#------------------------------------------------------------------------------
#$Date: 2024-06-29 04:58:11 +0300 (Sat, 29 Jun 2024) $
#$Revision: 292658 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023184.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_2023184
loop_
_publ_author_name
'Brydson, Rowan K. H.'
'Kennedy, Alan R.'
_publ_section_title
;
A monoclinic polymorph of chlorothiazide
;
_journal_coeditor_code VU2004
_journal_issue 7
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 806
_journal_page_last 810
_journal_paper_doi 10.1107/S2056989024006078
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C7 H6 Cl N3 O4 S2'
_chemical_formula_moiety 'C7 H6 Cl N3 O4 S2'
_chemical_formula_sum 'C7 H6 Cl N3 O4 S2'
_chemical_formula_weight 295.72
_chemical_name_common
;
Chlorothiazide
;
_chemical_name_systematic
;
6-Chloro-1,1-dioxo-2H-1,2,4-benzothiazine-7-sulfonamide
;
_space_group_crystal_system monoclinic
_space_group_IT_number 4
_space_group_name_Hall 'P 2yb'
_space_group_name_H-M_alt 'P 1 21 1'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 92.2140(10)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 4.82960(10)
_cell_length_b 6.27030(10)
_cell_length_c 16.9551(2)
_cell_measurement_reflns_used 6651
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 71.2840
_cell_measurement_theta_min 2.5930
_cell_volume 513.069(15)
_computing_cell_refinement
;
CrysalisPro (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysalisPro (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysalisPro (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
MERCURY (Macrae et al., 2020)
;
_computing_publication_material
;
SHELXL2018 in WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Rigaku Synergy-i'
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0464
_diffrn_reflns_av_unetI/netI 0.0365
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 8271
_diffrn_reflns_theta_full 70.000
_diffrn_reflns_theta_max 71.406
_diffrn_reflns_theta_min 2.608
_diffrn_source 'microsource tube'
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 7.230
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.3933
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.914
_exptl_crystal_description tablet
_exptl_crystal_F_000 300
_exptl_crystal_size_max 0.23
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.05
_refine_diff_density_max 0.280
_refine_diff_density_min -0.333
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.00(2)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.061
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 167
_refine_ls_number_reflns 1953
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.060
_refine_ls_R_factor_all 0.0289
_refine_ls_R_factor_gt 0.0281
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.0232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0774
_refine_ls_wR_factor_ref 0.0779
_reflns_number_gt 1895
_reflns_number_total 1953
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vu2004.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21'
_cod_database_code 2023184
_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 -7 0-37.9020 50.6042 43
