#------------------------------------------------------------------------------
#$Date: 2023-06-29 17:53:46 +0200 (Thu, 29 Jun 2023) $
#$Revision: 284697 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022799.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_2022799
loop_
_publ_author_name
'Geetha, Doreswamy'
'Kavitha, Channappa N.'
'Divakara, Thayamma R.'
'Basavaraju, Yeriyur B.'
'Yathirajan, Hemmige S.'
'Parkin, Sean'
_publ_section_title
;
Crystal structure and Hirshfeld-surface analysis of a monoclinic
polymorph of 2-amino-5-chlorobenzophenone oxime at 90 K
;
_journal_coeditor_code TX2069
_journal_issue 7
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989023004668
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C13 H11 Cl N2 O'
_chemical_formula_moiety 'C13 H11 Cl N2 O'
_chemical_formula_sum 'C13 H11 Cl N2 O'
_chemical_formula_weight 246.69
_chemical_name_common
;
2-Amino-5-chlorobenzophenone oxime
;
_chemical_name_systematic
;
4-Chloro-2-[(hydroxyimino)(phenyl)methyl]aniline
;
_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 direct
_atom_sites_solution_secondary difmap
_audit_creation_method 'SHELXL-2019/2 and CIFFIX'
_cell_angle_alpha 90
_cell_angle_beta 109.5220(10)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.8264(3)
_cell_length_b 5.54230(10)
_cell_length_c 17.4082(4)
_cell_measurement_reflns_used 9975
_cell_measurement_temperature 90.0(2)
_cell_measurement_theta_max 27.53
_cell_measurement_theta_min 2.48
_cell_volume 1166.37(4)
_computing_cell_refinement
;
APEX3 (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
APEX3 (Bruker, 2016)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick,
2008)
;
_computing_publication_material
;
SHELX (Sheldrick, 2008) and publCIF (Westrip,
2010)'
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 90.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker D8 Venture dual source'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0420
_diffrn_reflns_av_unetI/netI 0.0222
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 26003
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.531
_diffrn_reflns_theta_min 2.404
_diffrn_source microsource
_exptl_absorpt_coefficient_mu 0.311
_exptl_absorpt_correction_T_max 0.971
_exptl_absorpt_correction_T_min 0.924
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour 'pale yellow'
_exptl_crystal_density_diffrn 1.405
_exptl_crystal_description 'semi-regular block'
_exptl_crystal_F_000 512
_exptl_crystal_size_max 0.300
_exptl_crystal_size_mid 0.240
_exptl_crystal_size_min 0.020
_refine_diff_density_max 0.320
_refine_diff_density_min -0.269
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.045
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 166
_refine_ls_number_reflns 2680
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.045
_refine_ls_R_factor_all 0.0429
_refine_ls_R_factor_gt 0.0333
_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^)+(0.0334P)^2^+0.6832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0781
_refine_ls_wR_factor_ref 0.0827
_reflns_number_gt 2294
_reflns_number_total 2680
