#------------------------------------------------------------------------------
#$Date: 2023-10-10 04:19:25 +0200 (Tue, 10 Oct 2023) $
#$Revision: 286864 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022891.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_2022891
loop_
_publ_author_name
'Rajendrakumar, Satyasree'
'Surampudi Venkata Sai Durga, Anuja'
'Balasubramanian, Sridhar'
_publ_section_title
;
Strategic synthon approach in obtaining cocrystals and cocrystal
polymorphs of a high-Z′ system deferiprone -- an anti-thalassemia
drug
;
_journal_coeditor_code LO5093
_journal_issue 6
_journal_name_full
'Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials'
_journal_page_first 946
_journal_page_last 964
_journal_paper_doi 10.1107/S205252062100980X
_journal_volume 77
_journal_year 2021
_chemical_formula_moiety 'C7 H9 N O2, C6 H6 O2'
_chemical_formula_sum 'C13 H15 N O4'
_chemical_formula_weight 249.26
_chemical_name_common 'Deferiprone-Catechol (1:1)'
_space_group_crystal_system orthorhombic
_space_group_IT_number 61
_space_group_name_Hall '-P 2ac 2ab'
_space_group_name_H-M_alt 'P b c a'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 9.42310(10)
_cell_length_b 10.39380(10)
_cell_length_c 24.7171(3)
_cell_measurement_reflns_used 9084
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 30.50
_cell_measurement_theta_min 2.72
_cell_volume 2420.84(5)
_computing_cell_refinement 'SAINT (Bruker, 2016)'
_computing_data_collection 'APEX3 (Bruker, 2016)'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution 'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON-100'
_diffrn_measurement_method '\w and \f'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0332
_diffrn_reflns_av_unetI/netI 0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 34
_diffrn_reflns_limit_l_min -35
_diffrn_reflns_number 16449
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.587
_diffrn_reflns_theta_min 2.718
_diffrn_source microfocus
_exptl_absorpt_coefficient_mu 0.102
_exptl_absorpt_correction_T_max 0.7461
_exptl_absorpt_correction_T_min 0.6954
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS, Bruker, 2016'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.368
_exptl_crystal_description needle
_exptl_crystal_F_000 1056
_exptl_crystal_size_max 0.320
_exptl_crystal_size_mid 0.160
_exptl_crystal_size_min 0.140
_refine_diff_density_max 0.439
_refine_diff_density_min -0.256
_refine_diff_density_rms 0.056
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.035
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 177
_refine_ls_number_reflns 3709
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.035
_refine_ls_R_factor_all 0.0623
_refine_ls_R_factor_gt 0.0442
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+1.3237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0984
_refine_ls_wR_factor_ref 0.1069
_reflns_Friedel_coverage 0.000
_reflns_number_gt 2970
_reflns_number_total 3709
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file lo5093sup1.cif
_cod_data_source_block KA955_0m_def-cat_1_1_form1
_cod_database_code 2022891