0 -7 -1 16892.5 751.488 43
0 -7 -1 16704.9 774.845 16
0 -7 2 95.7096 55.8848 43
0 -7 3 4843.44 305.481 43
0 -7 4 1368.91 140.026 43
0 -7 5 1281.40 134.646 43
0 -7 6 483.904 80.4051 43
0 -7 6 630.258 89.7250 22
0 -7 7 1393.99 131.939 43
0 -7 7 1539.45 139.173 22
0 -7 8 286.339 60.3548 43
0 -7 8 422.955 69.3157 22
0 -6 0 15561.1 799.149 43
0 -6 0 14765.2 812.083 16
0 -6 0 15821.0 828.345 30
0 -6 1 5877.82 402.053 16
0 -6 -1 5880.57 411.311 30
0 -6 1 5632.71 378.740 43
0 -6 -1 5496.54 393.088 16
0 -6 -1 5929.47 383.615 43
0 -6 2 1537.29 183.805 16
0 -6 2 1233.96 161.360 43
0 -6 -2 1679.13 197.939 30
0 -6 -2 1625.42 186.567 16
0 -6 -2 1711.84 178.311 43
0 -6 3 2226.27 222.057 43
0 -6 3 2827.24 254.815 16
0 -6 3 2785.64 242.159 22
0 -6 -3 3157.86 266.871 30
0 -6 -3 2904.44 240.159 43
0 -6 4 4114.95 341.075 16
0 -6 4 4684.54 335.194 43
0 -6 4 5003.58 349.352 22
0 -6 5 559.764 114.920 22
0 -6 5 368.047 96.5784 43
0 -6 -5 588.777 116.771 30
0 -6 -6 6183.12 387.719 24
0 -6 -6 7019.27 411.234 30
0 -6 6 5921.50 400.040 22
0 -6 -7 11478.5 578.110 30
0 -6 7 8676.10 551.502 43
0 -6 -7 10689.1 564.700 24
0 -6 7 9424.70 570.876 22
0 -6 8 1104.34 161.675 22
0 -6 -8 1518.54 155.299 24
0 -6 -9 4232.85 273.051 24
0 -6 9 3610.56 290.276 22
0 -6 10 3061.34 260.914 22
0 -6 -10 3982.07 248.126 24
0 -6 -11 4836.85 273.525 24
0 -6 11 4019.23 290.337 22
0 -6 12 790.777 100.238 43
0 -6 12 981.616 114.069 22
0 -6 13 2643.74 182.135 22
0 -5 0-18.4300 66.3878 16
0 -5 0-10.1707 65.2961 30
0 -5 0-8.41944 58.8457 43
0 -5 -1 6982.42 446.012 30
0 -5 1 6448.81 426.046 16
0 -5 -1 7297.96 437.751 16
0 -5 -2 2134.48 200.231 24
0 -5 -2 2573.85 236.218 30
0 -5 -2 2311.63 213.820 16
0 -5 2 2447.76 215.507 22
0 -5 2 2300.13 218.991 16
0 -5 3 20114.7 992.982 22
0 -5 -3 18920.1 974.381 24
0 -5 3 18785.3 1103.01 14
0 -5 3 19764.6 996.590 16
0 -5 -3 22085.9 1027.51 30
0 -5 4 3178.31 265.184 22
0 -5 -4 3070.96 245.909 24
0 -5 4 2736.80 251.788 16
0 -5 4 3220.53 343.746 14
0 -5 -4 2967.90 260.976 30
0 -5 -5 2762.82 242.613 30
0 -5 5 2392.00 233.297 16
0 -5 5 2440.86 239.485 22
0 -5 -5 2408.78 213.580 24
0 -5 6 1330.71 176.276 16
0 -5 -6 1352.49 156.263 24
0 -5 6 1454.52 186.802 22
0 -5 -6 1508.96 173.986 30
0 -5 7 21554.9 1119.28 22
0 -5 -7 22723.3 1091.42 30
0 -5 -7 22281.7 1084.25 24
0 -5 -8 4113.88 293.346 30
0 -5 -8 3931.48 290.962 24
0 -5 8 3615.10 320.655 22
0 -5 -9 4563.54 311.451 24
0 -5 9 3819.10 332.371 22
0 -5 -10 9467.85 518.029 24
0 -5 10 8451.78 549.280 22
0 -5 11 2800.85 266.706 22
0 -5 -11 3082.93 234.067 24
0 -5 -12 3925.61 266.160 24
0 -5 12 3790.64 298.951 22
0 -5 -13 452.013 78.1763 24
0 -5 13 337.831 88.5748 22
0 -5 14 9007.51 520.797 22
0 -5 -14 10777.1 508.653 24
0 -5 15 2014.08 160.284 22
0 -4 0 8472.44 537.267 14
0 -4 1 7893.64 512.356 14
0 -4 -1 8165.73 430.472 43
0 -4 1 7101.87 431.244 41
0 -4 -2 1794.77 175.575 30
0 -4 2 1729.49 213.157 14
0 -4 2 1569.51 157.595 16
0 -4 -2 1580.81 148.162 24
0 -4 2 1764.82 170.279 41
0 -4 3 1184.12 144.074 41
0 -4 3 1356.17 141.710 22
0 -4 -3 1492.17 138.324 43
0 -4 -3 1106.62 120.095 24
0 -4 3 943.735 126.230 16
0 -4 3 1343.20 185.379 14