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file tx2069sup1.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2022799
_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 0.913
_shelx_estimated_absorpt_t_max 0.994
_shelx_hkl_file
;
2 0 0 222.032 7.26447 5
2 0 0 221.892 6.82600 4
-2 0 0 216.120 7.31890 5
2 0 0 220.906 7.64959 1
2 0 0 213.809 7.49020 2
-2 0 0 225.490 6.85554 4
-2 0 0 217.836 7.36449 2
-2 0 0 224.482 7.76944 1
-3 0 0 1.01322 0.88824 2
-3 0 0 1.61781 0.94153 4
3 0 0 0.24469 0.92077 2
-3 0 0 0.34557 1.02249 1
3 0 0 2.00996 1.27222 5
3 0 0 1.21942 0.89530 4
-3 0 0 0.53695 1.05420 5
3 0 0 1.81234 1.39248 1
5 0 0 -0.6720 1.38177 4
5 0 0 1.95443 2.01154 2
-5 0 0 -0.2328 1.27334 4
-5 0 0 0.31298 1.54481 5
5 0 0 -0.2656 1.49162 1
-5 0 0 3.75639 1.85469 2
5 0 0 -0.1290 2.21754 5
-5 0 0 0.37423 1.67369 1
-6 0 0 189.005 10.9317 1
6 0 0 181.782 9.73567 5
-6 0 0 178.398 9.80242 2
6 0 0 190.903 9.13986 4
6 0 0 182.839 10.6131 1
6 0 0 184.399 10.6523 2
-6 0 0 186.217 10.2446 5
-6 0 0 184.851 9.01917 4
-7 0 0 -0.6088 2.42398 5
7 0 0 0.47533 2.34781 4
-7 0 0 15.5292 3.47911 4
7 0 0 3.89352 3.32416 2
7 0 0 2.60742 2.91342 5
-7 0 0 2.34769 3.02635 2
-7 0 0 1.86316 2.81766 1
7 0 0 3.60636 2.92264 1
8 0 0 60.2822 7.44231 1
8 0 0 61.6270 6.56213 4
8 0 0 77.2927 8.83840 2
-8 0 0 70.2721 6.60843 4
-8 0 0 74.2426 8.39882 5
-8 0 0 65.4437 7.97099 1
-8 0 0 73.6539 7.84957 2
8 0 0 78.6222 7.85711 5
9 0 0 1.55460 3.47602 4
9 0 0 1.17746 3.58365 1
-9 0 0 -3.2609 2.82754 4
-9 0 0 0.24795 4.71965 1
-9 0 0 -3.1079 4.14865 2
-9 0 0 4.24393 3.75757 5
9 0 0 6.11610 4.98454 2
9 0 0 3.46147 4.93084 5
10 0 0 176.472 13.6711 5
-10 0 0 205.925 16.2816 1
-10 0 0 176.165 13.2970 2
-10 0 0 200.474 13.9635 5
10 0 0 229.919 16.5378 2
10 0 0 187.091 12.1253 4
10 0 0 203.313 14.9468 1
-11 0 0 -8.9583 7.74709 1
11 0 0 -8.5883 6.12290 5
-11 0 0 0.54436 4.54996 5
-11 0 0 4.04385 6.11847 2
11 0 0 5.55348 6.71404 1
11 0 0 -1.5242 6.20150 2
11 0 0 3.42948 5.05512 4
12 0 0 69.6223 12.3289 1
-12 0 0 75.8948 11.4067 5
-12 0 0 84.9853 12.8290 2
12 0 0 74.5800 11.7879 5
12 0 0 67.5103 10.6826 4
-12 0 0 74.5381 12.4287 1
12 0 0 102.637 14.2366 2
12 0 0 91.9247 12.5443 5
-13 0 0 1.33519 9.11620 2
13 0 0 7.57131 7.32296 5
-13 0 0 4.83672 9.26705 1
-13 0 0 11.5462 8.36990 5
13 0 0 3.80079 8.29278 4
13 0 0 -11.143 8.42575 2
14 0 0 166.257 20.9940 2
-14 0 0 194.397 22.0301 1
14 0 0 158.514 21.1627 1
14 0 0 179.665 17.4339 5
-14 0 0 161.932 18.7989 5
14 0 0 190.275 19.1390 4
-15 0 0 0.36251 15.0710 1
15 0 0 -3.0134 12.2686 2
15 0 0 1.42452 10.2043 5
15 0 0 -7.0918 14.5593 1
0 -1 0 1.03110 0.72275 1
0 -1 0 -0.0592 0.45640 3
0 -1 0 1.40284 0.96146 2
0 1 0 -0.2564 0.88791 2
0 1 0 0.52285 0.54827 3
0 1 0 -0.4687 0.60300 5
0 1 0 1.17175 0.71928 1
-1 -1 0 910.406 23.9836 2
1 -1 0 849.777 21.3024 2
-1 -1 0 817.849 22.3656 1
-1 -1 0 851.477 21.3790 3
1 -1 0 857.512 21.5624 3
-1 -1 0 864.762 21.1737 5
1 -1 0 866.981 20.7797 5
1 -1 0 854.771 21.3733 1
1 1 0 860.428 22.6501 1
-1 1 0 858.491 21.2461 5
1 1 0 847.066 23.8612 2
1 1 0 871.385 21.3917 5
1 1 0 832.805 21.4258 3
