#------------------------------------------------------------------------------
#$Date: 2022-11-10 03:47:41 +0100 (Thu, 10 Nov 2022) $
#$Revision: 279171 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/26/2022698.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_2022698
loop_
_publ_author_name
'De Silva, Viraj'
'Magueres, Pierre Le'
'Averkiev, Boris B.'
'Aaker\"oy, Christer B.'
_publ_section_title
;
Competition between chalcogen and halogen bonding assessed through
isostructural species
;
_journal_coeditor_code BS3004
_journal_issue 12
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S205322962201052X
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac 'C8 H4 Br I N2 S'
_chemical_formula_moiety 'C8 H4 Br I N2 S'
_chemical_formula_sum 'C8 H4 Br I N2 S'
_chemical_formula_weight 367.00
_chemical_name_systematic
;
2-Bromo-5-(4-iodophenyl)-1,3,4-thiadiazole
;
_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 geom
_atom_sites_solution_primary dual
_audit_creation_method
;
OLEX2
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 10.9919(2)
_cell_length_b 6.99450(10)
_cell_length_c 26.4076(4)
_cell_measurement_reflns_used 5134
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 70.6430
_cell_measurement_theta_min 3.3330
_cell_volume 2030.29(6)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy Custom diffractometer with a HyPix-Arc 150\% detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0246
_diffrn_reflns_av_unetI/netI 0.0233
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 31
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 7258
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 70.701
_diffrn_reflns_theta_min 3.347
_diffrn_source 'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu 30.946
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.37294
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2020)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.401
_exptl_crystal_description plate
_exptl_crystal_F_000 1360
_exptl_crystal_size_max 0.048
_exptl_crystal_size_mid 0.039
_exptl_crystal_size_min 0.012
_refine_diff_density_max 0.566
_refine_diff_density_min -0.669
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.070
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 118
_refine_ls_number_reflns 1920
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.070
_refine_ls_R_factor_all 0.0229
_refine_ls_R_factor_gt 0.0210
_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^)+(0.0219P)^2^+2.6464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0509
_refine_ls_wR_factor_ref 0.0517
_reflns_number_gt 1802
_reflns_number_total 1920
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file bs3004sup1.cif
_cod_data_source_block T4
_cod_database_code 2022698
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 2 14747.8 481.337 1
0 0 -2 15622.0 482.520 1
0 0 3 33.9950 23.4203 3
0 0 3 4.64683 24.4542 1