0 -4 -3 1227.40 146.447 30
0 -4 4 16018.6 927.197 14
0 -4 -4 16845.2 838.399 30
0 -4 -4 17609.9 918.305 55
0 -4 4 16464.7 827.333 16
0 -4 4 17724.4 856.494 41
0 -4 -4 16163.7 803.747 24
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0 -4 -5 4605.27 304.356 30
0 -4 5 4356.58 310.810 22
0 -4 5 4651.55 324.588 41
0 -4 5 4088.34 294.587 16
0 -4 5 4012.84 374.765 14
0 -4 -5 4338.38 362.758 55
0 -4 -5 4169.41 279.113 24
0 -4 -6 11846.4 604.402 24
0 -4 6 12344.3 654.731 41
0 -4 6 10728.4 612.797 16
0 -4 6 11629.5 641.092 22
0 -4 -6 11979.4 619.324 30
0 -4 6 9860.06 718.234 14
0 -4 -6 12223.8 731.326 55
0 -4 -7 27984.4 1427.19 55
0 -4 7 26081.6 1453.32 14
0 -4 7 29133.1 1330.81 22
0 -4 7 24165.7 1278.62 16
0 -4 -7 29614.3 1284.59 24
0 -4 8 12252.0 855.634 14
0 -4 -8 13148.6 819.711 55
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0 -4 8 13977.5 735.681 22
0 -4 9 8403.35 535.343 22
0 -4 9 7621.43 651.799 14
0 -4 -9 8505.10 486.877 23
0 -4 -9 9021.37 633.258 55
0 -4 -9 8744.29 495.228 24
0 -4 -10 4810.52 326.595 23
0 -4 10 5177.93 383.576 22
0 -4 -10 4643.80 327.402 24
0 -4 -11 8318.06 494.521 23
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0 -4 11 9467.49 563.072 22
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0 -4 14 1799.08 192.914 28
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0 -4 -14 1992.64 176.543 23
0 -4 15 1864.22 179.662 28
0 -4 15 1744.24 176.705 22
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0 -4 -15 1696.57 152.338 23
0 -4 16 359.437 80.4103 28
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0 -4 17 4639.67 268.085 28
0 -4 -17 3977.97 236.881 24
0 -3 1 13452.3 692.002 14
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0 -3 2 13609.9 728.160 14
0 -3 -2 13949.6 704.004 5
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0 -3 3 1780.40 191.155 14
0 -3 4 7378.94 475.797 14
0 -3 -4 7593.24 465.940 55
0 -3 4 7491.07 466.540 12
0 -3 5 1331.54 174.430 12
0 -3 5 1389.03 181.481 14
0 -3 -5 1541.20 182.002 55
0 -3 6 10295.9 673.123 14
0 -3 6 11690.5 687.853 12
0 -3 -6 11793.0 672.138 55
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0 -3 -8 31891.1 1335.04 29
0 -3 8 26868.6 1467.49 12
0 -3 -8 30451.9 1321.71 21
0 -3 8 27765.6 1335.50 22
0 -3 8 24289.3 1447.35 14
0 -3 -8 26906.1 1290.59 23
0 -3 -8 27252.7 1421.96 55
0 -3 -8 28463.5 1298.80 24
0 -3 -9 4796.81 312.008 29
0 -3 9 4025.27 316.650 28
0 -3 9 4117.76 413.730 14
0 -3 9 3929.35 310.580 22
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0 -3 -10 12436.2 653.215 24
0 -3 -10 11643.1 647.736 23
0 -3 10 12611.6 699.334 22
0 -3 -10 12782.4 783.628 55
0 -3 -11 1636.06 230.534 55
0 -3 11 1531.88 269.967 14
0 -3 -11 1670.12 169.897 23
0 -3 11 1412.65 254.590 12
0 -3 11 1570.17 198.827 28
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0 -3 12 2123.38 231.897 22
0 -3 -12 2926.93 236.058 21
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0 -3 -13 118.697 58.7003 23
0 -3 13 121.788 80.0380 22
0 -3 13 318.197 108.187 28
0 -3 -13 167.584 61.6061 24
0 -3 -13 174.233 74.0206 29
0 -3 -14 8040.47 473.893 29
0 -3 -14 7198.84 444.494 24