-1 1 0 856.715 21.3615 1
-1 1 0 855.985 21.3402 3
-2 -1 0 1207.96 29.5924 5
-2 -1 0 1170.36 32.1966 2
2 -1 0 1217.96 28.4171 5
-2 -1 0 1178.05 30.2650 3
-2 -1 0 1178.64 31.0880 1
-2 1 0 1200.17 29.1077 5
2 1 0 1196.59 32.7632 2
2 1 0 1208.46 29.7888 5
-2 1 0 1179.11 30.2037 3
-2 1 0 1210.21 29.8990 4
-2 1 0 1197.37 29.5181 1
2 1 0 1182.45 31.1228 1
3 -1 0 509.500 14.3275 5
-3 -1 0 489.379 16.9626 1
3 -1 0 494.654 13.0886 2
-3 -1 0 511.974 15.6869 5
3 -1 0 504.995 15.0979 4
-3 -1 0 499.656 17.8800 2
3 1 0 527.049 15.9957 5
-3 1 0 505.789 15.1559 5
3 1 0 498.073 16.5965 4
-3 1 0 503.721 15.6296 1
3 1 0 519.388 18.6224 2
3 1 0 530.074 17.3069 1
-3 1 0 510.337 15.0902 4
-4 -1 0 285.641 11.2627 5
4 -1 0 282.329 9.11654 2
4 -1 0 271.968 9.82958 5
-4 -1 0 289.110 13.1602 2
4 -1 0 268.538 10.0813 4
-4 -1 0 272.548 12.3744 1
4 1 0 284.568 11.4182 5
-4 1 0 265.402 10.9744 1
4 1 0 254.961 11.3694 4
4 1 0 272.161 12.2672 1
-4 1 0 264.619 9.95309 4
4 1 0 268.696 13.4412 2
-4 1 0 276.379 10.9442 5
-5 -1 0 16.1986 4.19583 1
5 -1 0 8.55647 2.22809 2
5 -1 0 9.86164 2.45482 4
-5 -1 0 11.2974 2.70048 5
-5 -1 0 16.8274 4.60703 2
5 -1 0 14.3554 2.59589 5
5 1 0 12.7073 3.37967 1
-5 1 0 12.9224 3.21869 1
5 1 0 6.26307 3.22443 2
5 1 0 12.5924 2.90433 4
-5 1 0 8.67196 2.16768 4
-5 1 0 9.34630 2.10961 2
5 1 0 8.59144 2.97085 5
-6 -1 0 383.314 17.5995 1
-6 -1 0 386.289 15.9177 5
-6 -1 0 419.258 18.2164 2
6 -1 0 392.254 14.1900 4
6 -1 0 385.826 14.3030 5
6 -1 0 394.490 14.3478 2
6 1 0 398.701 19.1437 2
6 1 0 389.954 16.2904 5
-6 1 0 397.587 14.0163 4
-6 1 0 376.328 16.1555 1
6 1 0 401.364 17.6547 1
-6 1 0 383.198 13.3787 2
-6 1 0 420.480 16.4205 5
-7 -1 0 175.471 10.7951 5
7 -1 0 178.014 9.78234 2
7 -1 0 167.698 9.24177 4
-7 -1 0 160.172 11.5377 2
-7 -1 0 146.121 12.0204 1
-7 1 0 185.970 9.06630 2
-7 1 0 179.643 11.3099 5
-7 1 0 184.477 11.7063 1
7 1 0 172.646 10.3345 4
-7 1 0 177.204 8.97751 4
7 1 0 153.382 12.3615 2
7 1 0 190.083 11.9077 5
-8 -1 0 56.9983 8.68133 1
8 -1 0 83.7364 7.64618 5
8 -1 0 59.6458 7.05566 1
-8 -1 0 74.7094 8.10191 5
8 -1 0 69.9557 6.77947 4
-8 -1 0 70.3816 8.81055 2
8 -1 0 69.3939 7.49755 2
-8 1 0 61.6421 8.33230 1
8 1 0 65.2840 7.77427 4
8 1 0 72.3282 8.56895 5
-8 1 0 70.9005 6.21891 2
-8 1 0 70.6888 6.09267 4
8 1 0 63.2130 9.84471 2
-8 1 0 79.4685 8.46815 5
8 1 0 70.1545 8.68242 1
-9 -1 0 74.3754 9.21635 5
-9 -1 0 73.7159 9.86242 2
9 -1 0 70.4494 7.08911 4
9 -1 0 76.9299 8.25006 2
9 -1 0 64.9067 7.99832 1
9 -1 0 82.9211 8.37344 5
-9 -1 0 89.2388 10.7144 1
-9 1 0 65.3758 6.28057 4
-9 1 0 57.3764 6.51610 2
9 1 0 66.4741 9.20280 5
9 1 0 65.7278 8.74937 4
-9 1 0 73.0972 9.00135 1
9 1 0 66.4895 9.35212 1
9 1 0 84.4535 10.8510 2
-9 1 0 51.6319 7.70236 5
10 -1 0 68.4938 9.34571 2
-10 -1 0 38.5512 9.15633 2
-10 -1 0 65.7474 8.85143 5
10 -1 0 45.1619 6.93529 4
-10 -1 0 60.1863 9.85424 1
10 -1 0 61.8956 9.67308 1
10 -1 0 62.2368 8.56410 5
10 1 0 54.7145 9.17596 4
10 1 0 67.1552 10.3211 5
-10 1 0 38.1558 7.04240 5
10 1 0 56.7892 9.60852 1
10 1 0 62.2884 10.8135 2
-10 1 0 42.7053 6.61665 4
-10 1 0 56.4818 9.10596 1
-10 1 0 39.6039 6.79843 2
