
H H6 0.343025 0.650623 0.288933 0.072 Uiso calc 1 . .
C C7 0.41437(15) 0.5256(4) 0.33830(9) 0.0639(7) Uani d 1 . .
H H7 0.418692 0.615070 0.363935 0.077 Uiso calc 1 . .
C C7A 0.44886(13) 0.3480(4) 0.33472(8) 0.0533(6) Uani d 1 . .
C C8 0.34637(14) 0.3153(4) 0.22233(8) 0.0562(6) Uani d 1 . .
C C9 0.30014(13) 0.4507(4) 0.19276(8) 0.0545(6) Uani d 1 . .
C C10 0.31445(15) 0.6490(4) 0.18368(9) 0.0645(7) Uani d 1 . .
H H10 0.351325 0.709561 0.200381 0.077 Uiso calc 1 . .
C C11 0.27477(18) 0.7578(5) 0.15022(10) 0.0821(9) Uani d 1 . .
H H11 0.285832 0.889880 0.143567 0.099 Uiso calc 1 . .
C C12 0.21897(18) 0.6728(6) 0.12661(11) 0.0872(10) Uani d 1 . .
H H12 0.192488 0.746515 0.103745 0.105 Uiso calc 1 . .
C C13 0.20222(16) 0.4788(7) 0.13672(11) 0.0866(10) Uani d 1 . .
H H13 0.163240 0.423167 0.121828 0.104 Uiso calc 1 . .
C C14 0.24326(15) 0.3657(5) 0.16906(10) 0.0714(8) Uani d 1 . .
H H14 0.232702 0.232434 0.174914 0.086 Uiso calc 1 . .
C C15 0.37749(13) 0.2929(4) 0.53536(8) 0.0551(6) Uani d 1 . .
C C16 0.36743(15) 0.2196(4) 0.58508(9) 0.0663(7) Uani d 1 . .
H H16A 0.320578 0.217037 0.588954 0.085(3) Uiso calc 1 . .
H H16B 0.384926 0.084518 0.589999 0.085(3) Uiso calc 1 . .
C C17 0.34462(15) 0.4973(4) 0.52700(9) 0.0673(7) Uani d 1 . .
H H17A 0.297458 0.484927 0.529118 0.085(3) Uiso calc 1 . .
H H17B 0.362784 0.590435 0.551643 0.085(3) Uiso calc 1 . .
C C18 0.35096(14) 0.1436(4) 0.49694(10) 0.0646(7) Uani d 1 . .
H H18A 0.306589 0.103162 0.502539 0.085(3) Uiso calc 1 . .
H H18B 0.348183 0.208564 0.465850 0.085(3) Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1 0.0780(14) 0.0680(12) 0.0499(10) -0.0143(10) 0.0042(9) -0.0046(9)
O2 0.0646(13) 0.0603(11) 0.0655(11) -0.0026(9) 0.0045(9) 0.0066(8)
O3 0.1105(18) 0.0615(12) 0.0521(10) 0.0029(11) -0.0087(10) -0.0072(9)
O4 0.0914(16) 0.0912(14) 0.0542(11) -0.0137(12) 0.0111(11) -0.0006(10)
O5 0.128(2) 0.0646(12) 0.0634(12) 0.0050(13) -0.0105(12) 0.0097(9)
O6 0.0719(14) 0.0568(11) 0.0715(12) -0.0045(9) 0.0081(10) -0.0008(9)
N1 0.0542(14) 0.0564(12) 0.0435(10) -0.0057(9) -0.0004(9) 0.0008(8)
N4 0.0605(14) 0.0546(12) 0.0425(11) -0.0005(10) 0.0014(9) -0.0023(9)
C1 0.0518(16) 0.0641(15) 0.0495(13) -0.0002(12) 0.0014(11) 0.0004(11)
C2 0.077(2) 0.0726(18) 0.0556(15) 0.0166(15) 0.0014(14) -0.0042(13)
