#------------------------------------------------------------------------------
#$Date: 2021-04-06 04:16:15 +0300 (Tue, 06 Apr 2021) $
#$Revision: 263878 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/23/2022325.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_2022325
loop_
_publ_author_name
'Medviediev, Volodymyr'
'Daszkiewicz, Marek'
_publ_section_title
;
Structural and theoretical analysis of 2-chloro-4-nitroaniline and
2-methyl-6-nitroaniline salts
;
_journal_coeditor_code DV3005
_journal_issue 3
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 125
_journal_page_last 136
_journal_paper_doi 10.1107/S2053229621001455
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac 'C6 H6 Cl N2 O2 +, Br -'
_chemical_formula_moiety 'C6 H6 Cl N2 O2 +, Br -'
_chemical_formula_sum 'C6 H6 Br Cl N2 O2'
_chemical_formula_weight 253.49
_chemical_name_systematic
;
2-Chloro-4-nitroanilinium bromide
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.72152(9)
_cell_length_b 7.90017(17)
_cell_length_c 20.2729(4)
_cell_measurement_reflns_used 7548
_cell_measurement_temperature 295.0(10)
_cell_measurement_theta_max 27.3650
_cell_measurement_theta_min 2.7740
_cell_volume 916.35(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2008) and OLEX2 (Dolomanov et al.,
2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 295.0(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Rigaku Xcalibur Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0347
_diffrn_reflns_av_unetI/netI 0.0229
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 18773
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.994
_diffrn_reflns_theta_min 2.767
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 4.738
_exptl_absorpt_correction_T_max 0.446
_exptl_absorpt_correction_T_min 0.300
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
{CrysAlis PRO (Rigaku OD, 2015), based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour 'clear yellowish colourless'
_exptl_crystal_density_diffrn 1.837
_exptl_crystal_description block
_exptl_crystal_F_000 496
_exptl_crystal_size_max 0.358
_exptl_crystal_size_mid 0.261
_exptl_crystal_size_min 0.216
_refine_diff_density_max 0.331
_refine_diff_density_min -0.697
_refine_ls_abs_structure_details
;
Flack x determined using 881 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack -0.008(4)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.127
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 113
_refine_ls_number_reflns 2669
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.127
_refine_ls_R_factor_all 0.0366
_refine_ls_R_factor_gt 0.0278
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0598
_refine_ls_wR_factor_ref 0.0623
_reflns_number_gt 2340
_reflns_number_total 2669