11 -1 0 1050.70 37.1303 2
11 -1 0 999.473 38.0566 1
-11 -1 0 920.615 38.1876 2
11 -1 0 1014.87 33.2287 5
-11 -1 0 1039.81 41.3090 1
11 -1 0 1007.33 32.7982 4
11 1 0 1102.23 39.5412 5
11 1 0 1025.66 40.0275 1
-11 1 0 1073.06 39.7878 1
11 1 0 994.516 35.3035 4
-11 1 0 1081.08 39.0301 5
-11 1 0 1016.70 32.3331 4
11 1 0 1090.90 44.0526 2
-11 1 0 1055.79 33.8839 2
-12 -1 0 62.9996 12.0362 1
12 -1 0 64.5085 10.3156 4
12 -1 0 72.4043 10.7581 5
12 -1 0 48.0230 8.08430 5
12 -1 0 34.8277 9.36916 1
12 -1 0 60.0018 10.9167 2
-12 -1 0 63.9621 10.4430 5
-12 1 0 85.0430 11.7536 5
12 1 0 60.9140 12.4683 1
-12 1 0 51.7625 9.29181 2
12 1 0 57.6335 10.2294 5
12 1 0 66.3212 13.7884 2
-12 1 0 58.4365 11.3704 1
12 1 0 47.4959 10.0225 4
13 -1 0 21.1918 7.87726 5
-13 -1 0 8.28461 7.05460 5
13 -1 0 17.6181 8.29267 2
13 -1 0 17.7682 9.25927 5
13 -1 0 13.4441 9.41069 1
13 -1 0 10.4286 7.80991 4
-13 -1 0 22.8714 11.9162 1
-13 1 0 18.8268 9.02514 2
13 1 0 20.5159 9.94362 4
13 1 0 30.5085 10.5170 1
13 1 0 27.8518 10.1124 5
-13 1 0 17.9057 10.5299 1
-13 1 0 20.9872 8.01906 5
14 -1 0 79.2800 13.7970 1
14 -1 0 68.9898 14.1836 2
-14 -1 0 92.3790 16.3127 1
14 -1 0 49.3234 10.6350 4
14 -1 0 84.8093 12.1563 5
14 1 0 59.6435 15.6315 1
-14 1 0 66.1947 13.2031 1
14 1 0 64.2063 15.0470 2
-14 1 0 48.2534 11.0290 5
14 1 0 70.5522 13.4046 5
14 1 0 81.2395 15.2653 4
-14 1 0 60.8638 13.0208 2
15 -1 0 81.9937 15.4131 2
-15 -1 0 72.3194 20.1352 1
-15 -1 0 72.7932 13.6778 5
15 -1 0 61.9128 10.8610 5
15 1 0 66.0072 15.0005 5
-15 1 0 69.8531 18.3279 1
15 1 0 52.5434 17.5862 2
15 1 0 62.5054 17.0248 1
0 -2 0 1166.14 32.7377 2
0 -2 0 1175.80 31.1027 1
0 -2 0 1136.39 29.1121 3
0 2 0 1139.33 29.2097 5
0 2 0 1171.69 29.5723 3
0 2 0 1141.84 31.3833 1
0 2 0 1146.78 33.1038 2
0 2 0 1212.00 31.4592 5
1 -2 0 2632.35 61.5883 3
1 -2 0 2663.18 63.4298 2
-1 -2 0 2594.30 61.1432 3
-1 -2 0 2592.38 60.6747 5
-1 -2 0 2596.45 63.6846 1
1 -2 0 2631.55 62.3196 1
-1 -2 0 2697.89 66.2091 2
1 2 0 2643.80 61.6834 5
1 2 0 2616.31 63.7931 5
-1 2 0 2621.97 62.5555 5
-1 2 0 2740.96 63.0150 1
1 2 0 2542.46 61.5569 3
1 2 0 2609.83 64.1784 1
-1 2 0 2686.88 63.8947 2
-1 2 0 2628.57 61.2614 3
1 2 0 2567.52 66.5376 2
2 -2 0 585.823 17.9731 2
2 -2 0 630.076 18.9975 3
-2 -2 0 584.474 17.6145 5
2 -2 0 585.948 16.5463 5
-2 -2 0 621.333 20.4338 1
-2 -2 0 579.381 21.6255 2
-2 -2 0 573.883 17.9697 3
2 2 0 598.586 22.4943 2
2 2 0 579.198 18.2716 5
2 2 0 593.516 20.2877 1
-2 2 0 596.707 18.0367 3
-2 2 0 619.994 18.5174 1
2 2 0 577.626 18.4838 3
-2 2 0 587.149 18.2658 5
-2 2 0 585.885 18.2805 1
2 2 0 623.163 20.2995 5
-3 -2 0 236.436 10.6886 3
3 -2 0 236.335 8.47938 5
3 -2 0 226.652 8.84732 2
-3 -2 0 244.328 12.2599 1
-3 -2 0 205.235 12.4521 2
-3 -2 0 229.568 10.0071 5
-3 2 0 237.047 10.4551 3
3 2 0 250.505 10.8047 5
3 2 0 250.146 12.1929 1
-3 2 0 235.422 10.1390 1
3 2 0 226.940 13.7505 2
-3 2 0 247.304 10.3546 1
-3 2 0 245.565 10.3644 5
3 2 0 226.053 11.5207 5
-3 2 0 248.718 11.4318 4
4 -2 0 1556.65 40.7622 1
-4 -2 0 1594.35 46.4560 2
-4 -2 0 1602.26 41.2896 5
4 -2 0 1532.17 37.5938 2
-4 -2 0 1562.93 44.4032 1
-4 -2 0 1540.85 42.3984 3