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0 -3 14 7132.29 483.567 28
0 -3 -15 951.037 131.215 29
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0 -3 -15 1062.12 132.030 23
0 -3 -15 959.157 127.646 24
0 -3 -16 1997.93 174.262 23
0 -3 -16 1850.48 169.334 24
0 -3 16 1788.39 191.129 28
0 -3 -17 228.926 60.6024 24
0 -3 17 254.381 74.8448 28
0 -3 -17 254.181 60.8884 23
0 -3 -18 1952.89 153.393 24
0 -3 -18 2122.92 158.075 23
0 -3 19 756.230 85.9418 28
0 -2 0 123998. 5353.04 55
0 -2 0 127688. 5369.27 5
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0 -2 -3 1235.31 129.925 55
0 -2 3 1155.54 128.281 12
0 -2 3 1436.68 144.157 14
0 -2 -3 1355.84 112.946 5
0 -2 -4 60005.0 2569.25 55
0 -2 4 57258.0 2570.44 12
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0 -2 -5 1610.55 166.398 55
0 -2 5 1416.57 169.710 12
0 -2 6 6526.09 452.957 12
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0 -2 8 14922.9 871.669 12
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0 -2 9 13956.3 875.487 14
0 -2 -9 14559.3 808.184 55
0 -2 9 14897.8 880.502 12
0 -2 10 2057.09 211.444 28
0 -2 10 1783.14 271.978 14
0 -2 -10 2381.46 196.526 29
0 -2 -10 2065.70 184.445 21
0 -2 10 2038.78 277.400 12
0 -2 -10 2336.52 202.337 20
0 -2 -10 2211.61 240.998 55
0 -2 11 4459.21 450.826 14
0 -2 -11 5162.13 343.535 20
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0 -2 -11 4731.36 321.643 21
0 -2 11 5060.16 456.905 12
0 -2 -11 5170.51 330.862 29
0 -2 -11 4910.87 394.031 55
0 -2 11 4308.96 344.693 28
0 -2 12 1462.62 241.352 12
0 -2 -12 1217.24 150.344 29
0 -2 -12 1608.70 175.617 20
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0 -2 -12 1287.85 144.950 23
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0 -2 -14 3661.50 276.843 23
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0 -2 -15 2583.00 238.812 20
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0 -2 16 1697.86 195.499 28
0 -2 -17 10572.1 567.424 23
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0 -1 -2 820.283 73.6997 3
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0 -1 2 750.597 90.2450 50
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0 -1 2 786.545 66.5205 10
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0 -1 5 12480.6 656.250 1
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0 -1 8 55074.4 2455.00 12
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5 2 -1 1876.68 259.140 31
5 2 0 135.785 96.4286 42
5 2 0 19.5443 69.4357 39
5 2 0 226.435 150.676 33
5 2 1 679.331 156.316 42
5 2 1 784.124 201.940 33
5 2 2 1547.04 226.225 42
5 2 2 1857.69 299.627 33
5 2 3 5838.06 459.056 42
5 2 3 6973.63 583.511 33
5 2 4 675.575 151.458 42
5 2 4 1023.21 235.321 33
5 2 5 4686.80 371.839 42
5 2 5 4948.76 454.922 33
5 2 6 398.261 108.387 42
5 2 6 349.823 151.735 33
5 2 7 2682.27 251.250 42
5 2 7 3510.31 336.387 38
-5 2 -7 3089.50 195.217 34
5 2 7 2921.62 300.477 33
5 2 8 3259.31 292.605 38
-5 2 -8 2937.05 182.503 34
5 2 8 2465.62 255.383 33
5 3 -8 301.373 70.4639 25
5 3 -8 430.223 79.5698 31
5 3 -7 688.260 109.194 25
5 3 -7 738.439 89.3874 39
5 3 -7 888.877 127.337 31
5 3 -6 2187.91 215.992 25
5 3 -6 2282.14 183.279 39
