#------------------------------------------------------------------------------
#$Date: 2025-05-14 03:05:04 +0100 (Wed, 14 May 2025) $
#$Revision: 299654 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/35/2023509.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_2023509
loop_
_publ_author_name
'O'Connor, Molly A.'
'Pavlishchuk, Anna V.'
'Butcher, Raymond J.'
'Pavlishchuk, Vitaly V.'
'Addison, Anthony W.'
_publ_section_title
;
Some thioether-ketones and their related derivatives
;
_journal_issue 6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989025004037
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac 'C10 H18 N4 S3'
_chemical_formula_moiety 'C10 H18 N4 S3'
_chemical_formula_sum 'C10 H18 N4 S3'
_chemical_formula_weight 290.46
_chemical_name_systematic
(3E,8Z)-3,9-Dimethyl-1,11-dithia-4,5,7,8-tetraazacyclotetradeca-3,8-diene-6-thione
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 92.195(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.1219(3)
_cell_length_b 8.6565(2)
_cell_length_c 17.7935(7)
_cell_measurement_reflns_used 50347
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 78.6310
_cell_measurement_theta_min 4.8330
_cell_volume 1404.01(8)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0529
_diffrn_reflns_av_unetI/netI 0.0134
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 75253
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 78.925
_diffrn_reflns_theta_min 4.852
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 4.704
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.68317
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour 'pale yellow'
_exptl_crystal_density_diffrn 1.374
_exptl_crystal_description block
_exptl_crystal_F_000 616
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.34
_exptl_crystal_size_min 0.20
_refine_diff_density_max 0.218
_refine_diff_density_min -0.277
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.082
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 164
_refine_ls_number_reflns 2983
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.082
_refine_ls_R_factor_all 0.0321
_refine_ls_R_factor_gt 0.0307
_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^)+(0.0445P)^2^+0.3926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0854
_refine_ls_wR_factor_ref 0.0865
_reflns_number_gt 2806
_reflns_number_total 2983
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jy2055.cif
_cod_data_source_block Ctrsp
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2023509
_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 1 5.02401 5.50615 43
0 0 1 20.4415 7.37877 32
0 0 1 3.66403 4.79154 36
0 0 -2 2563.65 140.365 9
0 0 2 2452.18 139.232 43
0 0 2 2572.56 137.120 42
0 0 2 2428.34 136.295 21
0 0 -2 2225.27 128.774 35
0 0 2 2285.23 136.152 36
0 0 3 18.0156 29.4918 21
0 0 -3 58.3351 29.1502 22
0 0 4 7845.36 418.291 43
0 0 -4 7590.97 408.878 22
0 0 4 8155.25 415.310 21
0 0 -4 7966.04 400.881 29
0 0 -4 8156.18 402.839 35
0 0 4 8262.91 420.116 36
0 0 5 67.6717 40.4830 43
0 0 -5-5.96561 28.6275 22
0 0 5 6.17831 33.5054 21
0 0 -5 58.6255 32.2145 29
0 0 -5 24.8346 25.7506 35
0 0 5 52.1490 33.7787 36
0 0 -6 765561. 33198.8 41
0 0 6 759251. 33214.3 43
0 0 -6 781735. 33200.2 22
0 0 6 762835. 33202.5 21
0 0 6 741066. 33203.3 26
0 0 -6 766689. 33177.8 29
0 0 6 783013. 33211.6 36
0 0 -6 757799. 33176.3 35
0 0 7 68.1991 55.1416 40
0 0 -7 230.397 67.9914 41