_shelx_shelxl_version_number 2018/3
_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 0.968
_shelx_estimated_absorpt_t_max 0.986
_shelx_res_file
;
TITL KA955_0m_a.res in Pbca
KA955_0m.res
created by SHELXL-2018/3 at 11:28:44 on 10-Dec-2020
CELL 0.71073 9.4231 10.3938 24.7171 90.000 90.000 90.000
ZERR 8.00 0.0001 0.0001 0.0003 0.000 0.000 0.000
LATT 1
SYMM x+1/2, -y+1/2, -z
SYMM -x, y+1/2, -z+1/2
SYMM -x+1/2, -y, z+1/2
SFAC C H N O
UNIT 104 120 8 32
LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
TEMP -173
ACTA
L.S. 10
FMAP 2
PLAN 5
EQIV $1 -x+3/2, y+1/2, z
EQIV $2 x-1/2, -y+3/2, -z+1
HTAB O1 O3
HTAB O3 O2_$1
HTAB O4 O2
HTAB C5 O2_$2
HTAB C6 O4_$2
HTAB
SIZE 0.32 0.16 0.14
BOND $H
CONF
WGHT 0.042000 1.323700
FVAR 0.61201
MOLE 1
C1 1 0.667228 0.960799 0.557612 11.00000 0.01158 0.01161 =
0.01475 0.00094 -0.00114 -0.00011
C2 1 0.701588 0.943275 0.503856 11.00000 0.01059 0.01040 =
0.01539 0.00171 -0.00090 -0.00116
C3 1 0.629546 0.852297 0.470422 11.00000 0.01183 0.00855 =
0.01474 0.00009 -0.00111 0.00234
C4 1 0.521223 0.781102 0.496058 11.00000 0.01249 0.01142 =
0.01774 -0.00045 -0.00106 -0.00130
AFIX 43
H4 2 0.469658 0.718666 0.476022 11.00000 -1.20000
AFIX 0
C5 1 0.489540 0.800961 0.549506 11.00000 0.01121 0.01133 =
0.01911 0.00202 0.00097 -0.00071
AFIX 43
H5 2 0.415861 0.752016 0.565773 11.00000 -1.20000
AFIX 0
C6 1 0.519675 0.907431 0.637038 11.00000 0.01852 0.01955 =
0.01369 0.00142 0.00394 -0.00149
AFIX 137
H6A 2 0.483873 0.995152 0.642042 11.00000 -1.50000
H6B 2 0.602676 0.894006 0.660251 11.00000 -1.50000
H6C 2 0.445398 0.845602 0.646743 11.00000 -1.50000
AFIX 0
C7 1 0.742353 1.058269 0.591707 11.00000 0.02160 0.02172 =
0.01506 -0.00238 -0.00033 -0.00838
AFIX 137
H7A 2 0.819646 1.097080 0.570794 11.00000 -1.50000
H7B 2 0.781373 1.016220 0.623926 11.00000 -1.50000
H7C 2 0.675255 1.125362 0.602738 11.00000 -1.50000
AFIX 0
N1 3 0.560544 0.888615 0.579803 11.00000 0.01251 0.01188 =
0.01372 0.00220 0.00066 0.00080
O1 4 0.809508 1.014252 0.483402 11.00000 0.01925 0.02119 =
0.01472 0.00001 0.00225 -0.01031
H1O 2 0.805983 1.012258 0.448247 11.00000 0.03119
MOLE 2
C8 1 0.935397 1.085530 0.341850 11.00000 0.01259 0.01353 =
0.01122 0.00082 -0.00005 0.00167
C9 1 0.942230 0.960601 0.320845 11.00000 0.01379 0.01334 =
0.01234 0.00000 -0.00217 0.00063
C10 1 1.042688 0.930828 0.281798 11.00000 0.01757 0.02060 =
0.01395 -0.00423 -0.00135 0.00436
AFIX 43
H10 2 1.048064 0.845799 0.267849 11.00000 -1.20000
AFIX 0
C11 1 1.135418 1.024392 0.262960 11.00000 0.01708 0.03067 =
0.01490 0.00005 0.00342 0.00267
AFIX 43
H11 2 1.204309 1.003196 0.236352 11.00000 -1.20000
AFIX 0
C12 1 1.127508 1.148874 0.282987 11.00000 0.01799 0.02502 =
0.02039 0.00527 0.00233 -0.00253
AFIX 43
H12 2 1.190219 1.213222 0.269816 11.00000 -1.20000
AFIX 0
C13 1 1.027408 1.179357 0.322459 11.00000 0.01865 0.01475 =
0.01918 0.00195 0.00148 -0.00159
AFIX 43
H13 2 1.022025 1.264603 0.336171 11.00000 -1.20000
AFIX 0
O2 4 0.665002 0.839915 0.420143 11.00000 0.01876 0.01150 =
0.01369 -0.00116 0.00139 -0.00174
O3 4 0.835525 1.108091 0.380766 11.00000 0.01912 0.00997 =