0 0 4 47401.2 1497.19 3
0 0 4 47966.4 1499.07 1
0 0 5 40.4949 32.8125 3
0 0 5 10.1855 34.3832 1
0 0 6 57323.2 1800.96 3
0 0 6 57154.5 1802.42 1
0 0 7 5.99255 35.0099 3
0 0 7 23.6527 39.3503 1
0 0 8 262260. 8081.45 3
0 0 8 255850. 8083.44 1
0 0 9 9.71989 36.4951 3
0 0 9 49.0502 37.3009 1
0 0 10 4986.66 189.019 1
0 0 10 4902.49 187.230 3
0 0 11 37.4592 38.3046 3
0 0 12 2351.88 112.066 1
0 0 12 2474.19 112.975 3
0 0 13 23.7459 35.6048 3
0 0 13-20.8244 36.7882 1
0 0 14 83987.1 2608.54 3
0 0 14 80944.1 2607.89 1
0 0 15-8.00036 36.3209 1
0 0 16 5006.21 206.043 3
0 0 17-37.0772 38.8036 3
0 0 18 60243.3 1932.31 3
0 0 19 20.9371 41.9447 3
0 0 20 2677.54 139.934 3
0 0 21 40.0508 42.6219 3
0 0 22 1019.84 86.8653 3
0 0 23 65.2483 45.9235 3
0 0 24 15131.1 537.731 3
0 0 26 81930.9 2630.38 6
0 0 27 6.14382 40.3085 7
0 0 28 5231.79 225.182 7
0 0 29 14.7845 36.2130 7
0 0 30 11957.7 417.087 4
0 0 30 12521.8 429.190 7
0 0 31 7.36686 23.4512 4
0 1 0 4.39403 14.7766 4
0 1 1 9.26155 16.7124 5
0 1 -1 4.25190 16.0135 6
0 1 -1 2.60898 7.27548 9
0 1 -1 16.4772 15.9298 4
0 1 1 8.05701 15.8739 4
0 1 2 11.4855 18.3923 5
0 -1 -2 13.8140 18.7347 5
0 1 -2 17.1186 17.6506 6
0 1 2 21.9495 19.3748 4
0 1 -2 1.71933 18.4329 4
0 -1 2 13.2494 17.9511 6
0 1 -2 2.89580 12.4806 9
0 -1 3-12.4189 20.2537 6
0 -1 -3-10.5590 20.9034 5
0 -1 4 8.85035 22.3628 2
0 -1 -4 4.20817 24.1430 5
0 -1 4-1.33801 23.3392 6
0 1 4 26.4863 25.6308 3
0 1 5 13.7656 28.3854 3
0 1 -5 13.3039 12.5983 12
0 -1 -5-1.69285 27.8910 5
0 -1 5 25.2410 27.2830 2
0 -1 6 24.1392 28.4403 2
0 -1 -6-2.06841 32.5315 5
0 1 6 18.1987 32.9773 3
0 1 7 12.9146 35.0781 3
0 1 8 17.2744 35.5275 3
0 -1 8 24.3291 34.3410 1
0 1 9 36.1257 36.6230 3
0 -1 9 2.87399 38.5852 1
0 1 10 3.07668 37.1648 3
0 1 10 7.49215 15.5247 11
0 1 11 13.4449 38.3056 3
0 -1 12 51.6440 43.1884 1
0 -1 12-32.8977 39.1207 3
0 1 12 10.9162 38.0654 3
0 -1 13 3.83004 40.3383 3
0 1 13 11.7479 39.8637 3
0 -1 13 53.0221 41.2256 1
0 -1 14 29.7915 43.6231 1
0 -1 14-4.00547 38.4045 3
0 1 15 26.7210 42.3630 3
0 -1 15 13.5736 40.1665 1
0 -1 16 33.2369 39.3282 1
0 1 16 42.5002 43.4489 3
0 -1 16 4.46571 39.8308 3
0 -1 17 9.91779 39.2821 1
0 1 17 25.0732 45.7346 3
0 -1 17 14.0279 38.7255 3
0 -1 18 4.92699 40.8013 3
0 1 18-21.2355 42.7786 3
0 -1 18 20.8100 40.7268 1
0 -1 19-10.3834 39.7008 3
0 -1 19 10.9592 40.2993 1
0 -1 20-28.3758 43.3574 1
0 -1 20 60.5833 45.3671 3
0 1 20-46.2241 43.8663 3
0 -1 21 55.8014 44.7270 3
0 1 21 24.0206 47.5816 3
0 -1 22-28.2362 43.1501 3
0 -1 22-21.9864 47.6797 6
0 -1 23-7.44253 50.0550 6
0 -1 23-5.64465 43.1235 3
0 -1 24 150.167 53.3128 6
0 -1 24 22.1079 41.7455 3
0 -1 25-14.3692 49.4771 6
0 -1 26 24.5654 42.2912 7
0 -1 26-20.4154 45.0238 6
0 1 27 5.45807 41.4369 4
0 -1 27 5.67023 39.0474 7
0 1 27 12.1472 42.7794 7
0 1 28 19.1493 38.5770 4
0 1 28 43.6794 41.1882 7
0 -1 28-25.6611 39.6964 7
0 1 29 32.3678 33.5171 4
0 1 29 43.4541 37.1264 7
0 -1 29 13.2553 33.9772 7