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file dv3005sup1.cif
_cod_data_source_block 1
_cod_depositor_comments
'Adding full bibliography for 2022325--2022329.cif.'
_cod_database_code 2022325
_cod_database_fobs_code 2022325
_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
;
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0 0 -3 1372.28 192.649 9
0 0 3 1436.52 161.528 3
0 0 3 1197.89 180.462 1
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0 0 -4 306630. 5585.80 9
0 0 4 305657. 5553.15 1
0 0 4 306545. 5420.75 3
0 0 -4 295282. 5541.21 1
0 0 -5 545.650 230.477 1
0 0 5-38.1317 234.852 1
0 0 5 204.872 233.540 9
0 0 -5 545.421 274.735 9
0 0 5 484.424 205.429 3
0 0 6 615522. 10898.0 1
0 0 -6 623141. 10966.9 9
0 0 -6 604208. 10962.4 7
0 0 6 588938. 10921.7 9
0 0 6 613652. 10677.6 3
0 0 -6 594610. 10880.4 1
0 0 -7 262.285 276.597 1
0 0 7-192.406 234.749 3
0 0 7-427.758 295.155 9
0 0 -7 36.8172 347.197 9
0 0 7 115.566 330.255 1
0 0 -7 180.142 306.589 7
0 0 8 328811. 6239.70 3
0 0 -8 329707. 6623.72 7
0 0 8 322326. 6562.85 9
0 0 -8 326490. 6515.11 1
0 0 8 323957. 6529.11 1
0 0 -8 335701. 6633.00 9
0 0 -9 574.975 345.593 1
0 0 -9 215.373 364.968 9
0 0 -9 71.4397 362.037 7
0 0 9 122.960 253.997 3
0 0 9-72.4216 329.843 9
0 0 9 6.25635 390.004 1
0 0 -10 116303. 3090.42 1
0 0 -10 114778. 3172.32 7
0 0 10 113870. 2783.99 3
0 0 10 116119. 3093.40 1
0 0 -10 117279. 3194.69 9
0 0 11 42.6883 298.770 3
0 0 11 127.789 453.346 1
0 0 -11 54.7525 415.173 9
0 0 -11-353.301 487.444 7
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0 0 -13 139.285 567.307 7
0 0 -13-696.678 557.668 9
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0 0 14 8241.90 733.571 3
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0 0 -15 23.6927 619.883 9
0 0 -15 598.484 591.546 7
0 0 15 243.032 603.336 1
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0 0 -16 46603.4 2292.48 7
0 0 16 50584.6 1883.84 3
0 0 -17 651.531 748.907 7
0 0 -17 1675.71 866.925 9
0 0 17 371.232 426.997 3
0 0 17-415.668 797.448 1
0 0 18 103660. 3694.19 1
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-7 4 6 4060.51 1392.87 3
7 4 -6 2788.56 1300.64 5
-7 4 6 1713.75 1229.79 8
-7 -4 -5 8592.74 1617.63 7
-7 4 5 4215.53 1397.37 3
7 -4 5 7420.48 1760.64 6
7 4 -5 6084.28 1653.35 5
-7 4 5 7565.33 1758.48 8
-7 -4 -4 5804.39 1440.96 7
-7 4 4 5397.06 1352.96 3
7 -4 4 8899.78 1680.88 6
7 4 -4 8826.51 1824.80 5
-7 4 4 6379.28 1456.89 8
-7 -4 -3-751.404 1156.12 7
-7 4 3 4013.76 1522.81 3
7 -4 3 1524.70 1157.26 6
7 4 -3 2004.86 1514.20 5
-7 4 3 543.141 1161.13 8
-7 -4 -2 10272.4 1616.10 7
-7 4 2 7915.45 1651.97 3
7 -4 2 8551.82 1895.50 6
7 4 -2 8652.93 1863.64 5
-7 4 2 9689.58 1823.70 8
-7 -4 -1 6156.82 1294.86 7
-7 4 1 6138.20 1503.48 3
7 -4 1 7442.55 1706.20 6
7 4 -1 5153.20 1591.53 5