0 0 7 38.4310 52.1678 26
0 0 7 45.4582 54.4589 21
0 0 -7 90.0274 51.9738 22
0 0 -7 57.2466 39.7455 30
0 0 -7 50.5639 41.7462 29
0 0 7 48.9302 54.2707 36
0 0 -7 43.6750 37.8324 35
0 0 8 70284.6 3327.96 40
0 0 8 75211.4 3346.29 43
0 0 -8 70162.3 3306.34 41
0 0 8 73642.7 3338.07 36
0 0 -8 73488.1 3291.09 35
0 0 -8 72766.9 3285.86 30
0 0 -8 74142.4 3291.30 29
0 0 8 70804.5 3322.73 26
0 0 -8 74284.9 3321.73 22
0 0 8 75476.6 3326.17 21
0 0 9-14.2559 70.2413 43
0 0 9 123.178 81.8565 40
0 0 -9 12.0245 50.8717 41
0 0 -9 14.3702 30.6712 75
0 0 9 43.8109 36.1277 88
0 0 9 117.361 44.3254 86
0 0 9-27.2875 65.4351 36
0 0 -9 29.7447 40.4354 35
0 0 9 10.0259 38.4609 65
0 0 -9 113.041 36.1735 68
0 0 -9 29.9595 34.3675 69
0 0 -9 43.7905 33.4914 59
0 0 9 29.8053 33.7272 63
0 0 9 224.449 83.3794 21
0 0 -9 63.5685 60.9781 22
0 0 9 130.212 70.5884 26
0 0 -9 60.1932 35.4428 53
0 0 9 22.4302 36.9911 89
0 0 -9 52.6305 37.1086 92
0 0 -9 39.2469 45.7487 30
0 0 -9 29.9953 46.6180 29
0 0 10 110830. 4464.99 89
0 0 -10 102198. 4442.03 92
0 0 10 102047. 4441.28 82
0 0 10 95686.0 4430.04 80
0 0 10 103515. 4609.36 43
0 0 -10 100325. 4560.26 41
0 0 10 102691. 4597.96 40
0 0 10 105022. 4457.31 88
0 0 10 97499.2 4445.31 86
0 0 -10 100618. 4441.45 75
0 0 -10 99741.1 4429.31 76
0 0 10 106580. 4605.60 36
0 0 -10 99602.5 4524.96 35
0 0 -10 96366.9 4441.58 69
0 0 -10 101680. 4435.08 68
0 0 10 99503.4 4443.19 65
0 0 10 100756. 4444.86 63
0 0 -10 100236. 4441.98 59
0 0 -10 96648.1 4441.93 53
0 0 10 98977.4 4437.00 47
0 0 -10 100903. 4431.34 51
0 0 -10 103603. 4531.76 30
0 0 -10 104612. 4536.11 29
0 0 10 97910.9 4582.23 26
0 0 10 93348.7 4559.78 24
0 0 -10 104915. 4584.86 22
0 0 10 106666. 4586.86 21
0 0 11 108.104 44.5908 80
0 0 -11 230.537 51.4947 83
0 0 11 26.1299 41.8071 81
0 0 11 50.0480 41.2713 82
0 0 11 36.6770 82.9156 40
0 0 11 38.0903 77.6222 43
0 0 -11 31.2031 55.7878 41
0 0 -11 138.177 52.6746 75
0 0 -11 33.4196 32.8793 78
0 0 -11-16.8110 33.5688 76
0 0 11 54.2883 46.0547 86
0 0 11-14.2763 42.7309 88
0 0 -11 25.5745 56.0004 35
0 0 11 36.2736 82.0041 36
0 0 -11 17.7754 34.2010 68
0 0 -11 117.719 50.1639 69
0 0 11 52.3215 46.7858 63
0 0 11 16.5676 52.9916 24
0 0 11 16.3678 66.7183 21
0 0 -11 17.1833 64.4319 22
0 0 11-16.9429 63.5312 26
0 0 -11 13.1608 38.6917 53
0 0 -11 33.5219 36.3246 51
0 0 11 125.979 47.0099 47
0 0 11-7.30876 42.9631 89
0 0 -11 6.40212 48.0311 92
0 0 -11 239.286 82.3038 29
0 0 -11 51.3539 50.2970 30
0 0 12 22566.3 1053.16 89
0 0 -12 22227.1 1035.45 92
0 0 12 21681.8 1044.20 88
0 0 12 20186.2 1032.63 86
0 0 12 20437.5 1196.25 40
0 0 12 22188.8 1222.28 43
0 0 -12 21856.2 1166.74 41
0 0 -12 20875.4 1007.28 83
0 0 12 20585.9 1031.87 81
0 0 12 20724.6 1015.16 80
0 0 12 22182.9 1030.39 82
0 0 -12 20152.6 999.091 78
0 0 -12 22138.4 1020.25 76
0 0 -12 21853.8 1030.93 75
0 0 12 20904.0 1211.56 39
0 0 -12 21405.5 1121.88 35
0 0 -12 21405.5 1034.82 69
0 0 -12 21098.7 1022.09 68
0 0 12 22504.9 1041.65 65
0 0 12 20488.7 1031.77 63
0 0 -12 21457.1 1033.26 53
0 0 12 20357.8 1018.20 47
0 0 -12 21610.0 1016.88 51
0 0 -12 21512.0 1132.62 29
0 0 12 22903.8 1199.59 26
0 0 -12 21609.6 1130.16 30
0 0 12 23441.0 1196.23 24
0 0 -12 21225.4 1189.61 22
0 0 12 22608.6 1192.18 21
0 0 13-18.0936 56.9288 89
0 0 -13 49.2538 54.8888 92
0 0 13 17.0666 52.8258 86
0 0 13 8.76199 48.5169 88
0 0 13-23.2290 83.0132 40
0 0 -13 19.2811 57.6547 41
0 0 13 24.1265 72.1391 43
0 0 13-28.9602 44.0703 47