0 -1 30 18.5828 30.4542 7
0 1 30 16.1543 31.8310 4
0 1 30 24.4643 33.4098 7
0 2 0 1742.72 75.3304 4
0 2 1 4633.84 150.380 5
0 2 -1 4554.62 150.866 6
0 2 -1 4395.13 147.416 4
0 2 1 4479.62 148.300 4
0 2 2 203337. 6359.10 4
0 2 2 204771. 6360.32 5
0 2 -2 202041. 6362.19 6
0 2 -2 205534. 6358.83 4
0 2 3 399499. 11937.3 4
0 2 -3 403217. 11941.0 6
0 -2 3 369792. 11918.4 7
0 2 3 403392. 11937.8 5
0 2 -3 401044. 11936.5 4
0 2 4 5048.73 188.519 5
0 2 4 5478.20 188.645 4
0 -2 5 116582. 3677.58 2
0 2 5 117771. 3681.74 4
0 -2 5 118729. 3682.11 6
0 -2 6 30077.0 949.457 2
0 -2 6 28623.6 953.796 6
0 2 6 30686.8 954.697 4
0 -2 -6 29630.5 957.881 5
0 2 7 1519.10 77.3706 4
0 -2 7 1433.14 77.7741 6
0 -2 -7 1471.31 82.1378 5
0 -2 7 1553.16 75.1735 2
0 -2 8 1807.72 93.1162 6
0 -2 8 1952.53 90.2793 2
0 -2 9 20970.4 692.019 2
0 -2 9 21483.7 701.630 6
0 -2 10 14403.3 497.068 6
0 -2 11 127916. 4045.88 6
0 -2 11 128808. 4038.46 1
0 -2 12 3874.09 171.866 6
0 -2 12 3370.38 159.673 1
0 -2 13 232.191 53.7723 1
0 -2 13 329.949 56.8171 6
0 -2 14 3118.13 164.010 6
0 -2 14 3220.54 159.312 1
0 -2 15 19180.3 654.190 1
0 -2 15 18414.8 645.381 3
0 -2 16 362.468 59.3256 1
0 -2 16 159.821 54.3567 6
0 -2 16 278.936 56.7414 3
0 -2 17 8842.53 337.299 1
0 -2 17 8233.74 328.427 3
0 -2 17 9248.93 353.592 6
0 -2 18 164.208 49.0135 3
0 -2 18 124.101 51.8645 6
0 -2 18 11.8003 41.9487 1
0 -2 19 1923.80 114.015 3
0 -2 19 1780.25 114.345 1
0 -2 19 1660.32 119.737 6
0 -2 20 5542.38 240.211 1
0 -2 20 5648.31 253.944 6
0 -2 20 5750.24 236.934 3
0 -2 21 26811.6 914.367 1
0 -2 21 27746.2 910.817 3
0 -2 21 26742.8 930.215 6
0 -2 22 399.118 67.5717 6
0 -2 22 248.381 57.5371 3
0 2 22 363.414 64.5485 4
0 -2 23 29768.5 997.758 7
0 -2 23 29333.5 1010.63 6
0 2 23 30202.4 1004.99 4
0 -2 24 8510.61 333.478 7
0 2 24 8787.06 341.014 4
0 -2 24 8609.23 345.938 6
0 -2 25 832.928 81.7640 6
0 -2 25 711.678 72.5888 7
0 -2 26 445.750 59.1348 7
0 2 26 522.255 64.4715 4
0 2 26 509.171 65.7434 7
0 2 27 9487.68 361.469 7
0 2 27 10151.7 361.309 4
0 -2 27 9457.63 354.243 7
0 2 28 10725.8 380.777 4
0 -2 28 10263.4 375.591 7
0 2 28 10927.6 385.755 7
0 2 29 35337.5 1182.00 7
0 2 29 37595.3 1180.00 4
0 2 30 1968.53 92.2424 4
0 3 0 5.16178 28.4049 4
0 3 0 22.2695 30.2651 5
0 3 1 11.0121 30.5691 5
0 3 1 13.1546 29.9808 4
0 3 -1-17.8963 28.4720 4
0 3 -2 42.3996 30.8756 4
0 3 2-2.84341 28.7431 5
0 3 2 24.3950 30.7208 4
0 3 3 11.8218 28.6814 5
0 3 3 38.6255 29.7246 4
0 3 -3 24.5419 30.7329 4
0 3 4-14.5476 31.1426 4
0 3 4 58.2527 32.0766 5
0 3 5 9.13056 31.3044 4
0 -3 6-5.64837 29.0474 2
0 3 6 16.2006 32.5110 4
0 3 7 14.0594 30.9325 4
0 -3 7 68.0368 34.1074 2
0 -3 8 6.39645 31.7403 2
0 -3 9-3.41177 33.9844 2
0 3 10-13.3581 39.5283 4
0 -3 10-22.7523 36.0485 6
0 3 11 4.90569 39.9726 4
0 -3 11 15.1782 37.4260 6
0 3 12 75.5678 44.7609 4
0 -3 13 10.5423 41.5113 1
0 3 13-29.3698 46.5291 4
0 -3 13-18.6726 43.1921 6
0 -3 14 34.1932 43.7111 6