C3 0.093(2) 0.0651(17) 0.0601(16) 0.0177(16) -0.0038(15) -0.0089(13)
C4 0.0460(15) 0.0620(16) 0.0500(13) 0.0002(11) -0.0059(10) 0.0021(12)
C5 0.0540(16) 0.0590(14) 0.0425(12) -0.0018(12) -0.0003(11) 0.0009(11)
C6 0.0700(18) 0.0572(15) 0.0514(14) 0.0053(13) -0.0021(12) -0.0032(11)
C7 0.078(2) 0.0625(16) 0.0483(13) 0.0064(14) -0.0069(13) -0.0095(12)
C7A 0.0583(16) 0.0537(14) 0.0465(13) -0.0026(11) 0.0002(11) -0.0022(10)
C8 0.0624(17) 0.0608(15) 0.0450(13) -0.0079(12) 0.0043(11) 0.0004(11)
C9 0.0526(16) 0.0680(16) 0.0421(12) -0.0010(12) 0.0020(11) -0.0045(11)
C10 0.0650(19) 0.0667(17) 0.0588(15) -0.0027(13) -0.0068(13) -0.0028(12)
C11 0.096(3) 0.077(2) 0.0690(18) 0.0207(18) -0.0128(18) 0.0017(15)
C12 0.077(2) 0.116(3) 0.0642(19) 0.033(2) -0.0136(16) -0.0076(18)
C13 0.0513(19) 0.139(3) 0.0670(19) 0.003(2) -0.0064(14) -0.022(2)
C14 0.0592(18) 0.095(2) 0.0592(16) -0.0165(16) 0.0048(14) -0.0107(14)
C15 0.0510(16) 0.0599(15) 0.0525(14) -0.0032(12) -0.0029(11) 0.0013(11)
C16 0.0646(19) 0.0730(18) 0.0619(16) -0.0060(14) 0.0102(14) 0.0032(13)
C17 0.0662(19) 0.0673(17) 0.0658(17) 0.0085(14) -0.0042(14) 0.0018(13)
C18 0.0521(17) 0.0678(17) 0.0708(17) -0.0031(13) -0.0068(13) -0.0043(13)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C16 O4 H4 . . 109.5 ?
C17 O5 H5 . . 109.5 ?
C18 O6 H6A . . 109.5 ?
H1A N1 H1B . . 109.5 ?
H1A N1 H1C . . 109.5 ?
H1B N1 H1C . . 109.5 ?
C15 N1 H1A . . 109.5 ?
C15 N1 H1B . . 109.5 ?
C15 N1 H1C . . 109.5 ?
C5 N4 C3 . . 135.6(2) ?
C7A N4 C3 . . 113.9(2) ?
C7A N4 C5 . . 110.5(2) ?
C2 C1 H1 . . 109.0 ?
C4 C1 H1 . . 109.0 ?
C4 C1 C2 . . 115.8(2) ?
C7A C1 H1 . . 109.0 ?
C7A C1 C2 . . 102.7(2) ?
C7A C1 C4 . . 111.2(2) ?
C1 C2 H2A . . 110.1 ?
C1 C2 H2B . . 110.1 ?
H2A C2 H2B . . 108.4 ?
C3 C2 C1 . . 108.0(2) ?
C3 C2 H2A . . 110.1 ?
C3 C2 H2B . . 110.1 ?
N4 C3 C2 . . 103.5(2) ?
N4 C3 H3A . . 111.1 ?
N4 C3 H3B . . 111.1 ?
C2 C3 H3A . . 111.1 ?
C2 C3 H3B . . 111.1 ?
H3A C3 H3B . . 109.0 ?
O1 C4 O2 . . 125.0(2) ?
O1 C4 C1 . . 115.9(2) ?
O2 C4 C1 . . 119.1(2) ?
N4 C5 C6 . . 105.4(2) ?
N4 C5 C8 . . 121.5(2) ?
C6 C5 C8 . . 132.8(2) ?
C5 C6 H6 . . 125.4 ?
C7 C6 C5 . . 109.2(2) ?
C7 C6 H6 . . 125.4 ?
C6 C7 H7 . . 126.7 ?
C7A C7 C6 . . 106.7(2) ?
C7A C7 H7 . . 126.7 ?