0.01638 -0.00147 0.00556 0.00040
H3O 2 0.843112 1.189322 0.393188 11.00000 0.05082
O4 4 0.850510 0.866886 0.337542 11.00000 0.02058 0.01148 =
0.01881 -0.00248 0.00456 -0.00154
H4O 2 0.797228 0.891120 0.363386 11.00000 0.03317
HKLF 4 1 1 0 0 0 1 0 0 0 1
REM KA955_0m_a.res in Pbca
REM wR2 = 0.1069, GooF = S = 1.035, Restrained GooF = 1.035 for all data
REM R1 = 0.0442 for 2970 Fo > 4sig(Fo) and 0.0623 for all 3709 data
REM 177 parameters refined using 0 restraints
END
WGHT 0.0420 1.3237
REM Instructions for potential hydrogen bonds
HTAB C5 O2_$2
HTAB C6 O4_$2
HTAB O1 O3
HTAB O3 O2_$1
HTAB O4 O2
REM Highest difference peak 0.439, deepest hole -0.256, 1-sigma level 0.056
Q1 1 0.6805 0.9546 0.5307 11.00000 0.05 0.44
Q2 1 0.6697 0.8960 0.4865 11.00000 0.05 0.36
Q3 1 0.5427 0.8984 0.6070 11.00000 0.05 0.33
Q4 1 0.9805 1.1343 0.3288 11.00000 0.05 0.32
Q5 1 0.9504 1.0130 0.3362 11.00000 0.05 0.30
;
_shelx_res_checksum 57585
_shelx_hkl_file
;
-1 0 0 0.28 0.59
2 0 0 1402.52 47.44
-2 0 0 1443.19 47.46
-3 0 0 -0.75 1.11
3 0 0 -0.64 0.91
4 0 0 72.55 4.15
-4 0 0 64.96 4.31
5 0 0 1.12 1.73
6 0 0 5764.60 191.18
7 0 0 4.41 3.88
8 0 0 197.97 11.62
9 0 0 -1.31 4.39
10 0 0 754.78 30.78
11 0 0 -0.21 6.48
13 0 0 14.54 8.15
-1 1 0 0.23 0.25
-1 -1 0 0.33 0.55
1 1 0 0.55 0.55
1 -1 0 0.14 0.25
1 1 0 -0.03 0.41
-1 -1 0 0.25 0.41
-2 -1 0 1846.48 61.13
-2 1 0 1893.13 61.37
-2 -1 0 1907.41 62.09
2 1 0 1803.66 60.94
2 -1 0 1847.87 61.34
2 1 0 1866.46 62.07
-3 -1 0 -1.02 1.10
3 1 0 -1.34 1.11
-3 1 0 -0.39 1.01
3 -1 0 -0.08 0.93
-3 -1 0 0.36 0.60
4 -1 0 82.73 4.24
-4 1 0 77.04 4.31
4 1 0 75.49 4.64
5 -1 0 -0.05 1.47
5 1 0 -1.67 1.64
6 -1 0 351.50 14.37
7 -1 0 -0.40 2.56
7 1 0 2.27 3.56
8 -1 0 85.20 8.18
8 1 0 99.28 8.61
9 -1 0 2.87 4.63
9 1 0 -3.95 4.40
10 1 0 206.73 13.66
10 -1 0 185.15 12.31
11 1 0 -1.75 6.80
11 -1 0 -8.59 5.91
12 1 0 1.07 8.21
12 -1 0 -10.73 6.16
13 1 0 -3.26 9.60
0 -2 0 9352.78 329.00
0 2 0 9056.50 328.36
-1 -2 0 0.29 0.75
-1 2 0 0.02 0.65
1 2 0 0.09 0.83
1 2 0 0.59 0.76
1 -2 0 -0.76 0.52
-1 -2 0 0.50 0.92
-2 -2 0 5474.69 176.58
2 2 0 5270.18 176.54
-2 -2 0 5352.24 175.80
-3 -2 0 0.79 0.91
-3 2 0 0.47 0.85
3 2 0 -0.67 1.20
3 2 0 0.69 0.72
3 -2 0 0.05 0.79
4 -2 0 86.64 4.22
-4 2 0 84.52 4.28
-4 -2 0 87.97 4.09
4 2 0 83.02 5.23
-5 -2 0 2.66 1.26
-5 2 0 0.19 1.61
5 -2 0 -1.10 1.39
5 2 0 -1.52 1.88
6 2 0 149.80 9.36
6 -2 0 162.63 7.63
-6 -2 0 157.74 6.76
8 -2 0 1075.15 38.98
8 2 0 1058.59 40.32
9 -2 0 -4.31 4.41
9 2 0 -1.35 4.69
10 -2 0 102.09 9.58
10 2 0 98.59 10.52
11 -2 0 7.62 5.16
12 2 0 9.79 8.22
13 2 0 9.76 9.52
0 3 0 0.88 0.95
0 -3 0 0.74 0.91
0 3 0 1.06 0.67
0 -3 0 -1.43 0.83
-1 -3 0 -2.44 1.10
1 3 0 -0.97 0.91
1 -3 0 0.16 0.56
1 -3 0 0.99 0.80
-1 3 0 -0.15 0.44
1 3 0 0.25 0.91
-1 -3 0 0.27 1.03
-1 3 0 -1.09 0.88
-2 -3 0 3925.26 127.91
2 3 0 3778.94 127.74
-2 3 0 3879.30 127.42
-2 -3 0 4025.09 128.57
2 3 0 3792.25 128.46
-3 3 0 -0.52 0.51
-3 -3 0 -1.81 1.03
3 3 0 -0.49 0.95
3 3 0 1.68 1.51
3 -3 0 -0.07 0.58
-3 3 0 0.32 0.80
4 3 0 35.74 3.81
-4 3 0 36.01 2.39
4 3 0 35.11 2.38
4 -3 0 36.82 2.33
5 3 0 1.83 3.01
-5 3 0 -0.03 1.53
5 -3 0 0.76 1.39