-7 4 1 8952.85 1788.76 8
-7 -4 0-1024.74 917.230 7
-7 4 0 208.893 942.653 3
7 -4 0-166.558 1303.84 6
7 4 0-177.530 1185.00 5
7 4 0 108.683 828.469 4
-7 4 0 302.592 1268.72 8
-7 4 -1 5960.78 1361.39 3
7 -4 -1 9506.60 1814.01 6
7 4 1 6748.25 1606.20 5
7 4 1 6380.14 1192.01 4
-7 4 -1 5733.46 1524.96 8
7 -4 -2 8924.31 1946.01 6
7 4 2 6765.19 1597.26 5
7 4 2 8451.29 1235.22 4
-7 4 -2 4775.75 1327.99 8
7 -4 -3 348.216 1363.00 6
-7 -4 3 5167.11 1410.04 2
7 4 3 1140.20 900.526 4
-7 4 -3 3486.50 1565.05 8
7 -4 -4 6022.04 1499.72 6
-7 -4 4 6628.11 1384.44 2
7 4 4 8551.31 1400.77 4
-7 4 -4 6472.36 1594.85 8
7 -4 -5 5898.03 1460.13 6
-7 -4 5 6116.30 1390.48 2
7 4 5 4883.14 1274.72 4
-7 4 -5 4292.31 1525.72 8
7 -4 -6 2285.09 1217.25 6
-7 -4 6 4144.32 1430.49 2
7 4 6 2684.96 1129.99 4
-7 4 -6 2206.96 1325.79 8
7 -4 -7 4420.29 1437.20 6
7 4 7 8681.67 1457.03 4
-7 4 -7 7624.19 1817.68 8
7 -4 -8 320.946 1259.46 6
-7 -4 8 1118.80 1044.62 2
7 4 8 1923.14 970.974 4
-7 4 -8 1671.86 1353.18 8
7 -4 -9 4156.84 1592.82 6
-7 -4 9 3695.47 1260.57 2
7 4 9 5443.28 1371.99 4
-7 4 -9 4331.48 1486.99 8
7 -4 -10 3426.17 1442.22 6
7 4 10 1820.33 1095.00 4
7 -4 -11 1833.30 1370.43 6
7 4 11 1539.44 948.896 4
-7 4 -11 1314.29 1253.56 8
7 -4 -12 1789.29 1257.80 6
7 4 12 962.267 970.254 4
-7 4 -12 4775.93 1507.58 8
-7 4 -13 375.007 1313.99 8
-7 4 -14-580.179 1275.32 8
-7 5 8 876.733 1231.74 3
-7 5 8-564.150 1057.99 8
-7 -5 -7 5361.40 1456.94 7
-7 5 7 6672.93 1721.70 3
7 -5 7 8467.68 1954.13 6
-7 5 7 8600.97 1890.03 8
-7 -5 -6 3.59572 1125.25 7
-7 5 6-936.306 1428.69 3
7 5 -6-284.520 1480.22 5
-7 5 6 599.273 1068.74 8
-7 -5 -5-637.864 872.784 7
-7 5 5-1920.03 1520.17 3
7 -5 5 2369.38 1565.36 6
7 5 -5-464.781 1446.48 5
-7 5 5 942.409 1421.76 8
-7 -5 -4 2486.15 1227.63 7
-7 5 4 1758.67 1284.85 3
7 -5 4 1320.22 1289.02 6
7 5 -4 2465.53 1553.07 5
-7 5 4 1187.52 1369.73 8
-7 -5 -3 3971.34 1348.85 7
-7 5 3 3373.73 1445.88 3
7 -5 3 4889.85 1615.51 6
7 5 -3 3294.97 1477.89 5
-7 5 3 5622.58 1657.99 8
-7 -5 -2 4339.48 1401.95 7
-7 5 2 6278.47 1495.41 3
7 -5 2 5703.37 1894.56 6
7 5 -2 6836.10 1750.73 5
-7 5 2 7329.20 1692.26 8
-7 -5 -1-17.4802 1147.76 7
-7 5 1 140.612 1143.06 3
7 -5 1 285.059 1365.37 6
7 5 -1 1208.27 869.718 4
-7 5 1 16.6268 1197.18 8
-7 5 0 3740.90 1266.15 3
7 -5 0 384.984 1382.76 6
7 5 0 3015.94 1106.81 4
-7 5 0 2556.12 1273.89 8
-7 5 -1 1377.18 930.344 3
7 -5 -1 1946.29 1469.52 6
7 5 1 1636.09 1006.07 4
-7 5 -1 1125.77 1516.80 8
-7 5 -2 3002.86 1196.60 3
7 -5 -2 7099.61 1918.09 6
-7 -5 2 5561.98 1292.14 2
7 5 2 2749.27 996.233 4
-7 5 -2 6857.00 1875.75 8
7 -5 -3 5230.14 1580.87 6
-7 -5 3 7062.31 1444.70 2
7 5 3 7213.23 1317.80 4
-7 5 -3 5194.06 1626.71 8
7 -5 -4 2524.46 1343.35 6
-7 -5 4 2107.61 1330.69 2
7 5 4 3817.57 1125.56 4