0 3 14-18.8993 45.9741 4
0 -3 14-11.6435 49.2259 1
0 -3 15 51.5645 51.8887 6
0 3 15 13.3407 47.6729 4
0 -3 15 6.32986 47.4474 1
0 -3 16 6.88846 53.9250 1
0 -3 16-7.76167 52.2010 6
0 3 16 6.95564 48.9913 4
0 -3 17 21.2293 51.2871 1
0 3 17 35.7349 51.7984 4
0 -3 17-8.00984 46.4013 6
0 -3 17-30.4517 52.2793 3
0 -3 18 41.7026 48.2758 3
0 3 18-14.5143 54.7462 4
0 -3 18 6.83910 50.9269 1
0 -3 18 16.2016 51.3158 6
0 -3 19-5.75210 44.4907 3
0 3 19 7.26040 50.3810 4
0 -3 19-24.1432 50.0432 6
0 -3 19-13.3347 46.6148 1
0 -3 20-46.1664 50.6991 1
0 3 20 14.3161 53.6501 4
0 -3 20-5.65765 46.3512 3
0 -3 20 39.6449 50.6806 6
0 -3 21 7.72687 49.8280 6
0 3 21 6.99757 49.2872 4
0 -3 22-54.5433 46.5905 1
0 -3 22-37.2588 49.3047 6
0 3 22 74.3787 50.3517 4
0 -3 23 57.7348 46.7878 1
0 3 23-5.96321 41.6969 7
0 3 24 33.6220 41.1740 7
0 3 24-18.2207 41.8249 4
0 3 25 52.2935 43.5377 7
0 3 25-16.9860 43.2584 4
0 3 26 4.67977 37.7099 7
0 3 26 10.0193 40.1406 4
0 3 27 45.1746 37.2909 7
0 3 27-8.65887 35.6647 4
0 3 28-10.8383 30.2364 4
0 3 29 2.82640 26.1129 4
0 4 0 41100.5 1329.53 5
0 4 0 41231.8 1326.50 4
0 4 1 35763.5 1170.23 5
0 4 -1 36270.7 1171.01 5
0 4 1 35725.5 1165.94 4
0 4 -1 36294.5 1167.24 4
0 4 -2 34140.3 1121.42 5
0 4 2 35467.6 1118.62 4
0 4 2 33586.3 1119.04 5
0 4 -2 34340.5 1116.59 4
0 4 3 21230.3 702.993 5
0 4 3 21192.2 700.513 4
0 4 -3 20448.7 696.431 4
0 4 4 16921.0 591.558 5
0 4 4 17802.6 591.259 4
0 4 5 61311.6 1958.36 4
0 -4 6 104407. 3315.91 2
0 4 6 106067. 3323.46 4
0 -4 7 18240.7 607.353 2
0 4 7 17632.7 611.690 4
0 4 8 42051.4 1334.95 4
0 -4 8 40167.4 1326.14 2
0 -4 9 25607.2 843.828 2
0 4 9 25107.4 850.455 4
0 4 10 150.893 47.3471 4
0 -4 10 209.025 47.1305 2
0 4 11 1203.99 92.3457 4
0 -4 11 1126.98 86.4325 2
0 4 12 5019.20 224.846 4
0 4 13 2060.51 130.473 4
0 -4 14 27299.7 932.321 1
0 4 14 27464.0 937.470 4
0 4 15 1103.09 98.4967 4
0 -4 15 1109.95 100.647 1
0 4 16-23.5866 57.3805 4
0 -4 16 84.9105 59.3427 1
0 -4 17 673.817 89.2369 1
0 4 17 839.892 92.7757 4
0 4 18 9517.97 382.883 4
0 -4 19 454.561 71.4529 1
0 4 19 562.556 78.1319 4
0 4 20 2826.73 161.346 4
0 -4 20 3000.39 159.959 1
0 -4 21 4193.77 197.198 1
0 -4 22 4899.88 208.167 1
0 4 22 4365.37 208.627 4
0 4 23 3635.50 173.132 4
0 -4 23 3713.67 169.617 1
0 -4 24 11710.0 416.751 1
0 4 24 11761.8 425.082 4
0 4 25 11444.8 408.528 4
0 4 26 8769.12 318.131 4
0 4 27 7660.42 275.761 4
0 5 0 44.8465 44.1511 4
0 5 0 6.04177 43.1827 5
0 5 -1-5.51858 39.4372 4
0 5 -1 24.2116 42.0015 5
0 5 1 22.6383 41.0184 4
0 5 1-18.0501 43.3030 5
0 5 2-33.7877 39.0779 4
0 5 2 6.04513 40.9850 5
0 5 -2-6.02130 39.8398 5
0 5 3-11.3331 38.4189 4
0 5 -3 12.0017 39.7045 5
0 5 3-36.5118 41.5837 5
0 5 4 28.5270 39.2975 4
0 5 -4 24.2949 41.5106 5
0 5 -5-6.24922 38.1193 5
0 5 5 23.1220 38.8772 4
0 -5 5 5.04049 39.2235 2
0 5 6 36.3706 42.3885 4
0 -5 6 20.2511 35.9301 2
0 5 7-6.22155 41.8463 4
0 -5 7-26.1709 40.9782 2
0 5 8 6.42871 39.5962 4