-6 3 0 1558.10 53.46
6 -3 0 1628.27 53.55
6 3 0 1550.79 55.98
7 3 0 -2.23 3.94
7 -3 0 4.93 2.24
8 3 0 139.07 10.57
8 -3 0 129.96 7.87
9 -3 0 3.04 5.04
9 3 0 -3.32 5.05
10 -3 0 157.74 10.31
10 3 0 167.97 13.10
11 3 0 -6.10 6.85
12 3 0 18.55 8.82
13 3 0 -1.74 9.41
0 -4 0 3467.75 118.28
0 -4 0 3635.22 118.10
0 4 0 3663.86 118.58
0 4 0 3566.72 118.07
1 -4 0 -0.66 0.90
-1 4 0 1.98 0.67
1 -4 0 -0.46 1.04
-1 4 0 -2.34 1.08
1 4 0 0.61 1.24
-1 -4 0 -0.21 1.49
1 4 0 1.90 1.15
-2 4 0 110.60 5.08
2 -4 0 104.79 4.55
2 4 0 105.78 5.56
2 4 0 98.47 5.27
3 4 0 4.63 1.95
-3 4 0 -0.46 1.15
3 4 0 2.51 1.45
4 4 0 2141.35 74.17
4 4 0 2143.16 72.18
-4 4 0 2209.58 71.84
5 4 0 -3.32 2.84
6 4 0 71.45 6.76
-6 4 0 62.76 3.99
6 -4 0 72.63 3.98
-7 4 0 -3.92 2.53
7 -4 0 3.99 1.93
7 4 0 0.96 3.78
8 4 0 13.51 5.47
8 -4 0 16.56 2.70
10 4 0 546.88 88.43
-10 -4 0 417.05 65.69
11 4 0 6.12 7.61
12 4 0 6.58 9.12
0 -5 0 3.42 1.70
0 5 0 5.46 1.75
1 -5 0 -0.72 1.18
1 5 0 0.30 1.65
-1 5 0 0.64 0.89
1 5 0 -1.50 1.29
-1 5 0 0.71 1.60
2 -5 0 103.05 4.95
-2 5 0 107.43 5.62
2 5 0 110.74 6.03
2 5 0 108.76 6.00
3 5 0 0.83 1.93
3 5 0 -1.14 1.82
-3 5 0 0.60 1.55
-4 5 0 102.21 5.36
4 5 0 106.22 5.85
4 5 0 93.58 7.48
5 5 0 3.35 1.95
5 5 0 6.09 3.45
-5 5 0 0.72 1.62
6 5 0 351.12 13.17
6 5 0 349.01 16.91
-6 5 0 353.12 13.26
7 5 0 5.17 4.21
8 5 0 22.60 6.36
9 5 0 4.25 5.81
10 5 0 46.37 9.06
11 5 0 1.97 8.28
12 5 0 180.85 17.90
0 6 0 242.27 10.40
0 -6 0 234.31 9.77
0 6 0 241.20 9.65
1 6 0 -0.22 1.51
1 6 0 -1.89 1.45
-1 6 0 -0.96 1.02
1 -6 0 -0.13 1.49
-1 6 0 1.71 1.64
2 6 0 683.06 24.15
-2 6 0 570.26 24.74
2 6 0 655.24 23.65
-3 6 0 -1.04 2.04
3 6 0 0.29 1.66
3 6 0 -1.71 2.97
4 6 0 1091.36 38.61
-4 6 0 1136.38 38.56
4 6 0 1086.65 40.53
5 6 0 0.65 3.78
5 6 0 -2.42 1.74
-5 6 0 -1.08 2.23
-6 6 0 686.52 24.85
6 6 0 694.97 24.68
6 6 0 682.83 28.38
7 6 0 2.85 2.26
7 6 0 -2.76 4.83
-7 6 0 3.39 2.52
8 6 0 203.70 14.51
9 6 0 5.70 7.37
10 6 0 26.55 7.96
11 6 0 5.85 8.54
12 6 0 -9.09 9.68
0 7 0 10.81 1.78
1 -7 0 2.14 1.80
-1 7 0 -0.07 1.20
-1 7 0 -2.15 1.67
1 7 0 -1.63 1.66
1 7 0 0.69 2.01
2 -7 0 108.48 4.46
2 7 0 107.76 6.47
2 7 0 111.01 6.75
-2 7 0 107.15 6.31
3 7 0 0.40 1.66
-3 7 0 1.53 1.84
3 7 0 -1.62 3.09
-4 7 0 2497.11 83.18
4 7 0 2430.83 85.08
4 7 0 2447.50 83.27
5 7 0 -2.88 1.90
-5 7 0 3.78 2.17
5 7 0 1.03 4.25
6 7 0 164.72 8.31
6 7 0 176.12 12.36
-6 7 0 178.20 8.57
-7 7 0 4.84 2.60
7 7 0 3.71 5.02
7 7 0 3.33 2.10
8 7 0 218.35 15.01
-8 7 0 202.76 9.42
9 7 0 -1.35 6.66
10 7 0 99.06 14.06
11 7 0 12.08 9.10
0 8 0 2.98 1.93
0 8 0 2.99 2.11
1 8 0 -2.25 2.27
-1 8 0 -1.73 1.97
1 8 0 -4.19 1.84
1 -8 0 -3.78 2.23
2 8 0 273.28 12.49
2 -8 0 262.51 9.76
2 8 0 279.12 13.15
-2 8 0 277.96 12.30
3 8 0 2.65 2.05
3 8 0 0.82 3.72
-3 8 0 1.76 2.00
4 8 0 1510.80 55.12
-4 8 0 1540.96 53.35
4 8 0 1527.53 53.43
5 8 0 3.00 2.25
-5 8 0 0.01 2.28
5 8 0 -8.11 4.24
6 8 0 81.90 9.85
-6 8 0 84.73 6.13
6 8 0 90.45 6.08
-7 8 0 2.64 2.67
7 8 0 10.55 6.01
7 8 0 -0.97 2.24
8 8 0 12.13 7.50
9 8 0 6.26 7.60
10 8 0 50.54 10.22
11 8 0 -1.19 10.05
0 9 0 6.19 2.26
1 9 0 2.11 3.41
-1 9 0 -2.65 2.25
1 9 0 -2.25 2.47
2 9 0 153.53 9.60
2 9 0 159.93 9.11