0 0 13 490.353 87.6050 81
0 0 -13 75.4605 46.0637 83
0 0 13 22.8967 41.3750 82
0 0 13 33.3937 36.2097 80
0 0 -13 374.750 61.8150 84
0 0 -13-7.88903 38.8725 75
0 0 -13 5.75737 33.8220 78
0 0 -13-7.04375 49.7182 14
0 0 -13 15.8011 45.5347 17
0 0 13 48.0766 94.1028 39
0 0 -13 353.105 96.5971 35
0 0 13 8.20637 54.0822 65
0 0 -13-8.22839 51.7806 69
0 0 -13 363.811 72.6669 68
0 0 13-16.4458 48.2940 63
0 0 -13-7.01409 48.2234 10
0 0 13-42.7129 80.0469 26
0 0 -13 419.105 136.528 22
0 0 13 20.5023 76.8459 24
0 0 13 7.15973 37.9627 20
0 0 -13 16.5525 41.8378 53
0 0 -13 13.9212 35.1915 51
0 0 -13 64.3473 65.5510 29
0 0 -13 31.1825 58.4426 30
0 0 13 19.7647 77.3751 27
0 0 -14 11728.7 606.675 10
0 0 14 12404.4 641.806 89
0 0 14 11535.7 623.810 86
0 0 14 12330.5 635.542 88
0 0 14 11763.7 811.809 40
0 0 14 10471.3 589.133 45
0 0 14 10904.0 801.803 43
0 0 -14 12242.1 767.396 41
0 0 -14 12293.0 625.234 17
0 0 -14 11441.0 604.634 14
0 0 14 11039.1 604.749 82
0 0 -14 11076.7 587.188 83
0 0 14 10598.5 614.983 81
0 0 -14 11714.3 616.616 75
0 0 -14 11300.2 599.411 76
0 0 14 11881.7 826.005 39
0 0 -14 11324.9 619.233 69
0 0 14 11717.9 620.448 65
0 0 -14 12053.1 613.057 68
0 0 14 11500.7 618.635 63
0 0 -14 11420.1 620.332 53
0 0 -14 11438.3 600.858 51
0 0 14 10648.6 595.213 47
0 0 14 11418.8 773.051 26
0 0 14 11152.8 759.405 27
0 0 14 11278.7 770.246 24
0 0 -14 11580.1 795.196 22
0 0 14 11149.6 600.830 20
0 0 15 39.4006 57.8384 86
0 0 15-9.88619 55.8587 88
0 0 15 27.2869 97.5076 40
0 0 -15 21.8987 60.6156 41
0 0 15 7.76964 43.0137 47
0 0 15 28.0611 95.1283 43
0 0 15 30.9225 64.8519 89
0 0 -15 21.0525 38.8501 83
0 0 15-9.70234 55.9056 81
0 0 15 8.37369 44.3841 82
0 0 -15 9.23334 45.4814 75
0 0 -15-16.0082 48.7089 76
0 0 -15-18.4979 55.3049 17
0 0 -15 48.7677 57.3595 14
0 0 15 28.3702 96.1763 39
0 0 -15-17.2121 41.2613 68
0 0 -15 19.3112 57.7363 69
0 0 15 27.9687 50.5254 65
0 0 15 121.982 61.8276 63
0 0 -15 102.348 67.1677 10
0 0 -15-25.8958 77.4221 22
0 0 15-24.7786 68.5868 26
0 0 15 47.1134 84.1783 24
0 0 15-8.06069 48.2000 20
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0 0 -15 7.95627 44.0468 51
0 0 -15-9.70698 51.4505 53
0 0 15-22.7713 77.1960 27
0 0 -16 19046.0 941.867 52
0 0 -16 18194.2 913.152 51
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0 0 -16 16751.7 891.538 83
0 0 16 17236.1 911.033 82
0 0 16 17885.9 1163.16 43
0 0 16 17475.6 1146.21 40
0 0 -16 18424.6 915.470 76
0 0 -16 19123.7 938.285 75
0 0 16 18731.4 944.889 88
0 0 16 18773.4 944.777 86
0 0 -16 19066.2 926.019 14
0 0 -16 20567.5 953.577 17
0 0 16 17979.3 1167.07 39
0 0 16 18908.4 936.375 65
0 0 -16 18289.3 923.552 68
0 0 16 18950.1 937.378 63
0 0 -16 19461.8 949.831 53
0 0 -16 19651.3 924.845 10
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0 0 16 18116.5 1110.05 24
0 0 -16 16806.1 1124.78 22
0 0 16 16761.4 1103.09 25
0 0 16 18170.8 1110.00 27
0 0 16 19015.5 1138.73 26
0 0 17-9.40474 61.0502 85
0 0 17 9.85087 59.9455 86
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0 0 -17-23.1378 40.8787 51
0 0 -17 10.0745 54.5975 53
0 0 -17 19.6662 58.7965 52
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0 0 -17 47.3447 52.4192 75
0 0 17 98.1641 72.7393 81
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0 0 -17 28.4694 65.2289 17
0 0 -17 17.2834 43.6718 68
0 0 17-9.03206 55.9025 65
0 0 17-18.3461 56.7750 63
0 0 17 56.2144 71.8055 54
0 0 -17-25.3897 95.6352 13
0 0 -17 38.2053 62.2642 10