0 -5 8-10.8034 45.2059 2
0 -5 9-5.49860 43.0452 2
0 5 9 20.1407 44.4182 4
0 -5 10 34.2238 47.5067 2
0 5 10 56.3800 47.4185 4
0 5 11 44.3750 51.7147 4
0 -5 11 17.8090 42.4314 2
0 5 12 15.4532 52.7987 4
0 5 13 32.1081 53.5577 4
0 5 14 57.8052 53.2821 4
0 5 15 50.1814 59.7866 4
0 -5 15 46.4568 53.7484 1
0 5 16 83.0284 61.0241 4
0 -5 16 23.6271 52.1282 1
0 5 17 16.1478 53.8623 4
0 -5 17 7.84837 56.4866 1
0 -5 18 7.35231 57.2129 1
0 5 19 42.7593 48.6971 4
0 -5 19-45.1420 48.6479 1
0 5 20 45.5771 47.5205 4
0 -5 20 5.66797 43.3065 1
0 5 21 23.4786 41.6471 4
0 -5 21-40.1201 44.1033 1
0 5 22 20.7573 40.1375 4
0 -5 22-4.26567 35.3252 1
0 5 23-17.9535 35.5523 4
0 -5 23 10.7310 32.3337 1
0 5 24-22.8698 30.8940 4
0 5 25 6.27993 28.7615 4
0 6 0 26898.5 924.001 5
0 6 -1 362.071 63.0463 5
0 6 1 431.762 65.0266 4
0 6 2 11639.1 433.204 4
0 6 -2 11101.8 435.206 5
0 6 -3 10305.2 411.516 5
0 -6 3 10733.1 404.053 2
0 6 3 11025.8 413.737 4
0 6 4 38683.0 1283.85 4
0 6 -4 37392.6 1284.36 5
0 -6 4 39610.0 1274.93 2
0 -6 5 4581.71 208.774 2
0 6 -5 4466.84 219.961 5
0 6 5 4778.31 220.388 4
0 -6 6 8340.22 320.531 2
0 6 -6 7471.83 327.742 5
0 6 6 8241.46 330.039 4
0 6 -7 16815.2 624.542 5
0 6 7 17922.9 623.756 4
0 -6 7 17203.1 609.535 2
0 6 8 21678.1 730.790 4
0 -6 8 20466.8 710.904 2
0 6 -8 19740.9 727.892 5
0 6 9 1894.30 129.398 4
0 -6 9 1689.12 116.463 2
0 6 -9 1944.09 132.386 5
0 6 -10 3331.91 193.399 5
0 6 10 3718.07 194.790 4
0 -6 10 3960.15 183.703 2
0 6 -11 8683.58 377.033 5
0 6 11 9685.96 377.308 4
0 6 -12 8894.45 377.919 5
0 6 12 9120.53 369.412 4
0 -6 13 14.1532 51.2964 1
0 6 -13 56.2082 65.5022 5
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-12 2 -1 5255.53 212.448 10
-12 -2 -1 5085.05 214.659 8
-12 2 2 60.4720 39.6349 10
-12 2 -2 69.5973 43.1146 10
-12 -2 -2 101.132 41.9414 8
-12 -2 -3 10.8453 44.6787 10
-12 2 3 66.3869 37.8537 10
-12 2 -3 84.3442 41.9896 10
-12 -2 -3-19.9505 39.5204 8
-12 -2 -4 901.421 79.2208 10
-12 2 -4 699.217 68.2493 10
-12 -2 -4 892.615 74.3441 8
-12 -2 -5 267.244 56.8192 10
-12 2 -5 433.326 56.0147 10
-12 -2 -5 488.778 61.2631 9
-12 -2 -5 369.676 55.9407 8
-12 -2 -6 20.1306 45.3200 10
-12 2 -6 102.725 44.8000 10
-12 -2 -6 20.4439 42.5830 9
-12 -2 -6 78.7576 43.1152 8
-12 -2 -7 6358.62 262.380 10
-12 2 -7 6825.60 264.150 10
-12 -2 -7 7148.22 269.660 9
-12 -2 -7 6923.19 266.188 8
-12 -2 -8 2389.93 122.567 10
-12 2 -8 2315.42 123.365 10
-12 -2 -8 2522.31 128.313 9
-12 -2 -8 2507.56 126.966 8
-12 2 -9 240.818 46.2622 10
-12 -2 -9 284.609 51.6088 8
-12 2 -10 632.827 60.3313 10
-12 -2 -10 630.429 62.0735 8
-12 2 -11 208.611 44.6513 10
-12 -2 -11 221.452 44.5334 8
-12 2 -12 1088.50 73.4540 10
-12 -2 -12 1275.62 78.4190 8
-12 3 0 2653.50 137.051 11
-12 3 1 126.155 49.9477 11
-12 3 2 3898.22 179.308 11
-12 3 3 603.987 68.5129 11
-12 -3 -3 446.610 54.0059 8
-12 3 4 126.643 48.1262 11
-12 3 -4 85.2409 31.8450 10
-12 -3 -4 174.915 42.9923 8