-2 9 0 157.40 8.88
3 9 0 -0.84 3.80
3 9 0 3.83 2.68
-3 9 0 5.03 2.65
-4 9 0 417.35 17.70
4 9 0 410.40 17.77
4 9 0 438.68 19.62
-5 9 0 -0.94 2.84
5 9 0 -3.09 2.72
5 9 0 2.37 4.80
6 9 0 15.30 3.60
-6 9 0 10.57 3.38
6 9 0 14.65 6.06
7 9 0 4.42 6.77
7 9 0 -2.96 2.85
-7 9 0 -1.80 3.47
8 9 0 27.88 7.70
9 9 0 -8.87 7.66
10 9 0 -3.44 9.18
0 10 0 51.43 6.11
0 10 0 60.57 4.94
1 10 0 -3.31 3.23
1 10 0 -3.67 2.75
-1 10 0 0.47 2.82
2 10 0 723.73 28.21
2 10 0 711.43 28.01
-2 10 0 704.14 28.06
-3 10 0 4.63 3.19
3 10 0 -1.36 4.04
3 10 0 1.09 3.11
4 10 0 475.93 21.76
4 10 0 490.66 20.25
-4 10 0 457.98 20.05
-5 10 0 10.37 3.73
5 10 0 3.73 3.35
5 10 0 -6.68 5.46
6 10 0 42.97 6.42
6 10 0 33.52 12.95
-6 10 0 52.30 6.74
7 10 0 8.09 7.20
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-2 -4 -32 37.61 7.09
2 4 -32 41.97 10.03
2 4 -32 35.85 5.23
2 4 32 33.41 6.81
-2 4 -32 26.31 8.76
-2 4 -32 27.46 4.80
2 -4 -32 31.44 8.69
3 4 -32 3.51 4.52
-3 -4 -32 -0.95 6.15
3 4 -32 4.35 9.70
3 4 32 14.98 6.51
3 -4 -32 14.50 8.54
-3 4 -32 -1.20 3.64
-3 4 -32 3.95 7.78
-4 -4 -32 104.04 10.90
4 4 -32 96.68 14.01
4 4 -32 98.59 9.54
4 -4 -32 128.56 14.80
-4 4 -32 98.45 8.00
4 4 32 109.73 11.30
-4 4 -32 88.14 13.18
0 5 -32 5.50 4.05
0 5 32 -4.08 5.32
0 5 -32 -2.10 8.49
0 -5 -32 3.09 6.71
1 5 -32 138.95 9.66
-1 -5 -32 135.47 12.73
1 5 -32 165.65 16.78
-1 5 32 141.48 11.22
-1 5 -32 144.44 15.13
-1 5 -32 145.93 9.62
1 5 32 175.32 12.01
1 -5 -32 165.96 13.12
2 5 -32 153.43 9.94
2 5 -32 185.66 17.18
-2 -5 -32 165.23 12.63
-2 5 -32 162.85 15.60
2 -5 -32 136.26 14.77
2 5 32 154.50 12.48
-2 5 -32 121.38 9.29
3 5 -32 7.00 4.35
3 5 -32 15.75 10.19
-3 -5 -32 20.73 6.26
3 -5 -32 19.96 9.12
3 5 32 19.23 7.14
-3 5 -32 20.69 9.23
0 6 -32 184.16 11.04
0 -6 -32 203.53 14.71
0 6 32 202.97 13.21
0 6 -32 169.78 16.91
-1 6 32 4.06 5.82
-1 -6 -32 -7.67 6.30
1 6 -32 10.59 4.21
1 -6 -32 6.26 7.43
-1 6 -32 -6.33 8.99
-1 6 -32 5.43 4.01
1 6 32 -2.39 5.28
0 0 -33 7.68 7.32
1 0 -33 -7.69 7.37
-1 0 -33 -6.18 6.78
-2 0 -33 -2.56 6.93
2 0 -33 -7.80 8.09
-3 0 -33 3.69 6.81
3 0 -33 12.23 8.70
4 0 -33 7.33 9.69
-4 0 -33 -11.29 6.28
0 -1 -33 8.17 7.07
0 1 -33 -2.12 7.25
-1 -1 -33 94.28 11.58
1 1 -33 94.51 12.02
1 -1 -33 98.10 12.31
-1 1 -33 75.49 10.13
2 1 -33 13.14 8.19
-2 -1 -33 12.31 6.80
-2 1 -33 -11.96 6.40
2 -1 -33 -6.11 7.93
3 1 -33 221.11 18.34
-3 -1 -33 206.03 15.03
3 -1 -33 223.71 17.62
-3 1 -33 233.33 15.80
3 1 33 253.29 15.16
-4 -1 -33 32.78 7.13
4 1 -33 49.88 11.40
4 -1 -33 40.31 10.51
-4 1 -33 33.13 7.75
0 2 -33 26.25 5.23
0 -2 -33 28.99 7.77
0 2 -33 46.39 9.32
-1 -2 -33 19.60 7.09
1 2 -33 27.52 8.98
1 -2 -33 2.81 7.28
-1 2 -33 11.27 7.75
-1 2 -33 15.38 4.84
-2 -2 -33 43.78 8.00
2 2 -33 42.96 10.18
2 -2 -33 56.29 9.73
-2 2 -33 50.05 8.78
-2 2 -33 49.15 7.24
3 2 -33 -0.53 9.06
-3 -2 -33 -9.04 6.02
-3 2 -33 2.30 6.77
3 2 33 -3.72 6.28
-3 2 -33 -4.28 3.99
3 -2 -33 -7.50 8.72
-4 -2 -33 40.48 7.65
4 2 -33 33.45 11.27
-4 2 -33 33.06 8.78
-4 2 -33 54.60 7.33
4 -2 -33 19.95 9.59
0 -3 -33 -4.68 6.78
0 3 -33 -14.87 7.99
0 3 -33 8.45 4.09
1 3 -33 6.64 4.43
1 3 -33 36.19 9.68
-1 -3 -33 19.35 7.45