5 3 -6 2373.94 228.328 31
5 3 -5 1337.52 181.255 25
5 3 -5 1425.79 149.040 39
5 3 -5 1429.05 190.739 31
5 3 -4 770.700 147.407 25
5 3 -4 647.550 111.506 39
5 3 -4 824.293 146.546 31
5 3 -3 222.833 109.675 25
5 3 -3 371.572 100.120 39
5 3 -3 541.090 129.207 31
5 3 -2 2741.78 293.494 25
5 3 -2 2614.01 240.074 42
5 3 -2 2545.16 233.439 39
5 3 -2 2333.14 269.534 31
5 3 -1 1961.81 262.140 25
5 3 -1 2554.89 244.578 42
5 3 -1 1807.70 197.172 39
5 3 -1 2114.84 255.759 31
5 3 0 1160.20 185.710 42
5 3 0 753.253 175.026 31
5 3 1 3007.97 302.632 42
5 3 1 3859.44 391.812 33
5 3 1 3103.60 310.277 31
5 3 2 4912.67 397.391 42
5 3 2 6094.37 508.667 33
5 3 2 4925.87 404.789 31
5 3 3 3885.49 341.921 42
5 3 3 4768.80 462.136 33
5 3 3 4594.10 376.922 31
5 3 4 2756.45 262.592 42
5 3 4 3186.97 362.407 33
5 3 5 3316.59 274.308 42
-5 3 -5 3172.05 198.005 34
5 3 5 3449.74 363.624 33
-5 3 -6 1553.43 117.923 34
5 3 6 1690.35 230.878 33
5 4 -3 1116.00 143.997 25
5 4 -3 1211.69 148.730 31
5 4 -2 697.109 124.168 25
5 4 -2 645.689 119.464 31
5 4 -1 310.459 110.129 25
5 4 -1 353.806 93.7864 31
5 4 0 1458.84 196.278 25
5 4 0 1090.42 154.522 31
5 4 1 1980.27 214.792 31
5 4 2 676.416 142.560 31
0 0 0 0.00 0.00 0
TITL rowan_Ba_smart in P2(1)
REM P2(1) (#4 in standard setting)
CELL 1.54184 4.829647 6.270335 16.955114 90.0000 92.2141 90.0000
ZERR 1.00 0.000063 0.000092 0.000211 0.0000 0.0012 0.0000
LATT -1
SYMM -x, y+1/2,-z
SFAC C N O Cl Ba
UNIT 30.00 4.00 12.00 2.00 1.00
REM CrysAlisPro recorded range (K): Min=99.7; max=100.2; aver:100.0
TEMP -173
TREF
HKLF 4
END
;
_shelx_hkl_checksum 97637
_shelx_res_file
;
TITL shelxt_a.res in P2(1)
shelx.res
created by SHELXL-2018/3 at 12:50:44 on 17-Jun-2024
CELL 1.54184 4.8296 6.2703 16.9551 90.000 92.214 90.000
ZERR 2.00 0.0001 0.0001 0.0002 0.000 0.001 0.000
LATT -1
SYMM - X, 1/2 + Y, - Z
SFAC S CL O N C H
UNIT 4 2 8 6 14 12
MERG 2
OMIT -3.00 180.00
TWIN
dfix .88 .01 n2 h1n n3 h2n n3 h3n
EQIV $1 x, y+1, z
HTAB N2 O1_$1
EQIV $2 -x+1, y+1/2, -z
HTAB N3 O4_$2
EQIV $3 x+1, y, z
HTAB N3 O4_$3
EQIV $4 -x+2, y+1/2, -z
HTAB N3 O3_$4
FMAP 2
PLAN 20
ACTA 140.00
BOND $H
CONF
L.S. 24
TEMP -173.00
WGHT 0.051800 0.023200
BASF 0.00306
FVAR 4.09504
S1 1 1.241467 -0.056445 0.375966 11.00000 0.01884 0.01378 =
0.01526 -0.00040 -0.00157 0.00040
S2 1 0.690839 -0.054791 0.091492 11.00000 0.01703 0.01662 =
0.01433 -0.00127 -0.00021 -0.00150
CL1 2 0.390024 0.392397 0.146827 11.00000 0.02159 0.01792 =
0.02266 0.00334 -0.00375 0.00140
O1 3 1.062920 -0.177796 0.425727 11.00000 0.02485 0.01527 =
0.01899 0.00119 0.00136 0.00072
O2 3 1.452468 -0.175120 0.338340 11.00000 0.01921 0.02130 =
0.02185 -0.00128 -0.00094 0.00555
O3 3 0.830797 -0.255768 0.096686 11.00000 0.02296 0.01312 =
0.02094 -0.00200 0.00091 -0.00123
O4 3 0.397202 -0.052697 0.074471 11.00000 0.01799 0.02411 =
0.01977 -0.00359 0.00001 -0.00207
N1 4 1.382229 0.131140 0.429648 11.00000 0.02394 0.01628 =
0.01817 -0.00268 -0.00420 -0.00164
N2 4 1.037773 0.384199 0.389873 11.00000 0.02350 0.01597 =
0.01704 -0.00310 -0.00049 -0.00058
N3 4 0.829253 0.084318 0.025244 11.00000 0.01907 0.02137 =
0.01880 0.00421 0.00042 0.00041