0 0 17-23.9032 71.4640 24
0 0 17 15.6547 45.1010 20
0 0 17 73.5691 73.3171 25
0 0 17-25.4449 76.0731 26
0 0 17 22.9867 89.9807 27
0 0 18-9.12223 53.5629 81
0 0 -18-18.6752 51.6920 52
0 0 -18 38.4822 55.4330 53
0 0 -18 6.83205 36.2114 51
0 0 18-8.54429 57.1204 71
0 0 -18-38.2936 65.3393 14
0 0 -18 26.9068 62.4761 17
0 0 -18 20.9037 41.6641 76
0 0 -18-8.92198 48.3512 75
0 0 -18 31.8732 45.0212 68
0 0 18-48.7820 55.1240 65
0 0 18-24.9278 56.3371 63
0 0 18-43.8430 63.4459 54
0 0 -18 13.8620 54.2624 10
0 0 -18 71.2888 81.5453 13
0 0 18 7.01916 46.9247 20
0 0 18 55.1906 59.7107 86
0 0 18-8.81089 62.1775 85
0 0 18-17.6932 54.7543 88
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0 0 -19-16.8050 52.8706 52
0 0 19-30.0219 65.1501 71
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0 0 -19-31.6784 50.6301 75
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0 0 -19-27.1047 40.5248 68
0 0 19-7.00177 43.3427 63
0 0 19-23.1668 56.5575 54
0 0 -19-45.1338 58.0856 10
0 0 -19-69.7517 79.2166 13
0 0 19 11.5666 38.6702 20
0 0 19 23.9815 50.2998 86
0 0 19-46.7267 58.3791 85
0 0 19 22.9738 50.4640 88
0 0 20 1140.97 119.183 81
0 0 -20 848.551 109.982 52
0 0 20 1078.67 112.147 72
0 0 20 1040.50 112.950 71
0 0 -20 1133.56 115.551 14
0 0 20 854.553 94.3933 65
0 0 20 888.582 99.4585 63
0 0 20 1012.08 112.972 85
0 0 20 1061.17 110.990 88
0 0 20 887.629 107.815 86
0 0 20 766.736 83.5488 20
0 0 20 1077.39 115.097 54
0 0 -20 861.344 105.422 75
0 0 -20 1099.88 121.235 13
0 0 -21-46.7374 53.4655 13
0 0 21 47.3745 45.4262 54
0 0 21-19.3588 36.6884 86
0 0 21-4.81631 36.5111 85
0 0 21-19.7800 34.8983 81
0 0 -21 4.74103 31.2410 75
0 0 21-21.2661 39.0472 72
0 0 21-18.1012 39.2803 71
0 0 -21 5.55821 36.6250 52
0 0 22-13.8650 26.4044 16
0 0 -22 12.7459 33.8400 13
0 -1 0 118.813 17.4572 41
0 1 0 104.910 18.7619 9
0 1 0 11.8558 14.7587 33
0 1 0 22.6100 11.6292 91
0 -1 -1 50423.8 2163.61 37
0 1 1 51234.9 2180.59 33
0 -1 -1 48832.0 2151.64 38
0 1 1 48387.2 2159.44 39
0 -1 -1 51226.0 2164.95 23
0 1 1 47288.0 2149.90 25
0 1 1 46619.2 2146.07 24
0 1 1 50306.9 2158.66 26
0 -1 -1 51164.8 2165.61 28
0 1 1 47173.1 2153.12 40
0 1 1 51525.8 2147.01 9
0 1 -1 51519.6 2165.34 91
0 1 1 50613.5 2176.93 1
0 1 2 98461.5 4314.69 24
0 1 2 99758.4 4319.16 25
0 -1 2 97662.4 4308.51 21
0 -1 -2 100912. 4329.72 23
0 1 2 98606.4 4326.45 26
0 -1 -2 98932.1 4331.49 28
0 1 -2 99881.5 4300.59 30
0 -1 2 97262.1 4322.14 26
0 -1 2 103205. 4333.88 43
0 -1 2 98129.0 4316.89 42
0 1 2 95410.7 4316.28 40
0 1 -2 99123.6 4327.93 91
0 -1 -2 98031.4 4321.12 38
0 1 -2 98996.6 4328.70 33
0 -1 -2 99907.6 4333.33 37
0 -1 2 98563.7 4329.15 36
0 1 2 98720.9 4324.28 39
0 1 2 103165. 4331.57 33
0 1 2 97694.7 4325.88 1
0 1 -2 100451. 4328.03 1
0 -1 -3 259821. 11423.5 23
0 -1 3 269166. 11402.9 21
0 1 3 254439. 11408.8 24
0 -1 3 259481. 11422.9 25
0 1 -3 255159. 11414.2 22
0 1 3 258048. 11412.7 25
0 1 3 264478. 11423.5 26
0 -1 3 269450. 11420.0 26
0 1 -3 262597. 11392.3 29
0 -1 -3 264051. 11425.6 28
0 1 -3 251984. 11385.3 30
0 1 3 268301. 11405.8 33
0 -1 -3 263898. 11417.4 38
0 1 -3 274963. 11406.0 33
0 -1 -3 263560. 11429.3 37
0 1 3 258451. 11433.4 36
0 -1 3 273097. 11421.4 36
0 1 -3 257197. 11378.8 35
0 1 3 257663. 11417.4 39
0 1 3 253400. 11409.2 40
0 -1 3 277240. 11406.2 42
0 -1 3 274162. 11426.5 43
0 1 -3 266251. 11404.2 1
0 1 3 262201. 11401.7 1
0 1 -4 390127. 18634.2 22
0 -1 4 438761. 18631.1 21
0 -1 -4 435398. 18652.6 23