1 -3 -33 15.81 7.57
-1 3 -33 26.39 8.55
-1 3 -33 22.05 4.57
2 3 -33 2.72 4.54
-2 -3 -33 8.93 6.79
2 3 -33 15.52 9.26
-2 3 -33 5.39 3.87
2 -3 -33 9.13 8.57
2 3 33 18.51 6.47
-2 3 -33 1.65 7.72
3 3 -33 43.06 11.38
-3 -3 -33 39.80 7.80
3 3 33 28.79 7.37
-3 3 -33 31.94 8.73
-3 3 -33 22.11 4.73
3 -3 -33 25.39 9.77
-4 -3 -33 -2.76 6.23
4 3 -33 -2.47 9.96
-4 3 -33 -4.69 7.42
4 -3 -33 0.89 9.48
0 4 -33 -3.04 8.58
0 4 33 2.22 5.04
0 -4 -33 -3.17 7.24
0 4 -33 7.91 4.08
-1 -4 -33 7.85 7.00
1 4 -33 -2.74 8.96
1 4 -33 -0.27 4.10
-1 4 -33 3.01 8.96
1 4 33 -6.88 5.50
-1 4 -33 -6.28 3.81
1 -4 -33 -0.44 7.42
-2 -4 -33 51.75 8.56
2 4 -33 55.63 7.24
2 4 -33 67.64 11.18
2 4 33 54.90 7.86
-2 4 -33 57.60 7.01
2 -4 -33 55.72 10.53
-2 4 -33 56.32 9.87
3 4 -33 -2.05 4.44
-3 -4 -33 20.32 6.53
3 4 -33 4.01 9.96
-3 4 -33 6.09 4.11
3 4 33 13.89 6.86
-3 4 -33 3.43 8.09
3 -4 -33 9.36 8.85
0 -5 -33 0.92 7.11
0 5 -33 -0.76 9.30
0 5 -33 0.78 4.07
1 5 -33 37.20 5.30
-1 -5 -33 28.53 7.83
-1 5 33 24.56 6.11
1 5 -33 52.64 10.76
1 5 33 36.55 6.11
1 -5 -33 26.98 7.96
-1 5 -33 52.69 10.77
-1 5 -33 35.44 5.44
0 0 -34 116.03 13.48
-1 0 -34 86.29 11.33
1 0 -34 76.74 11.04
2 0 -34 56.29 10.71
3 0 -34 168.03 15.89
-3 0 -34 138.08 13.55
0 -1 -34 4.02 7.48
0 1 -34 7.01 8.20
1 1 -34 106.53 14.22
-1 -1 -34 126.10 12.60
-1 1 -34 124.99 13.01
1 -1 -34 120.29 13.93
2 1 -34 52.93 10.72
-2 -1 -34 46.67 8.77
2 -1 -34 50.68 10.07
-2 1 -34 35.59 8.84
3 1 -34 95.11 13.28
-3 -1 -34 130.07 12.48
3 1 34 121.91 11.69
-3 1 -34 117.37 12.45
3 -1 -34 117.18 15.41
0 2 -34 2.20 8.63
0 -2 -34 13.18 8.02
1 2 -34 33.91 9.04
-1 -2 -34 11.19 7.60
-1 2 -34 -7.82 7.68
1 -2 -34 2.17 8.30
-1 2 -34 9.33 4.35
-2 -2 -34 78.07 10.12
2 2 -34 73.80 12.33
-2 2 -34 58.74 9.98
-2 2 -34 78.25 8.04
2 2 34 86.93 10.73
2 -2 -34 68.19 10.57
-3 -2 -34 39.61 7.98
3 2 -34 25.62 9.89
3 2 34 40.62 7.76
3 -2 -34 42.23 10.53
-3 2 -34 37.10 8.34
-3 2 -34 61.00 7.78
0 3 -34 -8.59 8.89
0 -3 -34 9.36 7.28
1 3 -34 11.30 9.18
-1 -3 -34 17.53 7.34
1 3 -34 -2.03 4.33
1 -3 -34 -7.06 7.44
-1 3 -34 0.93 4.45
1 3 34 6.08 5.57
-1 3 -34 13.28 8.71
2 3 -34 1.78 4.33
-2 -3 -34 1.96 7.09
2 3 -34 -7.61 8.83
-2 3 -34 3.94 4.38
2 3 34 5.19 6.36
2 -3 -34 -4.78 8.05
-2 3 -34 3.19 8.15
0 4 34 66.16 9.25
0 -4 -34 61.76 9.65
0 4 -34 59.58 8.25
0 4 -34 84.68 12.04
0 0 -35 11.56 9.01
1 0 -35 -7.71 8.33
-1 0 -35 -9.69 7.33
0 1 -35 -1.45 8.45
-1 -1 -35 250.51 16.55
1 1 -35 223.83 17.95
1 -1 -35 225.52 16.96
-1 1 -35 204.40 16.57
0 -2 -35 2.22 7.70
0 0 0 0.00 0.00
_exptl_absorpt_process_details 'SADABS 2014/5'
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_max 0.7461
_exptl_absorpt_correction_T_min 0.6954
_exptl_special_details
)
The following wavelength and cell were deduced by SADABS from the
direction cosines etc. They are given here for emergency use only:
CELL 0.71073 9.439 10.411 24.743 90.004 90.035 89.986
)
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 40905
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
'x-1/2, y, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.66723(13) 0.96080(10) 0.55761(4) 0.0126(2) Uani 1 1 d . . . . .