C4 5 1.257733 0.315880 0.433900 11.00000 0.02342 0.02119 =
0.01455 0.00083 0.00137 -0.00521
AFIX 43
H4 6 1.331004 0.412655 0.472437 11.00000 -1.20000
AFIX 0
C5 5 0.931870 0.276681 0.323607 11.00000 0.01980 0.01406 =
0.01663 0.00025 0.00290 -0.00311
C6 5 1.033537 0.075280 0.305446 11.00000 0.01670 0.01381 =
0.01512 0.00145 0.00038 0.00029
C7 5 0.955016 -0.023223 0.234465 11.00000 0.01721 0.01275 =
0.01872 0.00104 0.00121 0.00028
AFIX 43
H7 6 1.034802 -0.155951 0.220703 11.00000 -1.20000
AFIX 0
C8 5 0.759779 0.073074 0.183849 11.00000 0.01556 0.01507 =
0.01513 0.00083 -0.00022 -0.00198
C9 5 0.644385 0.270231 0.205194 11.00000 0.01699 0.01839 =
0.01794 0.00460 0.00039 -0.00106
C10 5 0.731951 0.373950 0.273954 11.00000 0.02031 0.01393 =
0.01870 0.00061 0.00305 0.00182
AFIX 43
H10 6 0.657180 0.508943 0.287066 11.00000 -1.20000
AFIX 0
H1N 6 0.989105 0.513765 0.402549 11.00000 0.01996
H2N 6 0.730905 0.192724 0.006812 11.00000 0.02233
H3N 6 1.008880 0.098515 0.028305 11.00000 0.03687
HKLF 4
REM shelxt_a.res in P2(1)
REM wR2 = 0.0779, GooF = S = 1.061, Restrained GooF = 1.060 for all data
REM R1 = 0.0281 for 1895 Fo > 4sig(Fo) and 0.0289 for all 1953 data
REM 167 parameters refined using 4 restraints
END
WGHT 0.0518 0.0232
REM Highest difference peak 0.280, deepest hole -0.333, 1-sigma level 0.071
Q1 1 0.3963 0.1059 0.2555 11.00000 0.05 0.28
Q2 1 0.6455 0.2423 -0.0401 11.00000 0.05 0.27
Q3 1 1.3903 -0.3015 0.2173 11.00000 0.05 0.26
Q4 1 0.8541 0.4367 0.1962 11.00000 0.05 0.23
Q5 1 0.6444 -0.1567 -0.0223 11.00000 0.05 0.23
Q6 1 0.3525 0.1136 0.0349 11.00000 0.05 0.22
Q7 1 0.3470 0.0784 0.0902 11.00000 0.05 0.22
Q8 1 0.9677 -0.1604 0.4250 11.00000 0.05 0.21
Q9 1 0.7112 -0.3458 0.1899 11.00000 0.05 0.21
Q10 1 0.3561 0.5081 0.0798 11.00000 0.05 0.19
Q11 1 0.4027 -0.3174 0.0947 11.00000 0.05 0.19
Q12 1 0.9510 0.1181 0.3190 11.00000 0.05 0.19
Q13 1 0.3047 -0.0820 0.0998 11.00000 0.05 0.19
Q14 1 0.6610 0.2524 0.0489 11.00000 0.05 0.19
Q15 1 0.7510 -0.1996 0.2670 11.00000 0.05 0.19
Q16 1 1.3869 -0.3306 0.3178 11.00000 0.05 0.19
Q17 1 0.7023 0.2269 0.2007 11.00000 0.05 0.19
Q18 1 1.0917 -0.0621 0.4257 11.00000 0.05 0.18
Q19 1 0.9020 0.0766 0.0198 11.00000 0.05 0.18
Q20 1 1.4040 -0.0403 0.3248 11.00000 0.05 0.18
;
_shelx_res_checksum 44610
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, 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
S S1 1.24147(16) -0.05644(13) 0.37597(4) 0.0160(2) Uani d 1 . .
S S2 0.69084(16) -0.05479(14) 0.09149(4) 0.0160(2) Uani d 1 . .
Cl Cl1 0.39002(17) 0.39240(15) 0.14683(5) 0.0208(2) Uani d 1 . .
O O1 1.0629(5) -0.1778(5) 0.42573(14) 0.0197(6) Uani d 1 . .
O O2 1.4525(5) -0.1751(5) 0.33834(15) 0.0208(6) Uani d 1 . .
O O3 0.8308(5) -0.2558(4) 0.09669(15) 0.0190(6) Uani d 1 . .
O O4 0.3972(5) -0.0527(5) 0.07447(14) 0.0206(6) Uani d 1 . .
N N1 1.3822(7) 0.1311(6) 0.42965(18) 0.0196(7) Uani d 1 . .
N N2 1.0378(7) 0.3842(6) 0.38987(18) 0.0189(7) Uani d 1 . .
N N3 0.8293(6) 0.0843(6) 0.02524(17) 0.0198(7) Uani d 1 . .
C C4 1.2577(8) 0.3159(7) 0.4339(2) 0.0197(8) Uani d 1 . .
H H4 1.331004 0.412655 0.472437 0.024 Uiso calc 1 . .
C C5 0.9319(8) 0.2767(6) 0.3236(2) 0.0168(7) Uani d 1 . .