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-11 2 1 4718.47 272.419 19
-11 2 1 5275.63 287.346 12
-11 2 1 5063.38 279.312 8
11 2 0 284.390 45.5288 15
11 -2 0 338.286 56.6945 15
-11 2 0 225.525 53.9720 19
-11 2 0 236.522 57.2937 8
11 2 1 791.140 71.8193 15
11 -2 1 999.513 88.8930 15
-11 2 -1 1044.65 95.8446 19
-11 2 -1 975.517 91.3867 8
11 2 2 386.097 44.9419 15
11 -2 2 540.249 62.0171 15
-11 2 -2 431.025 65.6272 19
-11 2 -2 450.424 62.8419 12
-11 2 -2 528.424 65.0962 8
11 -2 3 1354.59 96.1283 15
-11 2 -3 1191.76 98.6400 19
-11 2 -3 1164.63 94.3611 8
11 -2 4 738.450 65.1795 15
-11 2 -4 525.892 64.0614 19
-11 2 -4 695.999 65.5675 8
11 3 -4 4.97360 24.4979 7
11 3 -4-6.52214 23.3062 10
11 3 -3 3429.55 175.160 7
-11 3 3 2870.15 171.869 12
11 3 -3 2982.99 167.373 10
-11 3 2 252.831 42.3014 19
11 3 -2 337.905 44.7565 7
-11 3 2 227.351 45.5001 12
11 3 -2 295.853 42.9610 10
-11 3 2 266.941 49.3180 8
-11 3 1 19.0072 28.8610 19
11 3 -1-19.4138 25.5783 7
-11 3 1 20.8433 28.5786 12
-11 3 1 10.2969 31.7475 8
-11 3 0 79.7262 34.6948 19
-11 3 0 37.3084 31.6993 8
-11 3 -1 85.2100 35.2310 19
-11 3 -1 126.022 35.3557 12
-11 3 -1 103.385 36.6074 8
-11 3 -2 2119.55 136.847 12
-11 3 -2 2352.93 145.514 19
0 0 0 0.00 0.00 0
TITL Addison-mao-0719ar_auto in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 1.54184 9.128478 8.659765 17.801564 90.0000 92.1565 90.0000
ZERR 20.00 0.000048 0.000073 0.000101 0.0000 0.0005 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O Cl
UNIT 20.00 20.00 20.00 20.00 20.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 7200
_shelx_res_file
;
TITL addison-mao-0719ar_auto_a.res in P2(1)/c
3.res
created by SHELXL-2019/3 at 15:24:22 on 27-Jan-2025
REM Old TITL Addison-mao-0719ar_auto in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.145, Rweak 0.111, Alpha 0.027
REM 0.540 for 63 systematic absences, Orientation as input
REM Formula found by SHELXT: C7 N14 Cl3
CELL 1.54184 9.1219 8.6565 17.7935 90 92.195 90
ZERR 4 0.0003 0.0002 0.0007 0 0.003 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H S N
UNIT 40 72 12 16
OMIT -1 1 2
OMIT -5 8 12
OMIT 5 1 1
LIST 4
Temp 20
L.S. 25
acta
conf
bond $h
htab
EQIV $1 -x+1, -y, -z+1
HTAB N1 S1_$1
HTAB N4 S3
HTAB N4 N2
EQIV $2 -x, y+1/2, -z+3/2
HTAB C6 S2_$2
WGHT 0.044500 0.392600
FVAR 5.32751
S1 3 0.697619 0.131615 0.536375 11.00000 0.04156 0.04282 =
0.07280 -0.01643 0.00102 0.00578
S2 3 0.031600 0.401849 0.703200 11.00000 0.05412 0.05592 =
0.05994 -0.00550 0.01997 -0.00071
S3 3 0.533763 0.645358 0.719563 11.00000 0.05286 0.05079 =
0.04506 -0.00093 -0.00629 0.00232
N1 4 0.424557 0.185958 0.572319 11.00000 0.04193 0.03338 =
0.05124 -0.00700 0.00448 0.00065
H1N 2 0.406054 0.098392 0.556033 11.00000 0.06081
N2 4 0.310583 0.289791 0.582684 11.00000 0.04044 0.03775 =
0.04438 -0.00433 0.00314 0.00405
N3 4 0.703378 0.474261 0.576646 11.00000 0.04114 0.03893 =
0.04987 -0.00337 -0.00075 -0.00079
N4 4 0.572153 0.395381 0.580046 11.00000 0.03934 0.03553 =
0.05195 -0.00596 0.00216 0.00056
H4N 2 0.496554 0.433498 0.596705 11.00000 0.05313
C1 1 0.560861 0.244573 0.563436 11.00000 0.04238 0.03482 =
0.03599 -0.00268 -0.00168 0.00240
C2 1 0.185606 0.236258 0.600047 11.00000 0.04359 0.04309 =
0.04294 -0.00539 0.00484 -0.00082
C3 1 0.147241 0.072679 0.615646 11.00000 0.06203 0.04706 =
0.08504 -0.00333 0.02635 -0.00506
AFIX 137
H3A 2 0.235385 0.014447 0.625703 11.00000 -1.50000