C2 C 0.70159(12) 0.94328(10) 0.50386(4) 0.0121(2) Uani 1 1 d . . . . .
C3 C 0.62955(13) 0.85230(10) 0.47042(4) 0.0117(2) Uani 1 1 d . . . . .
C4 C 0.52122(13) 0.78110(10) 0.49606(5) 0.0139(2) Uani 1 1 d . . . . .
H4 H 0.469658 0.718666 0.476022 0.017 Uiso 1 1 calc R U . . .
C5 C 0.48954(13) 0.80096(10) 0.54951(4) 0.0139(2) Uani 1 1 d . . . . .
H5 H 0.415861 0.752016 0.565773 0.017 Uiso 1 1 calc R U . . .
C6 C 0.51967(14) 0.90743(12) 0.63704(4) 0.0173(2) Uani 1 1 d . . . . .
H6A H 0.483873 0.995152 0.642042 0.026 Uiso 1 1 calc R U . . .
H6B H 0.602676 0.894006 0.660251 0.026 Uiso 1 1 calc R U . . .
H6C H 0.445398 0.845602 0.646743 0.026 Uiso 1 1 calc R U . . .
C7 C 0.74235(15) 1.05827(12) 0.59171(5) 0.0195(3) Uani 1 1 d . . . . .
H7A H 0.819646 1.097080 0.570794 0.029 Uiso 1 1 calc R U . . .
H7B H 0.781373 1.016220 0.623926 0.029 Uiso 1 1 calc R U . . .
H7C H 0.675255 1.125362 0.602738 0.029 Uiso 1 1 calc R U . . .
N1 N 0.56054(11) 0.88862(9) 0.57980(4) 0.0127(2) Uani 1 1 d . . . . .
O1 O 0.80951(10) 1.01425(8) 0.48340(3) 0.0184(2) Uani 1 1 d . . . . .
H1O H 0.8060(19) 1.0123(17) 0.4482(7) 0.031(5) Uiso 1 1 d . . . . .
C8 C 0.93540(13) 1.08553(10) 0.34185(4) 0.0124(2) Uani 1 1 d . . . . .
C9 C 0.94223(13) 0.96060(10) 0.32084(4) 0.0132(2) Uani 1 1 d . . . . .
C10 C 1.04269(14) 0.93083(12) 0.28180(5) 0.0174(2) Uani 1 1 d . . . . .
H10 H 1.048064 0.845799 0.267849 0.021 Uiso 1 1 calc R U . . .
C11 C 1.13542(15) 1.02439(13) 0.26296(5) 0.0209(3) Uani 1 1 d . . . . .
H11 H 1.204309 1.003196 0.236352 0.025 Uiso 1 1 calc R U . . .
C12 C 1.12751(15) 1.14887(13) 0.28299(5) 0.0211(3) Uani 1 1 d . . . . .
H12 H 1.190219 1.213222 0.269816 0.025 Uiso 1 1 calc R U . . .
C13 C 1.02741(14) 1.17936(11) 0.32246(5) 0.0175(2) Uani 1 1 d . . . . .
H13 H 1.022025 1.264603 0.336171 0.021 Uiso 1 1 calc R U . . .
O2 O 0.66500(10) 0.83992(7) 0.42014(3) 0.01465(18) Uani 1 1 d . . . . .
O3 O 0.83552(10) 1.10809(8) 0.38077(3) 0.01516(18) Uani 1 1 d . . . . .
H3O H 0.843(2) 1.189(2) 0.3932(8) 0.051(6) Uiso 1 1 d . . . . .
O4 O 0.85051(10) 0.86689(8) 0.33754(3) 0.01696(19) Uani 1 1 d . . . . .
H4O H 0.797(2) 0.8911(17) 0.3634(7) 0.033(5) Uiso 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0116(6) 0.0116(5) 0.0148(5) 0.0009(4) -0.0011(4) -0.0001(4)
C2 0.0106(6) 0.0104(4) 0.0154(5) 0.0017(3) -0.0009(4) -0.0012(4)
C3 0.0118(6) 0.0085(4) 0.0147(5) 0.0001(3) -0.0011(4) 0.0023(4)
C4 0.0125(6) 0.0114(5) 0.0177(5) -0.0004(4) -0.0011(4) -0.0013(4)
C5 0.0112(6) 0.0113(5) 0.0191(5) 0.0020(4) 0.0010(4) -0.0007(4)
C6 0.0185(6) 0.0196(5) 0.0137(5) 0.0014(4) 0.0039(4) -0.0015(5)
C7 0.0216(7) 0.0217(6) 0.0151(5) -0.0024(4) -0.0003(5) -0.0084(5)
N1 0.0125(5) 0.0119(4) 0.0137(4) 0.0022(3) 0.0007(4) 0.0008(4)
O1 0.0192(5) 0.0212(4) 0.0147(4) 0.0000(3) 0.0022(3) -0.0103(4)
C8 0.0126(6) 0.0135(5) 0.0112(4) 0.0008(4) 0.0000(4) 0.0017(4)
C9 0.0138(6) 0.0133(5) 0.0123(4) 0.0000(4) -0.0022(4) 0.0006(4)
C10 0.0176(7) 0.0206(5) 0.0140(5) -0.0042(4) -0.0014(4) 0.0044(5)
C11 0.0171(7) 0.0307(7) 0.0149(5) 0.0000(4) 0.0034(5) 0.0027(5)
C12 0.0180(7) 0.0250(6) 0.0204(5) 0.0053(4) 0.0023(5) -0.0025(5)
C13 0.0186(7) 0.0148(5) 0.0192(5) 0.0020(4) 0.0015(5) -0.0016(5)
O2 0.0188(5) 0.0115(3) 0.0137(4) -0.0012(3) 0.0014(3) -0.0017(3)
O3 0.0191(5) 0.0100(4) 0.0164(4) -0.0015(3) 0.0056(3) 0.0004(3)
O4 0.0206(5) 0.0115(4) 0.0188(4) -0.0025(3) 0.0046(3) -0.0015(3)
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 119.07(10) . . ?