-7 5 -4 2582.29 1381.78 8
7 -5 -5 1344.91 1337.66 6
-7 -5 5 1382.73 1015.20 2
7 5 5 270.171 898.070 4
-7 5 -5 470.834 1458.62 8
7 -5 -6 2652.47 1485.96 6
-7 -5 6 1531.61 1346.69 2
7 5 6-230.746 966.696 4
-7 5 -6-1548.76 1304.07 8
7 -5 -7 4457.44 1542.97 6
7 5 7 5737.74 1424.65 4
-7 5 -7 3201.08 1411.61 8
7 -5 -8 1519.51 1240.24 6
7 5 8-500.028 890.543 4
-7 5 -8-1265.55 1459.92 8
7 5 9 5529.74 1464.64 4
-7 5 -9 7562.54 1807.01 8
-7 6 5 892.153 1247.12 3
-7 6 4 2010.60 1243.20 3
-7 6 3 839.276 1226.44 3
-7 6 2 6602.77 1516.40 3
-7 6 1 954.902 1061.96 3
7 6 -1 4315.27 1252.80 4
-7 6 0 597.740 1054.58 3
7 6 0 202.111 1073.51 4
7 6 1 2019.24 1176.08 4
-7 -6 2 4558.62 1405.21 2
7 6 2 7144.53 1435.43 4
7 6 3 2911.64 1110.50 4
7 6 4 2511.33 1127.10 4
7 6 5 2333.96 1285.04 4
7 6 6 2016.40 1314.09 4
8 0 0 352.385 1074.44 6
8 0 0-906.050 1180.16 5
8 0 1 13359.7 2151.63 6
8 0 -1 12779.7 2149.95 6
8 0 -1 12406.1 1855.79 5
8 0 1 15633.2 2061.72 5
8 0 2 1160.35 1426.78 6
8 0 -2-1314.65 1381.71 6
8 0 -2 661.913 1067.49 5
8 0 2 1857.80 1286.30 5
8 0 3 1553.04 1412.96 6
8 0 -3 1179.41 1126.30 6
8 0 -3 557.427 1071.62 5
8 0 3 519.609 1064.21 5
8 0 -4-1150.05 1327.57 6
8 0 -4 858.485 1261.77 5
8 0 -5 15240.4 2123.18 6
8 0 -5 14826.4 2131.12 5
-8 0 -6 459.554 850.410 7
8 0 -6-241.069 1279.81 6
8 0 -6 517.379 1088.98 5
-8 0 -7 17232.9 1834.76 7
8 0 -7 13560.6 1985.52 6
-8 0 -8 2494.96 1063.59 7
8 0 -8 1508.09 1217.01 6
-8 0 -9 520.285 911.207 7
8 0 -9-184.536 1303.73 6
-8 0 -10-1493.89 1247.46 7
8 0 -10 840.252 1132.83 6
-8 0 -11 6112.81 1414.08 7
8 0 -11 5960.66 1637.09 6
8 1 -10 1524.09 1259.90 6
-8 -1 -9 324.889 1087.46 7
8 1 -9-660.955 1299.85 6
-8 -1 -8 546.850 1077.19 7
8 1 -8 1733.77 1270.51 6
-8 -1 -7 629.419 890.451 7
8 1 -7-395.133 1081.82 6
-8 -1 -6 5520.72 1227.00 7
8 1 -6 6416.07 1502.32 6
8 1 -6 6037.14 1614.09 5
-8 -1 -5 2406.43 1061.19 7
8 1 -5 3460.37 1438.82 6
8 1 -5 2861.68 1327.29 5
-8 -1 -4 3854.38 1102.31 7
8 1 -4 3485.60 1312.66 6
8 1 -4 4817.08 1666.48 5
-8 -1 -3 179.969 1004.59 7
8 1 -3-253.145 1142.40 6
8 1 -3 41.2539 1246.18 5
-8 -1 -2 4013.06 1088.93 7
8 1 -2 4670.41 1684.87 6
8 -1 2-48.5452 1458.62 6
8 -1 2 4588.80 1423.85 5
8 1 -2 4623.69 1543.59 5
-8 -1 -1 4133.73 1209.48 7
8 1 -1 7022.41 1837.41 6
8 -1 1 8436.40 1893.46 6
8 -1 1 2834.29 1108.06 5
8 1 -1 2954.39 1367.68 5
8 1 0 7321.61 1633.15 6
8 -1 0 7455.53 1833.58 6
8 -1 0 7077.58 1475.44 5
8 1 0 7810.61 1732.81 5
8 1 1 5909.83 1782.99 6
8 -1 -1 3988.39 1573.26 6
8 -1 -1 6635.79 1626.60 5
8 1 1 2991.32 1248.65 5
8 1 2 5653.05 1752.68 6
8 -1 -2 4103.36 1703.44 6
8 -1 -2 6357.54 1601.75 5
8 1 2 2557.47 1227.03 5
8 -1 -3 3011.00 1420.51 6
8 -1 -3 1898.22 1235.96 5
8 1 3 2281.76 1169.95 5
8 -1 -4 1383.34 1211.49 6
8 -1 -4 3218.17 1351.17 5
8 -1 -5 3486.26 1351.55 6