N4 C7A C1 . . 111.3(2) ?
N4 C7A C7 . . 108.2(2) ?
C7 C7A C1 . . 140.4(2) ?
O3 C8 C5 . . 120.1(2) ?
O3 C8 C9 . . 118.5(2) ?
C5 C8 C9 . . 121.4(2) ?
C10 C9 C8 . . 123.3(2) ?
C10 C9 C14 . . 118.8(3) ?
C14 C9 C8 . . 117.5(3) ?
C9 C10 H10 . . 119.7 ?
C11 C10 C9 . . 120.6(3) ?
C11 C10 H10 . . 119.7 ?
C10 C11 H11 . . 119.9 ?
C12 C11 C10 . . 120.3(3) ?
C12 C11 H11 . . 119.9 ?
C11 C12 H12 . . 120.0 ?
C11 C12 C13 . . 119.9(3) ?
C13 C12 H12 . . 120.0 ?
C12 C13 H13 . . 120.0 ?
C12 C13 C14 . . 120.1(3) ?
C14 C13 H13 . . 120.0 ?
C9 C14 H14 . . 119.9 ?
C13 C14 C9 . . 120.1(3) ?
C13 C14 H14 . . 119.9 ?
N1 C15 C16 . . 107.9(2) ?
N1 C15 C17 . . 109.1(2) ?
N1 C15 C18 . . 107.9(2) ?
C16 C15 C17 . . 109.1(2) ?
C16 C15 C18 . . 111.8(2) ?
C18 C15 C17 . . 111.0(2) ?
O4 C16 C15 . . 107.9(2) ?
O4 C16 H16A . . 110.1 ?
O4 C16 H16B . . 110.1 ?
C15 C16 H16A . . 110.1 ?
C15 C16 H16B . . 110.1 ?
H16A C16 H16B . . 108.4 ?
O5 C17 C15 . . 110.6(2) ?
O5 C17 H17A . . 109.5 ?
O5 C17 H17B . . 109.5 ?
C15 C17 H17A . . 109.5 ?
C15 C17 H17B . . 109.5 ?
H17A C17 H17B . . 108.1 ?
O6 C18 C15 . . 112.2(2) ?
O6 C18 H18A . . 109.2 ?
O6 C18 H18B . . 109.2 ?
C15 C18 H18A . . 109.2 ?
C15 C18 H18B . . 109.2 ?
H18A C18 H18B . . 107.9 ?
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 C4 . 1.245(3) ?
O2 C4 . 1.258(3) ?
O3 C8 . 1.247(3) ?
O4 H4 . 0.8200 ?
O4 C16 . 1.413(3) ?
O5 H5 . 0.8200 ?
O5 C17 . 1.408(3) ?
O6 H6A . 0.8200 ?
O6 C18 . 1.416(3) ?
N1 H1A . 0.8900 ?
N1 H1B . 0.8900 ?
N1 H1C . 0.8900 ?
N1 C15 . 1.489(3) ?
N4 C3 . 1.457(3) ?
N4 C5 . 1.379(3) ?
N4 C7A . 1.341(3) ?
C1 H1 . 0.9800 ?
C1 C2 . 1.545(4) ?
C1 C4 . 1.530(3) ?
C1 C7A . 1.491(3) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C2 C3 . 1.515(4) ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C5 C6 . 1.385(3) ?
C5 C8 . 1.434(3) ?
C6 H6 . 0.9300 ?
C6 C7 . 1.382(4) ?
C7 H7 . 0.9300 ?
C7 C7A . 1.382(4) ?
C8 C9 . 1.486(4) ?
C9 C10 . 1.379(4) ?
C9 C14 . 1.388(4) ?
C10 H10 . 0.9300 ?
C10 C11 . 1.374(4) ?
C11 H11 . 0.9300 ?
C11 C12 . 1.370(5) ?
C12 H12 . 0.9300 ?
C12 C13 . 1.371(5) ?
C13 H13 . 0.9300 ?
C13 C14 . 1.385(4) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.514(3) ?
C15 C17 . 1.521(4) ?
C15 C18 . 1.520(3) ?