-12 -3 -5 461.854 53.3087 8
-12 -3 -6 5700.57 221.667 8
-12 -3 -7 862.588 65.5746 8
-12 -3 -8 672.040 57.8337 8
-13 0 0-12.6668 37.4809 10
-13 0 -1-34.0343 36.1708 10
-13 0 -2 362.247 51.2936 10
-13 0 -3 17.1087 36.1696 10
-13 0 -4-4.23307 36.8725 10
-13 0 -5 29.0684 37.8815 10
-13 0 -6 222.701 43.1972 10
-13 0 -7-3.88820 32.5398 10
-13 0 -8 98.5860 38.0646 10
-13 1 0 11.2485 33.1298 10
-13 1 -1 962.315 69.0497 10
-13 1 -2 2733.81 127.640 10
-13 1 -3 356.961 47.4464 10
-13 -1 -4 12.1999 36.4330 10
-13 1 -4-30.5753 34.8577 10
-13 -1 -5 3496.62 152.562 10
-13 1 -5 3684.93 152.114 10
-13 -1 -5 3257.79 147.630 8
-13 -1 -6 209.981 42.3324 10
-13 1 -6 275.127 44.5517 10
-13 -1 -6 322.278 44.4077 8
-13 1 -7 2036.05 102.276 10
-13 -1 -7 2039.84 100.644 8
0 0 0 0.00 0.00 0
TITL T4 in Pbca
REM Pbca (#61, found as Pcab in ba-c setting)
CELL 1.54184 10.991880 6.994535 26.407628 90.0000 90.0000 90.0000
ZERR 9.00 0.000162 0.000124 0.000375 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N S Br I
UNIT 72.00 36.00 18.00 9.00 9.00 9.00
SIZE 0.01 0.04 0.05
TREF
HKLF 4
END
;
_shelx_hkl_checksum 73294
_shelx_res_file
;
TITL T4_a.res in Pbca
T4.res
created by SHELXL-2018/3 at 23:44:44 on 05-Nov-2022
REM Old TITL T4 in Pbca
REM SHELXT solution in Pbca: R1 0.100, Rweak 0.001, Alpha 0.015
REM 0.616 for 329 systematic absences, Orientation as input
REM Formula found by SHELXT: C10 N S Br I
CELL 1.54184 10.9919 6.9945 26.4076 90 90 90
ZERR 8 0.0002 0.0001 0.0004 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Br I N S
UNIT 64 32 8 8 16 8
L.S. 10
PLAN 1
CONF
MORE -1
BOND $H
fmap 2
acta
REM
REM
REM
WGHT 0.021900 2.646400
FVAR 1.04085
C1 1 0.672925 0.373176 0.408368 11.00000 0.02092 0.02114 =
0.01841 -0.00284 0.00000 0.00076
C2 1 0.555074 0.400880 0.388957 11.00000 0.01898 0.02911 =
0.02036 -0.00397 -0.00096 0.00193
AFIX 43
H2 2 0.487684 0.378054 0.409375 11.00000 -1.20000
AFIX 0
C3 1 0.539152 0.461914 0.339639 11.00000 0.02437 0.03026 =
0.02108 -0.00440 -0.00462 0.00207
AFIX 43
H3 2 0.461242 0.482985 0.327092 11.00000 -1.20000
AFIX 0
C4 1 0.639145 0.491504 0.309066 11.00000 0.03216 0.02605 =
0.01524 -0.00214 -0.00249 0.00106
C5 1 0.757131 0.465062 0.327102 11.00000 0.02458 0.02594 =
0.01919 -0.00130 0.00302 0.00085
AFIX 43
H5 2 0.823891 0.487009 0.306263 11.00000 -1.20000
AFIX 0
C6 1 0.772980 0.405297 0.376805 11.00000 0.02021 0.02356 =
0.02139 -0.00041 -0.00029 -0.00166
AFIX 43
H6 2 0.851192 0.386382 0.389268 11.00000 -1.20000
AFIX 0
C7 1 0.693091 0.309732 0.460553 11.00000 0.01578 0.02437 =
0.02136 -0.00257 0.00221 0.00114
N8 5 0.802172 0.285060 0.479359 11.00000 0.01702 0.03416 =
0.01746 -0.00037 -0.00002 0.00045
N9 5 0.800640 0.225462 0.529082 11.00000 0.02014 0.03314 =
0.01760 -0.00066 -0.00085 0.00252
C10 1 0.690045 0.208145 0.545331 11.00000 0.02211 0.02670 =
0.01855 0.00104 -0.00079 0.00205
S11 6 0.576812 0.259394 0.502820 11.00000 0.01554 0.03432 =
0.02008 0.00398 0.00124 0.00069