H3B 2 0.094818 0.029794 0.572731 11.00000 -1.50000
H3C 2 0.086755 0.068214 0.658572 11.00000 -1.50000
AFIX 0
C4 1 0.067943 0.356312 0.606369 11.00000 0.04162 0.05041 =
0.05379 -0.00478 0.00370 0.00295
AFIX 23
H4A 2 -0.021574 0.319193 0.581314 11.00000 -1.20000
H4B 2 0.097687 0.449631 0.580904 11.00000 -1.20000
AFIX 0
C5 1 0.199948 0.497849 0.733313 11.00000 0.05853 0.05285 =
0.04469 -0.00265 0.00508 0.00449
AFIX 23
H5A 2 0.197519 0.516916 0.786970 11.00000 -1.20000
H5B 2 0.281462 0.428758 0.724999 11.00000 -1.20000
AFIX 0
C6 1 0.228126 0.648840 0.694102 11.00000 0.04966 0.04590 =
0.05368 -0.00514 0.00216 0.00827
AFIX 23
H6A 2 0.140912 0.712743 0.695429 11.00000 -1.20000
H6B 2 0.247669 0.628655 0.641806 11.00000 -1.20000
AFIX 0
C7 1 0.356799 0.735871 0.730241 11.00000 0.06475 0.04571 =
0.05670 -0.01614 0.00345 0.00469
AFIX 23
H7A 2 0.340343 0.747291 0.783489 11.00000 -1.20000
H7B 2 0.359541 0.838632 0.708604 11.00000 -1.20000
AFIX 0
C8 1 0.566799 0.700759 0.622923 11.00000 0.05249 0.03488 =
0.04956 0.00120 -0.00254 0.00434
AFIX 23
H8A 2 0.481977 0.675051 0.590806 11.00000 -1.20000
H8B 2 0.582617 0.811384 0.620125 11.00000 -1.20000
AFIX 0
C9 1 0.699421 0.616762 0.596551 11.00000 0.04662 0.03558 =
0.04406 0.00076 -0.00443 0.00035
C10 1 0.838997 0.706938 0.595518 11.00000 0.05162 0.04188 =
0.06662 -0.00147 -0.00360 -0.00489
AFIX 137
H10A 2 0.913013 0.646324 0.572404 11.00000 -1.50000
H10B 2 0.870766 0.732008 0.646114 11.00000 -1.50000
H10C 2 0.822889 0.800419 0.567373 11.00000 -1.50000
AFIX 0
HKLF 4
REM addison-mao-0719ar_auto_a.res in P2(1)/c
REM wR2 = 0.0865, GooF = S = 1.082, Restrained GooF = 1.082 for all data
REM R1 = 0.0307 for 2806 Fo > 4sig(Fo) and 0.0321 for all 2983 data
REM 164 parameters refined using 0 restraints
END
WGHT 0.0445 0.3926
REM Instructions for potential hydrogen bonds
HTAB N1 S1_$1
HTAB N4 S3
HTAB N4 N2
HTAB C6 S2_$2
REM Highest difference peak 0.218, deepest hole -0.277, 1-sigma level 0.040
Q1 1 0.0217 0.0651 0.6086 11.00000 0.05 0.22
Q2 1 0.1929 -0.0175 0.5819 11.00000 0.05 0.19
Q3 1 0.5580 0.3207 0.5584 11.00000 0.05 0.16
Q4 1 0.1383 0.2803 0.6044 11.00000 0.05 0.15
Q5 1 0.1901 0.0410 0.6860 11.00000 0.05 0.14
Q6 1 0.2933 0.6749 0.7124 11.00000 0.05 0.14
Q7 1 0.2037 0.5808 0.7152 11.00000 0.05 0.14
Q8 1 0.1655 0.1667 0.5993 11.00000 0.05 0.14
Q9 1 0.7191 0.2147 0.5073 11.00000 0.05 0.14
Q10 1 0.7453 0.6417 0.5952 11.00000 0.05 0.14
Q11 1 0.5005 0.2084 0.5787 11.00000 0.05 0.13
Q12 1 0.0273 0.2994 0.7360 11.00000 0.05 0.12
Q13 1 -0.1109 0.3987 0.7104 11.00000 0.05 0.12
Q14 1 0.2332 0.6385 0.6573 11.00000 0.05 0.12
Q15 1 0.2594 0.2602 0.6037 11.00000 0.05 0.12
Q16 1 0.7036 0.5335 0.5988 11.00000 0.05 0.12
Q17 1 0.3935 0.6402 0.7178 11.00000 0.05 0.12
Q18 1 -0.0818 0.5080 0.7232 11.00000 0.05 0.12
Q19 1 0.7559 0.4553 0.5540 11.00000 0.05 0.12
Q20 1 0.1394 0.5330 0.7898 11.00000 0.05 0.11
;
_shelx_res_checksum 81989
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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
S S1 0.69762(4) 0.13162(5) 0.53637(3) 0.05242(13) Uani d 1 . .
S S2 0.03160(5) 0.40185(5) 0.70320(3) 0.05621(13) Uani d 1 . .
S S3 0.53376(4) 0.64536(5) 0.71956(2) 0.04978(12) Uani d 1 . .
N N1 0.42456(13) 0.18596(15) 0.57232(7) 0.0421(3) Uani d 1 . .
H H1N 0.406(2) 0.098(2) 0.5560(12) 0.061(6) Uiso d 1 . .
N N2 0.31058(13) 0.28979(14) 0.58268(7) 0.0408(3) Uani d 1 . .
N N3 0.70338(13) 0.47426(15) 0.57665(7) 0.0434(3) Uani d 1 . .