4 -2 0 1538.05 37.6789 5
4 2 0 1580.46 44.5035 1
4 2 0 1561.56 41.7749 5
4 2 0 1503.48 47.7832 2
-4 2 0 1556.42 41.6539 4
-4 2 0 1566.21 40.8479 5
-4 2 0 1552.14 41.1977 1
-4 2 0 1540.67 42.3968 3
-5 -2 0 23.0441 5.41025 2
5 -2 0 16.3451 2.26629 2
-5 -2 0 21.1051 4.82669 1
5 -2 0 19.1766 3.56766 1
-5 -2 0 23.7631 4.75289 3
5 -2 0 13.0266 2.61458 5
-5 -2 0 23.2806 4.22564 5
5 2 0 17.5110 4.41609 4
-5 2 0 19.7464 4.22066 3
5 2 0 18.7318 4.39530 5
5 2 0 18.2144 4.29710 1
-5 2 0 21.7870 3.97639 1
-5 2 0 20.9626 4.07974 4
5 2 0 30.9079 6.55019 2
-5 2 0 14.3025 3.45841 5
6 -2 0 80.3742 4.59552 2
-6 -2 0 87.8565 7.37338 5
-6 -2 0 77.9971 8.50787 1
6 -2 0 81.3588 6.92797 1
-6 -2 0 77.4413 7.83576 3
6 -2 0 70.8373 5.21791 5
-6 -2 0 83.7842 9.41702 2
-6 2 0 83.2032 6.87968 4
6 2 0 70.8567 7.70757 5
-6 2 0 66.1900 8.07994 3
6 2 0 70.9011 7.90948 4
6 2 0 69.5963 8.30865 1
-6 2 0 79.0858 7.07380 1
6 2 0 61.5981 9.21512 2
7 -2 0 378.471 13.5696 5
-7 -2 0 372.042 17.2656 5
7 -2 0 376.017 12.9930 2
-7 -2 0 351.849 20.2680 2
-7 -2 0 402.778 19.6209 3
7 -2 0 388.323 17.1181 1
-7 -2 0 394.524 20.0992 1
7 2 0 398.156 22.8764 2
7 2 0 375.062 19.4869 1
-7 2 0 390.970 17.3478 5
7 2 0 357.623 17.9276 4
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1 3 -19 62.9801 15.6125 1
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;
_shelx_hkl_checksum 64792
_shelx_res_file
;
TITL m22290 : space group P21/n
m22290.res
created by SHELXL-2019/2 at 14:59:18 on 13-May-2023
CELL 0.71073 12.8264 5.5423 17.4082 90.000 109.522 90.000
ZERR 4 0.0003 0.0001 0.0004 0.000 0.001 0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C H CL N O
UNIT 52 44 4 8 4
TEMP -183
SIZE 0.30 0.24 0.02
REM COLR pale yellow
REM FORM semi-regular block
L.S. 10
BOND $H
LIST 4
CONF
REM Instructions for potential hydrogen bonds.
HTAB N1 O1
EQIV $1 -x+1, -y+1, -z+1
HTAB O1 N2_$1
HTAB
REM Conformation defining torsions:
RTAB tors N1 C1 C6 C7
RTAB tors C1 C6 C7 N2
RTAB tors C6 C7 N2 O1
REM Dihedrals between rings:
MPLA C1 C2 C3 C4 C5 C6
MPLA C8 C9 c10 C11 C12 C13
REM
ACTA
FMAP 2
PLAN 20
REM EXTI 0.000000 not needed.
WGHT 0.033400 0.683200
FVAR 0.95040
CL1 3 0.632739 0.542490 0.941338 11.00000 0.03811 0.03352 =
0.01636 0.00155 0.00354 -0.00308
O1 5 0.582505 0.649600 0.573283 11.00000 0.01391 0.03990 =
0.02356 -0.00402 0.00968 -0.00072
H1O 2 0.582985 0.571825 0.524497 11.00000 0.05488
N1 4 0.581203 1.119608 0.644515 11.00000 0.03232 0.02440 =
0.03247 0.00569 0.01278 -0.00636
H1NA 2 0.569049 1.042418 0.596185 11.00000 0.03652
H1NB 2 0.630134 1.238378 0.652260 11.00000 0.04507
N2 4 0.470230 0.620126 0.566501 11.00000 0.01268 0.02824 =
0.02051 0.00023 0.00813 0.00079
C1 1 0.595504 0.978544 0.713260 11.00000 0.01715 0.01914 =
0.02691 0.00071 0.01055 0.00092
C2 1 0.664730 1.055540 0.790121 11.00000 0.01784 0.01989 =
0.03418 -0.00579 0.01068 -0.00416
AFIX 43
H2 2 0.705557 1.200830 0.794290 11.00000 -1.20000
AFIX 0
C3 1 0.674958 0.925614 0.859709 11.00000 0.01495 0.02615 =
0.02470 -0.00810 0.00512 -0.00122
AFIX 43
H3 2 0.720922 0.983038 0.911337 11.00000 -1.20000
AFIX 0