BR12 3 0.656989 0.133988 0.612203 11.00000 0.02913 0.03565 =
0.01864 0.00393 0.00365 0.00341
I13 4 0.614711 0.587796 0.234555 11.00000 0.04468 0.03386 =
0.01605 0.00102 -0.00390 0.00057
HKLF 4
REM T4_a.res in Pbca
REM wR2 = 0.0517, GooF = S = 1.070, Restrained GooF = 1.070 for all data
REM R1 = 0.0210 for 1802 Fo > 4sig(Fo) and 0.0229 for all 1920 data
REM 118 parameters refined using 0 restraints
END
WGHT 0.0219 2.6466
REM Highest difference peak 0.566, deepest hole -0.669, 1-sigma level 0.089
Q1 1 0.6156 0.5816 0.1969 11.00000 0.05 0.57
;
_shelx_res_checksum 16669
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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
C C1 0.6729(3) 0.3732(4) 0.40837(11) 0.0202(6) Uani d 1 . .
C C2 0.5551(3) 0.4009(4) 0.38896(11) 0.0228(7) Uani d 1 . .
H H2 0.487684 0.378054 0.409375 0.027 Uiso calc 1 . .
C C3 0.5392(3) 0.4619(5) 0.33964(11) 0.0252(7) Uani d 1 . .
H H3 0.461242 0.482985 0.327092 0.030 Uiso calc 1 . .
C C4 0.6391(3) 0.4915(5) 0.30907(11) 0.0245(7) Uani d 1 . .
C C5 0.7571(3) 0.4651(5) 0.32710(11) 0.0232(6) Uani d 1 . .
H H5 0.823891 0.487009 0.306263 0.028 Uiso calc 1 . .
C C6 0.7730(3) 0.4053(4) 0.37681(12) 0.0217(6) Uani d 1 . .
H H6 0.851192 0.386382 0.389268 0.026 Uiso calc 1 . .
C C7 0.6931(3) 0.3097(5) 0.46055(11) 0.0205(6) Uani d 1 . .
N N8 0.8022(2) 0.2851(4) 0.47936(9) 0.0229(6) Uani d 1 . .
N N9 0.8006(2) 0.2255(4) 0.52908(9) 0.0236(6) Uani d 1 . .
C C10 0.6900(3) 0.2081(5) 0.54533(11) 0.0225(6) Uani d 1 . .
S S11 0.57681(6) 0.25939(12) 0.50282(3) 0.02332(17) Uani d 1 . .
Br Br12 0.65699(3) 0.13399(5) 0.61220(2) 0.02781(10) Uani d 1 . .
I I13 0.61471(2) 0.58780(3) 0.23455(2) 0.03153(9) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0209(14) 0.0211(16) 0.0184(15) 0.0008(12) 0.0000(12) -0.0028(11)
C2 0.0190(15) 0.0291(18) 0.0204(15) 0.0019(12) -0.0010(12) -0.0040(12)
C3 0.0244(15) 0.0303(18) 0.0211(14) 0.0021(14) -0.0046(13) -0.0044(13)
C4 0.0322(16) 0.0261(17) 0.0152(14) 0.0011(14) -0.0025(12) -0.0021(13)
C5 0.0246(14) 0.0259(17) 0.0192(14) 0.0008(13) 0.0030(12) -0.0013(13)
C6 0.0202(14) 0.0236(16) 0.0214(15) -0.0017(12) -0.0003(12) -0.0004(12)
C7 0.0158(13) 0.0244(16) 0.0214(14) 0.0011(13) 0.0022(11) -0.0026(12)
N8 0.0170(12) 0.0342(15) 0.0175(12) 0.0005(12) 0.0000(9) -0.0004(11)
N9 0.0201(12) 0.0331(15) 0.0176(12) 0.0025(12) -0.0008(10) -0.0007(11)
C10 0.0221(14) 0.0267(16) 0.0185(14) 0.0021(13) -0.0008(12) 0.0010(12)
S11 0.0155(3) 0.0343(4) 0.0201(3) 0.0007(3) 0.0012(3) 0.0040(3)
Br12 0.02913(18) 0.0356(2) 0.01864(17) 0.00341(15) 0.00365(13) 0.00393(13)
I13 0.04468(15) 0.03386(14) 0.01605(12) 0.00057(10) -0.00390(8) 0.00102(8)
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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0038
0 0 -1 0.0078
0 -1 0 0.0231
0 1 0 0.0251
-3 0 2 0.0133
3 0 -2 0.0213
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
C2 C1 C7 . . 121.6(3) ?