8 -1 -5 566.192 1369.84 5
8 -1 -6 6970.33 1553.02 6
8 -1 -6 6841.82 1701.14 5
8 -1 -7 3581.38 1444.45 6
8 -1 -8 3212.92 1458.78 6
8 -1 -9 1332.99 1328.83 6
8 -1 -10-540.920 1075.99 6
8 -1 -11 1595.53 1362.89 6
8 2 -10 7782.95 1701.37 6
8 2 -9 1502.40 1250.66 6
8 2 -8 5918.91 1661.11 6
-8 -2 -7 2677.60 1205.07 7
8 2 -7 618.590 1173.00 6
-8 -2 -6 864.486 1037.67 7
8 2 -6 468.712 1218.13 6
-8 -2 -5 438.258 877.240 7
8 2 -5 822.563 1116.08 6
-8 -2 -4 4691.62 1236.52 7
8 2 -4 7566.55 1673.78 6
8 2 -4 6487.73 1569.68 5
-8 -2 -3-172.158 955.263 7
8 2 -3-279.435 1335.47 6
8 2 -3-774.155 1265.07 5
-8 -2 -2 10370.5 1648.71 7
8 2 -2 13473.5 2154.82 6
8 -2 2 6907.32 1482.57 5
8 2 -2 10116.4 1827.35 5
-8 -2 -1 3555.16 1195.30 7
8 2 -1 995.573 1104.27 6
8 -2 1 2474.84 1250.87 5
8 2 -1-1132.99 1343.57 5
-8 -2 0-18.8959 985.662 7
8 -2 0 478.385 1207.35 5
8 2 0 766.134 1062.72 5
8 -2 -1 3699.03 1385.28 5
8 2 1-632.612 1259.89 5
8 -2 -2 6461.53 1544.65 5
8 2 2 6494.11 1495.42 5
8 -2 -3-1512.57 1280.84 5
8 2 3 1393.53 1267.96 5
8 -2 -4 5132.00 1625.79 5
8 2 4 5527.41 1393.36 5
8 -2 -5 267.865 1017.22 5
-8 -3 -4-304.791 1230.98 7
-8 -3 -3 8605.50 1617.08 7
-8 -3 -2 2596.21 1341.71 7
8 3 -2 245.223 1129.36 5
-8 -3 -1 1286.69 1110.99 7
8 -3 1 1956.55 1221.36 5
8 3 -1 1914.27 1354.11 5
8 -3 0 1370.42 1106.80 5
8 3 0 1938.05 1388.93 5
8 -3 -1 1784.76 1204.00 5
8 3 1 1176.36 1326.74 5
8 -3 -2 273.466 1225.43 5
8 3 2 824.804 1293.79 5
8 -3 -3 5159.17 1505.55 5
8 3 3 6778.93 1623.70 5
8 -3 -4 1520.29 1081.56 5
8 3 4 1652.24 1390.94 5
8 -4 0-511.506 1165.66 5
8 -4 -1 3702.69 1425.28 5
8 -4 -2 7471.73 1695.96 5
0 0 0 0.00 0.00 0
TITL V261_3 in P2(1)2(1)2(1)
REM P2(1)2(1)2(1) (#19 in standard setting)
CELL 0.71073 5.721516 7.900172 20.272862 90.0000 90.0000 90.0000
ZERR 4.00 0.000090 0.000171 0.000410 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 O Cl Br
UNIT 24.00 24.00 8.00 8.00 4.00 4.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 25565
_shelx_res_file
;
TITL V261_3 in P212121 #19
v261_3.res
created by SHELXL-2018/3 at 13:24:44 on 21-May-2020
REM reset to P212121 #19
CELL 0.71073 5.721516 7.900171 20.272862 90 90 90
ZERR 4 0.00009 0.000171 0.00041 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O Cl Br
UNIT 24 24 8 8 4 4
EQIV $1 -1+X,+Y,+Z
EQIV $2 -0.5+X,1.5-Y,1-Z
EQIV $3 -1+X,-1+Y,+Z
EQIV $4 1-X,0.5+Y,1.5-Z
L.S. 8
PLAN 1
TEMP 21.9(10)
CONF
HTAB N1 Br1
HTAB N1 Br1_$1
HTAB N1 Br1_$2
HTAB C3 Br1_$3
HTAB C5 O2_$4
BOND
MORE -1
BOND $H
fmap 2
acta
OMIT 0 60
REM
REM
REM
WGHT 0.032200
FVAR 7.43440
BR1 6 0.524430 0.844059 0.584614 11.00000 0.03208 0.03898 =
0.05173 0.00111 -0.00074 -0.00640
CL1 5 -0.310357 0.355859 0.539638 11.00000 0.04275 0.04904 =
0.05499 0.00172 -0.02013 -0.00997
O1 4 0.051603 -0.112565 0.689717 11.00000 0.06616 0.03716 =