N N4 0.57215(14) 0.39538(15) 0.58005(7) 0.0423(3) Uani d 1 . .
H H4N 0.497(2) 0.433(2) 0.5967(11) 0.053(5) Uiso d 1 . .
C C1 0.56086(15) 0.24457(16) 0.56344(7) 0.0378(3) Uani d 1 . .
C C2 0.18561(16) 0.23626(18) 0.60005(8) 0.0431(3) Uani d 1 . .
C C3 0.1472(2) 0.0727(2) 0.61565(12) 0.0641(5) Uani d 1 . .
H H3A 0.235385 0.014447 0.625703 0.096 Uiso calc 1 . .
H H3B 0.094818 0.029794 0.572731 0.096 Uiso calc 1 . .
H H3C 0.086755 0.068214 0.658572 0.096 Uiso calc 1 . .
C C4 0.06794(17) 0.3563(2) 0.60637(9) 0.0486(4) Uani d 1 . .
H H4A -0.021574 0.319193 0.581314 0.058 Uiso calc 1 . .
H H4B 0.097687 0.449631 0.580904 0.058 Uiso calc 1 . .
C C5 0.19995(19) 0.4978(2) 0.73331(9) 0.0519(4) Uani d 1 . .
H H5A 0.197519 0.516916 0.786970 0.062 Uiso calc 1 . .
H H5B 0.281462 0.428758 0.724999 0.062 Uiso calc 1 . .
C C6 0.22813(18) 0.64884(19) 0.69410(9) 0.0497(4) Uani d 1 . .
H H6A 0.140912 0.712743 0.695429 0.060 Uiso calc 1 . .
H H6B 0.247669 0.628655 0.641806 0.060 Uiso calc 1 . .
C C7 0.3568(2) 0.7359(2) 0.73024(10) 0.0557(4) Uani d 1 . .
H H7A 0.340343 0.747291 0.783489 0.067 Uiso calc 1 . .
H H7B 0.359541 0.838632 0.708604 0.067 Uiso calc 1 . .
C C8 0.56680(17) 0.70076(18) 0.62292(9) 0.0458(3) Uani d 1 . .
H H8A 0.481977 0.675051 0.590806 0.055 Uiso calc 1 . .
H H8B 0.582617 0.811384 0.620125 0.055 Uiso calc 1 . .
C C9 0.69942(17) 0.61676(17) 0.59655(8) 0.0422(3) Uani d 1 . .
C C10 0.83900(18) 0.7069(2) 0.59552(10) 0.0535(4) Uani d 1 . .
H H10A 0.913013 0.646324 0.572404 0.080 Uiso calc 1 . .
H H10B 0.870766 0.732008 0.646114 0.080 Uiso calc 1 . .
H H10C 0.822889 0.800419 0.567373 0.080 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
S1 0.0416(2) 0.0428(2) 0.0728(3) 0.00578(15) 0.00102(17) -0.01643(18)
S2 0.0541(2) 0.0559(3) 0.0599(2) -0.00071(18) 0.01997(18) -0.00550(18)
S3 0.0529(2) 0.0508(2) 0.0451(2) 0.00232(16) -0.00629(16) -0.00093(15)
N1 0.0419(6) 0.0334(6) 0.0512(7) 0.0007(5) 0.0045(5) -0.0070(5)
N2 0.0404(6) 0.0378(6) 0.0444(6) 0.0041(5) 0.0031(5) -0.0043(5)
N3 0.0411(6) 0.0389(7) 0.0499(7) -0.0008(5) -0.0008(5) -0.0034(5)
N4 0.0393(6) 0.0355(6) 0.0519(7) 0.0006(5) 0.0022(5) -0.0060(5)
C1 0.0424(7) 0.0348(7) 0.0360(6) 0.0024(5) -0.0017(5) -0.0027(5)
C2 0.0436(7) 0.0431(8) 0.0429(7) -0.0008(6) 0.0048(6) -0.0054(6)
C3 0.0620(11) 0.0471(10) 0.0850(13) -0.0051(8) 0.0263(9) -0.0033(9)
C4 0.0416(8) 0.0504(9) 0.0538(9) 0.0029(6) 0.0037(6) -0.0048(7)
C5 0.0585(9) 0.0528(10) 0.0447(8) 0.0045(7) 0.0051(7) -0.0026(7)
C6 0.0497(8) 0.0459(9) 0.0537(9) 0.0083(7) 0.0022(7) -0.0051(7)
C7 0.0647(10) 0.0457(9) 0.0567(9) 0.0047(8) 0.0035(7) -0.0161(7)
C8 0.0525(8) 0.0349(8) 0.0496(8) 0.0043(6) -0.0025(6) 0.0012(6)
C9 0.0466(8) 0.0356(7) 0.0441(7) 0.0003(6) -0.0044(6) 0.0008(6)
C10 0.0516(9) 0.0419(9) 0.0666(10) -0.0049(7) -0.0036(7) -0.0015(7)
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'
S S 0.3331 0.5567 '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'
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
C5 S2 C4 . . 101.40(7) yes
C7 S3 C8 . . 99.53(8) yes
C1 N1 N2 . . 117.78(12) yes
C1 N1 H1N . . 118.5(14) ?