C16 H16A . 0.9700 ?
C16 H16B . 0.9700 ?
C17 H17A . 0.9700 ?
C17 H17B . 0.9700 ?
C18 H18A . 0.9700 ?
C18 H18B . 0.9700 ?
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
O4 H4 O3 8 0.82 1.92 2.731(3) 171.7 yes
O5 H5 O6 1_565 0.82 1.95 2.762(3) 174.1 yes
O6 H6A O2 . 0.82 1.85 2.667(2) 177.2 yes
N1 H1A O1 . 0.89 1.89 2.771(2) 171.8 yes
N1 H1B O2 5_656 0.89 2.05 2.926(3) 169.1 yes
N1 H1C O1 5_666 0.89 1.92 2.756(3) 155.3 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O3 C8 C9 C10 . . . . -133.1(3) ?
O3 C8 C9 C14 . . . . 39.5(3) ?
N1 C15 C16 O4 . . . . 53.9(3) ?
N1 C15 C17 O5 . . . . 60.4(3) ?
N1 C15 C18 O6 . . . . 45.6(3) ?
N4 C5 C6 C7 . . . . 0.5(3) ?
N4 C5 C8 O3 . . . . 4.4(4) ?
N4 C5 C8 C9 . . . . -174.0(2) ?
C1 C2 C3 N4 . . . . -7.5(3) ?
C2 C1 C4 O1 . . . . 173.4(2) ?
C2 C1 C4 O2 . . . . -8.1(3) ?
C2 C1 C7A N4 . . . . -3.0(3) ?
C2 C1 C7A C7 . . . . 176.0(3) ?
C3 N4 C5 C6 . . . . -178.0(3) ?
C3 N4 C5 C8 . . . . 7.4(4) ?
C3 N4 C7A C1 . . . . -1.9(3) ?
C3 N4 C7A C7 . . . . 178.8(2) ?
C4 C1 C2 C3 . . . . 127.8(3) ?
C4 C1 C7A N4 . . . . -127.5(2) ?
C4 C1 C7A C7 . . . . 51.5(4) ?
C5 N4 C3 C2 . . . . -177.2(3) ?
C5 N4 C7A C1 . . . . -179.5(2) ?
C5 N4 C7A C7 . . . . 1.2(3) ?
C5 C6 C7 C7A . . . . 0.2(3) ?
C5 C8 C9 C10 . . . . 45.3(4) ?
C5 C8 C9 C14 . . . . -142.0(2) ?
C6 C5 C8 O3 . . . . -168.6(3) ?
C6 C5 C8 C9 . . . . 13.0(4) ?
C6 C7 C7A N4 . . . . -0.8(3) ?
C6 C7 C7A C1 . . . . -179.8(3) ?
C7A N4 C3 C2 . . . . 5.9(3) ?
C7A N4 C5 C6 . . . . -1.0(3) ?
C7A N4 C5 C8 . . . . -175.7(2) ?
C7A C1 C2 C3 . . . . 6.5(3) ?
C7A C1 C4 O1 . . . . -69.9(3) ?
C7A C1 C4 O2 . . . . 108.6(3) ?
C8 C5 C6 C7 . . . . 174.3(3) ?
C8 C9 C10 C11 . . . . 169.7(3) ?
C8 C9 C14 C13 . . . . -172.6(2) ?
C9 C10 C11 C12 . . . . 2.4(5) ?
C10 C9 C14 C13 . . . . 0.4(4) ?
C10 C11 C12 C13 . . . . 0.7(5) ?
C11 C12 C13 C14 . . . . -3.1(5) ?
C12 C13 C14 C9 . . . . 2.5(4) ?
C14 C9 C10 C11 . . . . -2.9(4) ?
C16 C15 C17 O5 . . . . 178.0(2) ?
C16 C15 C18 O6 . . . . -72.9(3) ?
C17 C15 C16 O4 . . . . -64.5(3) ?
C17 C15 C18 O6 . . . . 165.0(2) ?
C18 C15 C16 O4 . . . . 172.3(2) ?
C18 C15 C17 O5 . . . . -58.4(3) ?