C6 C1 C2 . . 119.0(3) ?
C6 C1 C7 . . 119.4(3) ?
C1 C2 H2 . . 119.9 ?
C3 C2 C1 . . 120.2(3) ?
C3 C2 H2 . . 119.9 ?
C2 C3 H3 . . 120.1 ?
C4 C3 C2 . . 119.8(3) ?
C4 C3 H3 . . 120.1 ?
C3 C4 C5 . . 121.4(3) ?
C3 C4 I13 . . 119.7(2) ?
C5 C4 I13 . . 118.8(2) ?
C4 C5 H5 . . 120.7 ?
C6 C5 C4 . . 118.7(3) ?
C6 C5 H5 . . 120.7 ?
C1 C6 H6 . . 119.6 ?
C5 C6 C1 . . 120.9(3) ?
C5 C6 H6 . . 119.6 ?
C1 C7 S11 . . 123.8(2) ?
N8 C7 C1 . . 122.4(3) ?
N8 C7 S11 . . 113.9(2) ?
C7 N8 N9 . . 113.0(2) ?
C10 N9 N8 . . 110.8(2) ?
N9 C10 S11 . . 116.4(2) ?
N9 C10 Br12 . . 121.3(2) ?
S11 C10 Br12 . . 122.26(17) ?
C10 S11 C7 . . 85.92(14) ?
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
C1 C2 . 1.407(4) ?
C1 C6 . 1.398(4) ?
C1 C7 . 1.465(4) ?
C2 H2 . 0.9300 ?
C2 C3 . 1.382(4) ?
C3 H3 . 0.9300 ?
C3 C4 . 1.379(4) ?
C4 C5 . 1.394(4) ?
C4 I13 . 2.097(3) ?
C5 H5 . 0.9300 ?
C5 C6 . 1.388(4) ?
C6 H6 . 0.9300 ?
C7 N8 . 1.309(4) ?
C7 S11 . 1.733(3) ?
N8 N9 . 1.378(3) ?
N9 C10 . 1.295(4) ?
C10 S11 . 1.714(3) ?
C10 Br12 . 1.876(3) ?
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 C2 C3 C4 . . . . 1.5(5) ?
C1 C7 N8 N9 . . . . 179.9(3) ?
C1 C7 S11 C10 . . . . -179.7(3) ?
C2 C1 C6 C5 . . . . 0.5(5) ?
C2 C1 C7 N8 . . . . -179.3(3) ?
C2 C1 C7 S11 . . . . 1.0(4) ?
C2 C3 C4 C5 . . . . -1.4(5) ?
C2 C3 C4 I13 . . . . -179.2(2) ?
C3 C4 C5 C6 . . . . 0.8(5) ?
C4 C5 C6 C1 . . . . -0.4(5) ?
C6 C1 C2 C3 . . . . -1.0(5) ?
C6 C1 C7 N8 . . . . 1.3(5) ?
C6 C1 C7 S11 . . . . -178.3(2) ?
C7 C1 C2 C3 . . . . 179.6(3) ?
C7 C1 C6 C5 . . . . 179.8(3) ?
C7 N8 N9 C10 . . . . 0.0(4) ?
N8 C7 S11 C10 . . . . 0.6(3) ?
N8 N9 C10 S11 . . . . 0.5(4) ?
N8 N9 C10 Br12 . . . . -178.7(2) ?
N9 C10 S11 C7 . . . . -0.6(3) ?
S11 C7 N8 N9 . . . . -0.5(4) ?
Br12 C10 S11 C7 . . . . 178.6(2) ?
I13 C4 C5 C6 . . . . 178.6(2) ?
_cod_database_fobs_code 2022698