N2 N1 H1N . . 119.7(14) ?
C2 N2 N1 . . 118.37(13) yes
C9 N3 N4 . . 115.41(13) yes
C1 N4 N3 . . 122.05(13) yes
C1 N4 H4N . . 114.1(14) ?
N3 N4 H4N . . 123.6(14) ?
N4 C1 N1 . . 113.64(13) yes
N4 C1 S1 . . 125.54(11) yes
N1 C1 S1 . . 120.81(11) ?
N2 C2 C3 . . 127.45(14) yes
N2 C2 C4 . . 114.43(14) yes
C3 C2 C4 . . 118.10(14) yes
C2 C3 H3A . . 109.5 ?
C2 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C2 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
C2 C4 S2 . . 112.30(11) yes
C2 C4 H4A . . 109.1 ?
S2 C4 H4A . . 109.1 ?
C2 C4 H4B . . 109.1 ?
S2 C4 H4B . . 109.1 ?
H4A C4 H4B . . 107.9 ?
C6 C5 S2 . . 114.76(12) yes
C6 C5 H5A . . 108.6 ?
S2 C5 H5A . . 108.6 ?
C6 C5 H5B . . 108.6 ?
S2 C5 H5B . . 108.6 ?
H5A C5 H5B . . 107.6 ?
C5 C6 C7 . . 112.15(14) yes
C5 C6 H6A . . 109.2 ?
C7 C6 H6A . . 109.2 ?
C5 C6 H6B . . 109.2 ?
C7 C6 H6B . . 109.2 ?
H6A C6 H6B . . 107.9 ?
C6 C7 S3 . . 114.77(11) yes
C6 C7 H7A . . 108.6 ?
S3 C7 H7A . . 108.6 ?
C6 C7 H7B . . 108.6 ?
S3 C7 H7B . . 108.6 ?
H7A C7 H7B . . 107.6 ?
C9 C8 S3 . . 109.38(10) yes
C9 C8 H8A . . 109.8 ?
S3 C8 H8A . . 109.8 ?
C9 C8 H8B . . 109.8 ?
S3 C8 H8B . . 109.8 ?
H8A C8 H8B . . 108.2 ?
N3 C9 C10 . . 117.74(14) yes
N3 C9 C8 . . 125.64(14) yes
C10 C9 C8 . . 116.61(13) yes
C9 C10 H10A . . 109.5 ?
C9 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C9 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
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
S1 C1 . 1.6704(14) yes
S2 C5 . 1.8091(18) yes
S2 C4 . 1.8104(17) yes
S3 C7 . 1.8109(18) yes
S3 C8 . 1.8214(16) yes
N1 C1 . 1.3577(18) yes
N1 N2 . 1.3919(17) yes
N1 H1N . 0.83(2) ?
N2 C2 . 1.2794(19) yes
N3 C9 . 1.2843(19) yes
N3 N4 . 1.3814(18) yes
N4 C1 . 1.3416(19) yes
N4 H4N . 0.83(2) ?
C2 C3 . 1.487(2) yes
C2 C4 . 1.501(2) yes
C3 H3A . 0.9600 ?
C3 H3B . 0.9600 ?
C3 H3C . 0.9600 ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C5 C6 . 1.508(2) yes
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C6 C7 . 1.517(2) yes
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C8 C9 . 1.502(2) yes
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C9 C10 . 1.494(2) yes
C10 H10A . 0.9600 ?
C10 H10B . 0.9600 ?
C10 H10C . 0.9600 ?
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 H1N S1 3_656 0.83(2) 2.73(2) 3.5178(14) 160.4(19) yes
N4 H4N S3 . 0.83(2) 2.864(19) 3.3218(13) 116.9(15) yes
N4 H4N N2 . 0.83(2) 2.11(2) 2.5572(18) 113.5(16) yes
C6 H6A S2 2_556 0.97 2.94 3.7524(17) 142.4 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
C1 N1 N2 C2 . . . . -171.77(13) ?
C9 N3 N4 C1 . . . . -177.66(14) ?
N3 N4 C1 N1 . . . . 177.97(12) ?
N3 N4 C1 S1 . . . . -0.4(2) ?
N2 N1 C1 N4 . . . . 11.94(18) ?
N2 N1 C1 S1 . . . . -169.57(10) ?
N1 N2 C2 C3 . . . . 4.1(2) ?
N1 N2 C2 C4 . . . . -177.19(12) ?
N2 C2 C4 S2 . . . . -103.13(14) ?
C3 C2 C4 S2 . . . . 75.67(17) ?
C5 S2 C4 C2 . . . . 68.26(13) ?
C4 S2 C5 C6 . . . . 65.09(13) ?
S2 C5 C6 C7 . . . . 170.72(11) ?
C5 C6 C7 S3 . . . . 67.92(17) ?
C8 S3 C7 C6 . . . . 78.04(15) ?
C7 S3 C8 C9 . . . . -171.14(11) ?
N4 N3 C9 C10 . . . . 178.75(13) ?
N4 N3 C9 C8 . . . . 0.4(2) ?
S3 C8 C9 N3 . . . . 76.54(17) ?
S3 C8 C9 C10 . . . . -101.80(14) ?