N1 C1 C7 119.53(10) . . ?
C2 C1 C7 121.39(10) . . ?
O1 C2 C1 117.64(10) . . ?
O1 C2 C3 120.12(10) . . ?
C1 C2 C3 122.23(10) . . ?
O2 C3 C4 124.49(10) . . ?
O2 C3 C2 119.96(10) . . ?
C4 C3 C2 115.56(10) . . ?
C5 C4 C3 120.77(10) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
N1 C5 C4 121.75(11) . . ?
N1 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 N1 C1 120.62(9) . . ?
C5 N1 C6 119.25(10) . . ?
C1 N1 C6 120.13(10) . . ?
C2 O1 H1O 109.3(12) . . ?
O3 C8 C13 123.51(10) . . ?
O3 C8 C9 116.88(10) . . ?
C13 C8 C9 119.61(11) . . ?
O4 C9 C10 118.88(10) . . ?
O4 C9 C8 121.35(10) . . ?
C10 C9 C8 119.77(11) . . ?
C9 C10 C11 120.46(11) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C12 C11 C10 120.00(12) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 119.88(12) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C8 C13 C12 120.27(11) . . ?
C8 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C8 O3 H3O 110.2(13) . . ?
C9 O4 H4O 112.9(12) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.3691(15) . ?
C1 C2 1.3797(15) . ?
C1 C7 1.4959(16) . ?
C2 O1 1.3542(14) . ?
C2 C3 1.4276(15) . ?
C3 O2 1.2933(13) . ?
C3 C4 1.4110(16) . ?
C4 C5 1.3700(16) . ?
C4 H4 0.9500 . ?
C5 N1 1.3559(14) . ?
C5 H5 0.9500 . ?
C6 N1 1.4792(14) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
O1 H1O 0.870(17) . ?
C8 O3 1.3660(14) . ?
C8 C13 1.3902(16) . ?
C8 C9 1.3999(15) . ?
C9 O4 1.3660(14) . ?
C9 C10 1.3868(17) . ?
C10 C11 1.3878(18) . ?
C10 H10 0.9500 . ?
C11 C12 1.3873(19) . ?
C11 H11 0.9500 . ?
C12 C13 1.3935(18) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
O3 H3O 0.90(2) . ?
O4 H4O 0.851(19) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1O O3 0.870(17) 1.963(17) 2.7289(11) 146.3(16) . yes
O3 H3O O2 0.90(2) 1.70(2) 2.5987(11) 172(2) 6_765 yes
O4 H4O O2 0.851(19) 1.950(19) 2.7024(12) 146.8(17) . yes
C5 H5 O2 0.95 2.57 3.4726(15) 158.0 2_466 yes
C6 H6C O4 0.98 2.41 3.3264(15) 154.7 2_466 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 O1 -178.68(10) . . . . ?
C7 C1 C2 O1 2.35(16) . . . . ?
N1 C1 C2 C3 0.04(17) . . . . ?
C7 C1 C2 C3 -178.93(11) . . . . ?
O1 C2 C3 O2 -1.74(16) . . . . ?
C1 C2 C3 O2 179.57(10) . . . . ?
O1 C2 C3 C4 178.45(10) . . . . ?
C1 C2 C3 C4 -0.24(16) . . . . ?
O2 C3 C4 C5 -179.45(11) . . . . ?
C2 C3 C4 C5 0.34(16) . . . . ?
C3 C4 C5 N1 -0.26(18) . . . . ?
C4 C5 N1 C1 0.04(17) . . . . ?
C4 C5 N1 C6 178.86(11) . . . . ?
C2 C1 N1 C5 0.07(16) . . . . ?
C7 C1 N1 C5 179.06(11) . . . . ?
C2 C1 N1 C6 -178.75(10) . . . . ?
C7 C1 N1 C6 0.24(16) . . . . ?
O3 C8 C9 O4 1.74(16) . . . . ?
C13 C8 C9 O4 -177.78(10) . . . . ?
O3 C8 C9 C10 -179.04(10) . . . . ?
C13 C8 C9 C10 1.44(17) . . . . ?
O4 C9 C10 C11 178.50(11) . . . . ?
C8 C9 C10 C11 -0.74(18) . . . . ?
C9 C10 C11 C12 -0.35(19) . . . . ?
C10 C11 C12 C13 0.7(2) . . . . ?
O3 C8 C13 C12 179.45(11) . . . . ?
C9 C8 C13 C12 -1.06(18) . . . . ?
C11 C12 C13 C8 -0.01(19) . . . . ?
_cod_database_fobs_code 2022891