C C6 1.0335(7) 0.0753(7) 0.3054(2) 0.0152(7) Uani d 1 . .
C C7 0.9550(7) -0.0232(7) 0.23446(19) 0.0162(8) Uani d 1 . .
H H7 1.034802 -0.155951 0.220703 0.019 Uiso calc 1 . .
C C8 0.7598(7) 0.0731(6) 0.1838(2) 0.0153(7) Uani d 1 . .
C C9 0.6444(7) 0.2702(6) 0.2052(2) 0.0178(8) Uani d 1 . .
C C10 0.7320(7) 0.3739(7) 0.2740(2) 0.0176(8) Uani d 1 . .
H H10 0.657180 0.508943 0.287066 0.021 Uiso calc 1 . .
H H1N 0.989(9) 0.514(4) 0.403(3) 0.020(12) Uiso d 1 . .
H H2N 0.731(8) 0.193(5) 0.007(3) 0.022(12) Uiso d 1 . .
H H3N 1.009(3) 0.099(10) 0.028(3) 0.037(14) Uiso 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
S1 0.0188(4) 0.0138(5) 0.0153(4) 0.0004(4) -0.0016(3) -0.0004(3)
S2 0.0170(4) 0.0166(5) 0.0143(4) -0.0015(4) -0.0002(3) -0.0013(3)
Cl1 0.0216(4) 0.0179(5) 0.0227(4) 0.0014(4) -0.0037(3) 0.0033(3)
O1 0.0249(14) 0.0153(15) 0.0190(13) 0.0007(11) 0.0014(11) 0.0012(10)
O2 0.0192(12) 0.0213(16) 0.0219(13) 0.0056(11) -0.0009(10) -0.0013(11)
O3 0.0230(13) 0.0131(15) 0.0209(13) -0.0012(11) 0.0009(10) -0.0020(10)
O4 0.0180(12) 0.0241(16) 0.0198(11) -0.0021(12) 0.0000(9) -0.0036(12)
N1 0.0239(16) 0.0163(18) 0.0182(14) -0.0016(14) -0.0042(12) -0.0027(12)
N2 0.0235(16) 0.0160(19) 0.0170(15) -0.0006(14) -0.0005(12) -0.0031(12)
N3 0.0191(16) 0.0214(18) 0.0188(15) 0.0004(14) 0.0004(12) 0.0042(14)
C4 0.0234(19) 0.021(2) 0.0146(17) -0.0052(16) 0.0014(14) 0.0008(16)
C5 0.0198(18) 0.0141(19) 0.0166(16) -0.0031(15) 0.0029(13) 0.0003(15)
C6 0.0167(17) 0.0138(19) 0.0151(15) 0.0003(15) 0.0004(13) 0.0015(14)
C7 0.0172(16) 0.013(2) 0.0187(16) 0.0003(15) 0.0012(12) 0.0010(14)
C8 0.0156(16) 0.0151(19) 0.0151(15) -0.0020(14) -0.0002(13) 0.0008(14)
C9 0.0170(18) 0.018(2) 0.0179(16) -0.0011(16) 0.0004(14) 0.0046(15)
C10 0.0203(17) 0.014(2) 0.0187(17) 0.0018(16) 0.0031(13) 0.0006(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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'
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'
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
O2 S1 O1 . . 115.93(18) ?
O2 S1 N1 . . 109.70(17) ?
O1 S1 N1 . . 107.51(16) ?
O2 S1 C6 . . 110.02(16) ?
O1 S1 C6 . . 108.02(16) ?
N1 S1 C6 . . 105.06(19) ?
O3 S2 O4 . . 118.73(17) ?
O3 S2 N3 . . 108.43(17) ?
O4 S2 N3 . . 106.97(16) ?
O3 S2 C8 . . 105.71(17) ?
O4 S2 C8 . . 108.81(16) ?
N3 S2 C8 . . 107.76(18) ?
C4 N1 S1 . . 119.3(3) ?
C4 N2 C5 . . 123.5(4) ?
C4 N2 H1N . . 112(3) ?
C5 N2 H1N . . 124(3) ?
S2 N3 H2N . . 116(3) ?
S2 N3 H3N . . 117(3) ?
H2N N3 H3N . . 118(5) ?
N1 C4 N2 . . 127.3(4) ?
N1 C4 H4 . . 116.3 ?
N2 C4 H4 . . 116.3 ?
N2 C5 C6 . . 119.7(3) ?