C4 1 0.617828 0.710921 0.853891 11.00000 0.01775 0.02352 =
0.01758 -0.00055 0.00575 0.00172
C5 1 0.547508 0.631102 0.779262 11.00000 0.01420 0.01777 =
0.01999 -0.00234 0.00633 -0.00095
AFIX 43
H5 2 0.507391 0.485190 0.776017 11.00000 -1.20000
AFIX 0
C6 1 0.535327 0.763846 0.708908 11.00000 0.01315 0.01825 =
0.01922 -0.00186 0.00690 0.00090
C7 1 0.451539 0.675329 0.632160 11.00000 0.01583 0.01670 =
0.01718 0.00199 0.00598 0.00181
C8 1 0.335907 0.643762 0.631015 11.00000 0.01525 0.01876 =
0.01349 0.00290 0.00571 0.00162
C9 1 0.291010 0.818211 0.668462 11.00000 0.01940 0.01911 =
0.01911 -0.00095 0.00769 -0.00073
AFIX 43
H9 2 0.335250 0.950014 0.695888 11.00000 -1.20000
AFIX 0
C10 1 0.182019 0.800256 0.665867 11.00000 0.02086 0.02460 =
0.02601 -0.00010 0.01284 0.00292
AFIX 43
H10 2 0.151395 0.920969 0.690712 11.00000 -1.20000
AFIX 0
C11 1 0.117817 0.606153 0.627015 11.00000 0.01582 0.02954 =
0.02482 0.00528 0.00858 -0.00031
AFIX 43
H11 2 0.043042 0.594435 0.624967 11.00000 -1.20000
AFIX 0
C12 1 0.162491 0.429216 0.591166 11.00000 0.02108 0.02399 =
0.02165 0.00024 0.00554 -0.00586
AFIX 43
H12 2 0.118668 0.294962 0.565375 11.00000 -1.20000
AFIX 0
C13 1 0.271406 0.447687 0.592846 11.00000 0.02066 0.01967 =
0.01707 0.00012 0.00732 0.00032
AFIX 43
H13 2 0.301768 0.326585 0.567964 11.00000 -1.20000
AFIX 0
HKLF 4
REM m22290 : space group P21/n
REM wR2 = 0.0827, GooF = S = 1.045, Restrained GooF = 1.045 for all data
REM R1 = 0.0333 for 2294 Fo > 4sig(Fo) and 0.0429 for all 2680 data
REM 166 parameters refined using 0 restraints
END
WGHT 0.0334 0.6832
REM Instructions for potential hydrogen bonds
HTAB O1 O1_$1
HTAB O1 N2_$1
HTAB N1 O1
HTAB N1 N2
EQIV $2 x, y+1, z
HTAB N1 O1_$2
EQIV $3 -x+3/2, y+1/2, -z+3/2
HTAB C3 O1_$3
REM Highest difference peak 0.320, deepest hole -0.269, 1-sigma level 0.046
Q1 1 0.3921 0.6553 0.6318 11.00000 0.05 0.32
Q2 1 0.4937 0.7195 0.6717 11.00000 0.05 0.30
Q3 1 0.6413 0.9928 0.7511 11.00000 0.05 0.27
Q4 1 0.5757 0.8527 0.7103 11.00000 0.05 0.27
Q5 1 0.5757 0.6861 0.8181 11.00000 0.05 0.26
Q6 1 0.3154 0.5120 0.6300 11.00000 0.05 0.25
Q7 1 0.4182 0.5771 0.5207 11.00000 0.05 0.25
Q8 1 0.4546 1.0517 0.5618 11.00000 0.05 0.24
Q9 1 0.5330 0.7300 0.7501 11.00000 0.05 0.24
Q10 1 0.2311 0.8134 0.6569 11.00000 0.05 0.24
Q11 1 0.1584 0.6802 0.6505 11.00000 0.05 0.23
Q12 1 0.6934 0.9275 0.8195 11.00000 0.05 0.22
Q13 1 0.3184 0.7091 0.6566 11.00000 0.05 0.22
Q14 1 0.3005 0.5867 0.5995 11.00000 0.05 0.22
Q15 1 0.1491 0.4759 0.6272 11.00000 0.05 0.22
Q16 1 0.1379 0.5540 0.5963 11.00000 0.05 0.21
Q17 1 0.3049 0.7566 0.6337 11.00000 0.05 0.21
Q18 1 0.6605 0.7792 0.8500 11.00000 0.05 0.19
Q19 1 0.2150 0.4412 0.5948 11.00000 0.05 0.19
Q20 1 0.6040 1.0027 0.6794 11.00000 0.05 0.19
;
_shelx_res_checksum 30655
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
Cl Cl1 0.63274(3) 0.54249(7) 0.94134(2) 0.03072(12) Uani d 1 . .
O O1 0.58250(8) 0.6496(2) 0.57328(6) 0.0249(2) Uani d 1 . .
H H1O 0.5830(17) 0.572(4) 0.5245(14) 0.055(6) Uiso d 1 . .
N N1 0.58120(12) 1.1196(3) 0.64451(9) 0.0292(3) Uani d 1 . .
H H1NA 0.5690(15) 1.042(4) 0.5962(12) 0.037(5) Uiso d 1 . .