0.06309 0.00770 0.00105 -0.00651
O2 4 0.290606 0.010383 0.756119 11.00000 0.07332 0.06397 =
0.06799 0.01913 -0.02805 0.00065
N1 3 0.021059 0.633918 0.576278 11.00000 0.03214 0.03377 =
0.04698 0.00238 -0.00433 -0.00413
AFIX 137
H1A 2 0.139212 0.703405 0.585339 11.00000 0.05116
H1B 2 -0.112446 0.680764 0.589483 11.00000 0.06077
H1C 2 0.015304 0.615323 0.533010 11.00000 0.05849
AFIX 0
N2 3 0.157644 0.011677 0.708827 11.00000 0.04474 0.04238 =
0.04328 0.00687 0.00236 0.00142
C1 1 0.055708 0.473473 0.610755 11.00000 0.02832 0.03203 =
0.03420 0.00009 0.00328 -0.00216
C2 1 -0.089264 0.336089 0.597234 11.00000 0.02732 0.03364 =
0.03389 -0.00504 -0.00192 -0.00161
C3 1 -0.056004 0.183791 0.629072 11.00000 0.03642 0.03004 =
0.03949 -0.00368 0.00027 -0.00715
AFIX 43
H3 2 -0.150708 0.090853 0.620220 11.00000 -1.20000
AFIX 0
C4 1 0.122740 0.174295 0.674507 11.00000 0.03575 0.03099 =
0.03397 0.00090 0.00198 -0.00020
C5 1 0.266510 0.306938 0.689178 11.00000 0.03683 0.04565 =
0.04092 0.00498 -0.00979 -0.00328
AFIX 43
H5 2 0.385125 0.295483 0.720224 11.00000 -1.20000
AFIX 0
C6 1 0.231161 0.459693 0.656525 11.00000 0.03430 0.03834 =
0.04243 0.00047 -0.00755 -0.01056
AFIX 43
H6 2 0.326256 0.552208 0.665712 11.00000 -1.20000
AFIX 0
HKLF 4
REM V261_3 in P212121 #19
REM wR2 = 0.0623, GooF = S = 1.127, Restrained GooF = 1.127 for all data
REM R1 = 0.0278 for 2340 Fo > 4sig(Fo) and 0.0366 for all 2669 data
REM 113 parameters refined using 0 restraints
END
WGHT 0.0322 0.0000
REM Highest difference peak 0.331, deepest hole -0.697, 1-sigma level 0.106
Q1 1 0.0275 0.3719 0.5102 11.00000 0.05 0.33
;
_shelx_res_checksum 24811
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -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
Br Br1 0.52443(5) 0.84406(4) 0.58461(2) 0.04093(10) Uani d 1 . .
Cl Cl1 -0.31036(14) 0.35586(13) 0.53964(4) 0.0489(2) Uani d 1 . .
O O1 0.0516(5) -0.1126(3) 0.68972(13) 0.0555(7) Uani d 1 . .
O O2 0.2906(5) 0.0104(4) 0.75612(13) 0.0684(8) Uani d 1 . .
N N1 0.0211(4) 0.6339(3) 0.57628(13) 0.0376(6) Uani d 1 . .
H H1A 0.139212 0.703405 0.585339 0.051(11) Uiso calc 1 . .
H H1B -0.112446 0.680764 0.589483 0.061(12) Uiso calc 1 . .
H H1C 0.015304 0.615323 0.533010 0.058(12) Uiso calc 1 . .
N N2 0.1576(5) 0.0117(4) 0.70883(14) 0.0435(7) Uani d 1 . .
C C1 0.0557(5) 0.4735(4) 0.61076(14) 0.0315(6) Uani d 1 . .
C C2 -0.0893(5) 0.3361(4) 0.59723(13) 0.0316(6) Uani d 1 . .
C C3 -0.0560(5) 0.1838(4) 0.62907(14) 0.0353(6) Uani d 1 . .
H H3 -0.150708 0.090853 0.620220 0.042 Uiso calc 1 . .
C C4 0.1227(5) 0.1743(4) 0.67451(14) 0.0336(6) Uani d 1 . .
C C5 0.2665(6) 0.3069(5) 0.68918(16) 0.0411(8) Uani d 1 . .
H H5 0.385125 0.295483 0.720224 0.049 Uiso calc 1 . .
C C6 0.2312(6) 0.4597(4) 0.65653(15) 0.0384(7) Uani d 1 . .