N2 C5 C10 . . 120.0(4) ?
C6 C5 C10 . . 120.3(3) ?
C7 C6 C5 . . 120.4(3) ?
C7 C6 S1 . . 120.9(3) ?
C5 C6 S1 . . 118.5(3) ?
C8 C7 C6 . . 119.8(4) ?
C8 C7 H7 . . 120.1 ?
C6 C7 H7 . . 120.1 ?
C7 C8 C9 . . 119.3(3) ?
C7 C8 S2 . . 116.6(3) ?
C9 C8 S2 . . 124.0(3) ?
C10 C9 C8 . . 121.1(3) ?
C10 C9 Cl1 . . 117.4(3) ?
C8 C9 Cl1 . . 121.4(3) ?
C9 C10 C5 . . 118.9(4) ?
C9 C10 H10 . . 120.5 ?
C5 C10 H10 . . 120.5 ?
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 O2 . 1.432(3) ?
S1 O1 . 1.446(3) ?
S1 N1 . 1.621(3) ?
S1 C6 . 1.740(4) ?
S2 O3 . 1.431(3) ?
S2 O4 . 1.436(2) ?
S2 N3 . 1.590(3) ?
S2 C8 . 1.779(4) ?
Cl1 C9 . 1.727(4) ?
N1 C4 . 1.308(5) ?
N2 C4 . 1.345(5) ?
N2 C5 . 1.391(5) ?
N2 H1N . 0.875(14) ?
N3 H2N . 0.880(14) ?
N3 H3N . 0.872(14) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.394(6) ?
C5 C10 . 1.396(5) ?
C6 C7 . 1.392(5) ?
C7 C8 . 1.388(5) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.409(5) ?
C9 C10 . 1.387(5) ?
C10 H10 . 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
N2 H1N O1 1_565 0.875(14) 2.00(2) 2.815(5) 154(4) yes
N3 H2N O4 2_655 0.880(14) 2.18(2) 3.015(4) 158(4) yes
N3 H3N O4 1_655 0.872(14) 2.22(4) 2.963(4) 143(5) yes
N3 H3N O3 2_755 0.872(14) 2.46(5) 2.870(4) 109(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
O2 S1 N1 C4 . . . . 143.1(3) ?
O1 S1 N1 C4 . . . . -90.0(3) ?
C6 S1 N1 C4 . . . . 24.8(3) ?
S1 N1 C4 N2 . . . . -9.9(5) ?
C5 N2 C4 N1 . . . . -10.0(6) ?
C4 N2 C5 C6 . . . . 7.7(5) ?
C4 N2 C5 C10 . . . . -169.9(3) ?
N2 C5 C6 C7 . . . . -172.1(3) ?
C10 C5 C6 C7 . . . . 5.5(5) ?
N2 C5 C6 S1 . . . . 12.0(5) ?
C10 C5 C6 S1 . . . . -170.4(3) ?
O2 S1 C6 C7 . . . . 40.0(4) ?
O1 S1 C6 C7 . . . . -87.4(3) ?
N1 S1 C6 C7 . . . . 158.0(3) ?
O2 S1 C6 C5 . . . . -144.1(3) ?
O1 S1 C6 C5 . . . . 88.4(3) ?
N1 S1 C6 C5 . . . . -26.1(3) ?
C5 C6 C7 C8 . . . . -4.4(5) ?
S1 C6 C7 C8 . . . . 171.4(3) ?
C6 C7 C8 C9 . . . . 0.2(5) ?
C6 C7 C8 S2 . . . . 175.6(3) ?
O3 S2 C8 C7 . . . . 9.1(3) ?
O4 S2 C8 C7 . . . . 137.6(3) ?
N3 S2 C8 C7 . . . . -106.7(3) ?
O3 S2 C8 C9 . . . . -175.7(3) ?
O4 S2 C8 C9 . . . . -47.1(4) ?
N3 S2 C8 C9 . . . . 68.5(3) ?
C7 C8 C9 C10 . . . . 3.0(5) ?
S2 C8 C9 C10 . . . . -172.1(3) ?
C7 C8 C9 Cl1 . . . . -177.2(3) ?
S2 C8 C9 Cl1 . . . . 7.7(5) ?
C8 C9 C10 C5 . . . . -2.0(5) ?
Cl1 C9 C10 C5 . . . . 178.2(3) ?
N2 C5 C10 C9 . . . . 175.3(3) ?
C6 C5 C10 C9 . . . . -2.3(5) ?