H H1NB 0.6301(17) 1.238(4) 0.6523(12) 0.045(6) Uiso d 1 . .
N N2 0.47023(9) 0.6201(2) 0.56650(7) 0.0198(3) Uani d 1 . .
C C1 0.59550(11) 0.9785(3) 0.71326(9) 0.0203(3) Uani d 1 . .
C C2 0.66473(11) 1.0555(3) 0.79012(9) 0.0235(3) Uani d 1 . .
H H2 0.705557 1.200830 0.794290 0.028 Uiso calc 1 . .
C C3 0.67496(11) 0.9256(3) 0.85971(9) 0.0223(3) Uani d 1 . .
H H3 0.720922 0.983038 0.911337 0.027 Uiso calc 1 . .
C C4 0.61783(11) 0.7109(3) 0.85389(8) 0.0197(3) Uani d 1 . .
C C5 0.54751(10) 0.6311(3) 0.77926(8) 0.0172(3) Uani d 1 . .
H H5 0.507391 0.485190 0.776017 0.021 Uiso calc 1 . .
C C6 0.53533(10) 0.7638(3) 0.70891(8) 0.0165(3) Uani d 1 . .
C C7 0.45154(10) 0.6753(2) 0.63216(8) 0.0165(3) Uani d 1 . .
C C8 0.33591(10) 0.6438(2) 0.63101(7) 0.0156(3) Uani d 1 . .
C C9 0.29101(11) 0.8182(3) 0.66846(8) 0.0189(3) Uani d 1 . .
H H9 0.335250 0.950014 0.695888 0.023 Uiso calc 1 . .
C C10 0.18202(11) 0.8003(3) 0.66587(9) 0.0226(3) Uani d 1 . .
H H10 0.151395 0.920969 0.690712 0.027 Uiso calc 1 . .
C C11 0.11782(11) 0.6062(3) 0.62701(9) 0.0229(3) Uani d 1 . .
H H11 0.043042 0.594435 0.624967 0.028 Uiso calc 1 . .
C C12 0.16249(12) 0.4292(3) 0.59117(9) 0.0226(3) Uani d 1 . .
H H12 0.118668 0.294962 0.565375 0.027 Uiso calc 1 . .
C C13 0.27141(11) 0.4477(3) 0.59285(8) 0.0189(3) Uani d 1 . .
H H13 0.301768 0.326585 0.567964 0.023 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
Cl1 0.0381(2) 0.0335(2) 0.01636(17) -0.00308(17) 0.00354(14) 0.00155(15)
O1 0.0139(5) 0.0399(7) 0.0236(5) -0.0007(4) 0.0097(4) -0.0040(5)
N1 0.0323(7) 0.0244(7) 0.0325(7) -0.0064(6) 0.0128(6) 0.0057(6)
N2 0.0127(5) 0.0282(7) 0.0205(6) 0.0008(5) 0.0081(4) 0.0002(5)
C1 0.0172(6) 0.0191(7) 0.0269(7) 0.0009(5) 0.0105(5) 0.0007(6)
C2 0.0178(6) 0.0199(7) 0.0342(8) -0.0042(6) 0.0107(6) -0.0058(6)
C3 0.0149(6) 0.0262(8) 0.0247(7) -0.0012(5) 0.0051(5) -0.0081(6)
C4 0.0177(6) 0.0235(7) 0.0176(6) 0.0017(5) 0.0057(5) -0.0005(5)
C5 0.0142(6) 0.0178(7) 0.0200(6) -0.0010(5) 0.0063(5) -0.0023(5)
C6 0.0132(6) 0.0182(7) 0.0192(6) 0.0009(5) 0.0069(5) -0.0019(5)
C7 0.0158(6) 0.0167(7) 0.0172(6) 0.0018(5) 0.0060(5) 0.0020(5)
C8 0.0153(6) 0.0188(7) 0.0135(6) 0.0016(5) 0.0057(5) 0.0029(5)
C9 0.0194(6) 0.0191(7) 0.0191(6) -0.0007(5) 0.0077(5) -0.0010(5)
C10 0.0209(7) 0.0246(8) 0.0260(7) 0.0029(6) 0.0128(6) -0.0001(6)
C11 0.0158(6) 0.0295(8) 0.0248(7) -0.0003(6) 0.0086(5) 0.0053(6)
C12 0.0211(7) 0.0240(8) 0.0216(7) -0.0059(6) 0.0055(5) 0.0002(6)
C13 0.0207(6) 0.0197(7) 0.0171(6) 0.0003(5) 0.0073(5) 0.0001(5)
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'
Cl Cl 0.1484 0.1585 '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
N2 O1 H1O . . 100.5(13) ?
C1 N1 H1NA . . 117.7(13) ?
C1 N1 H1NB . . 113.8(13) ?
H1NA N1 H1NB . . 112.5(17) ?
C7 N2 O1 . . 112.76(11) ?
N1 C1 C2 . . 120.65(14) ?
N1 C1 C6 . . 121.17(13) ?
C2 C1 C6 . . 118.03(13) ?
C3 C2 C1 . . 121.59(13) ?
C3 C2 H2 . . 119.2 ?
C1 C2 H2 . . 119.2 ?
C2 C3 C4 . . 119.53(13) ?
C2 C3 H3 . . 120.2 ?
C4 C3 H3 . . 120.2 ?
C3 C4 C5 . . 120.47(13) ?
C3 C4 Cl1 . . 119.77(11) ?
C5 C4 Cl1 . . 119.76(11) ?
C4 C5 C6 . . 120.23(13) ?
C4 C5 H5 . . 119.9 ?
C6 C5 H5 . . 119.9 ?
C5 C6 C1 . . 120.10(12) ?
C5 C6 C7 . . 116.75(12) ?
C1 C6 C7 . . 123.03(12) ?
N2 C7 C8 . . 116.31(12) ?
N2 C7 C6 . . 125.78(12) ?
C8 C7 C6 . . 117.90(11) ?
C13 C8 C9 . . 119.48(12) ?
C13 C8 C7 . . 121.94(12) ?
C9 C8 C7 . . 118.58(12) ?
C10 C9 C8 . . 120.30(13) ?
C10 C9 H9 . . 119.9 ?
C8 C9 H9 . . 119.9 ?
C11 C10 C9 . . 119.97(13) ?
C11 C10 H10 . . 120.0 ?
C9 C10 H10 . . 120.0 ?
C12 C11 C10 . . 120.11(13) ?
C12 C11 H11 . . 119.9 ?
C10 C11 H11 . . 119.9 ?
C11 C12 C13 . . 120.14(13) ?
C11 C12 H12 . . 119.9 ?
C13 C12 H12 . . 119.9 ?
C12 C13 C8 . . 119.98(13) ?
C12 C13 H13 . . 120.0 ?
C8 C13 H13 . . 120.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cl1 C4 . 1.7409(14) ?
O1 N2 . 1.4145(14) ?
O1 H1O . 0.95(2) ?
N1 C1 . 1.3894(19) ?
N1 H1NA . 0.91(2) ?
N1 H1NB . 0.89(2) ?
N2 C7 . 1.2809(17) ?
C1 C2 . 1.402(2) ?
C1 C6 . 1.4065(19) ?
C2 C3 . 1.377(2) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.383(2) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.3834(18) ?
C5 C6 . 1.3920(19) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.4903(18) ?
C7 C8 . 1.4869(17) ?
C8 C13 . 1.3927(19) ?
C8 C9 . 1.3937(19) ?
C9 C10 . 1.3871(18) ?
C9 H9 . 0.9500 ?
C10 C11 . 1.386(2) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.385(2) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.3913(19) ?
C12 H12 . 0.9500 ?
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
N1 H1NA O1 . 0.91(2) 2.23(2) 2.8875(19) 128.7(16) yes
O1 H1O N2 3_666 0.95(2) 1.84(2) 2.7411(16) 156.4(19) 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
N1 C1 C2 C3 . . . . 176.07(13) ?
C6 C1 C2 C3 . . . . 0.5(2) ?
C1 C2 C3 C4 . . . . 1.5(2) ?
C2 C3 C4 C5 . . . . -2.5(2) ?
C2 C3 C4 Cl1 . . . . 178.60(11) ?
C3 C4 C5 C6 . . . . 1.4(2) ?
Cl1 C4 C5 C6 . . . . -179.73(10) ?
C4 C5 C6 C1 . . . . 0.7(2) ?
C4 C5 C6 C7 . . . . -175.41(12) ?
N1 C1 C6 C5 . . . . -177.17(13) ?
C2 C1 C6 C5 . . . . -1.63(19) ?
N1 C1 C6 C7 . . . . -1.3(2) ?
C2 C1 C6 C7 . . . . 174.25(12) ?
O1 N2 C7 C8 . . . . -178.54(11) ?
O1 N2 C7 C6 . . . . 0.5(2) ?
C5 C6 C7 N2 . . . . -123.16(15) ?
C1 C6 C7 N2 . . . . 60.8(2) ?
C5 C6 C7 C8 . . . . 55.87(17) ?
C1 C6 C7 C8 . . . . -120.15(14) ?
N2 C7 C8 C13 . . . . 39.36(18) ?
C6 C7 C8 C13 . . . . -139.76(13) ?
N2 C7 C8 C9 . . . . -139.76(13) ?
C6 C7 C8 C9 . . . . 41.12(17) ?
C13 C8 C9 C10 . . . . -1.7(2) ?
C7 C8 C9 C10 . . . . 177.41(12) ?
C8 C9 C10 C11 . . . . 1.0(2) ?
C9 C10 C11 C12 . . . . 0.4(2) ?
C10 C11 C12 C13 . . . . -1.1(2) ?
C11 C12 C13 C8 . . . . 0.3(2) ?
C9 C8 C13 C12 . . . . 1.05(19) ?
C7 C8 C13 C12 . . . . -178.07(12) ?
_cod_database_fobs_code 2022799