H H6 0.326256 0.552208 0.665712 0.046 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
Br1 0.03208(15) 0.03898(17) 0.05173(17) -0.00640(13) -0.00074(12) 0.00111(15)
Cl1 0.0427(4) 0.0490(5) 0.0550(4) -0.0100(4) -0.0201(3) 0.0017(4)
O1 0.0662(17) 0.0372(14) 0.0631(15) -0.0065(13) 0.0010(13) 0.0077(11)
O2 0.073(2) 0.064(2) 0.0680(17) 0.0007(16) -0.0280(15) 0.0191(16)
N1 0.0321(12) 0.0338(13) 0.0470(14) -0.0041(11) -0.0043(11) 0.0024(11)
N2 0.0447(16) 0.0424(18) 0.0433(14) 0.0014(14) 0.0024(13) 0.0069(14)
C1 0.0283(14) 0.0320(15) 0.0342(13) -0.0022(12) 0.0033(11) 0.0001(12)
C2 0.0273(12) 0.0336(15) 0.0339(13) -0.0016(12) -0.0019(9) -0.0050(14)
C3 0.0364(14) 0.0300(16) 0.0395(14) -0.0072(12) 0.0003(12) -0.0037(13)
C4 0.0358(14) 0.0310(16) 0.0340(13) -0.0002(14) 0.0020(11) 0.0009(14)
C5 0.0368(16) 0.046(2) 0.0409(16) -0.0033(15) -0.0098(13) 0.0050(15)
C6 0.0343(16) 0.0383(18) 0.0424(15) -0.0106(14) -0.0076(13) 0.0005(15)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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 -4 5 0.1164
0 4 -5 0.1000
-5 0 3 0.1783
5 0 -3 0.1651
0 1 5 0.1121
0 -1 -5 0.1491
-4 1 5 0.1579
-4 -1 -5 0.1878
3 1 5 0.1447
1 -1 -5 0.1600
-1 -1 5 0.1364
1 -1 5 0.1426
0 -1 -1 0.1382
2 -4 -5 0.1656
0 -1 5 0.1218
0 5 -2 0.1016
4 5 -5 0.1392
0 2 -5 0.0939
0 0 1 0.1054
0 4 -27 0.1226
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
H1A N1 H1B . . 109.5 ?
H1A N1 H1C . . 109.5 ?
H1B N1 H1C . . 109.5 ?
C1 N1 H1A . . 109.5 ?
C1 N1 H1B . . 109.5 ?
C1 N1 H1C . . 109.5 ?
O1 N2 O2 . . 123.5(3) ?
O1 N2 C4 . . 119.0(3) ?
O2 N2 C4 . . 117.5(3) ?
C2 C1 N1 . . 120.1(3) ?
C6 C1 N1 . . 119.5(3) ?
C6 C1 C2 . . 120.5(3) ?
C1 C2 Cl1 . . 119.9(2) ?
C3 C2 Cl1 . . 119.7(2) ?
C3 C2 C1 . . 120.4(3) ?
C2 C3 H3 . . 121.2 ?
C4 C3 C2 . . 117.6(3) ?
C4 C3 H3 . . 121.2 ?
C3 C4 N2 . . 117.6(3) ?
C5 C4 N2 . . 119.0(3) ?
C5 C4 C3 . . 123.4(3) ?
C4 C5 H5 . . 120.8 ?
C4 C5 C6 . . 118.3(3) ?
C6 C5 H5 . . 120.8 ?
C1 C6 C5 . . 119.8(3) ?
C1 C6 H6 . . 120.1 ?
C5 C6 H6 . . 120.1 ?
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 C2 . 1.729(3) ?
O1 N2 . 1.217(4) ?
O2 N2 . 1.224(4) ?
N1 H1A . 0.8900 ?
N1 H1B . 0.8900 ?
N1 H1C . 0.8900 ?
N1 C1 . 1.461(4) ?
N2 C4 . 1.475(4) ?
C1 C2 . 1.393(4) ?
C1 C6 . 1.371(4) ?
C2 C3 . 1.379(4) ?
C3 H3 . 0.9300 ?
C3 C4 . 1.378(4) ?
C4 C5 . 1.365(5) ?
C5 H5 . 0.9300 ?
C5 C6 . 1.391(5) ?
C6 H6 . 0.9300 ?
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 H1A Br1 . 0.89 2.47 3.329(2) 162.7 yes
N1 H1B Br1 1_455 0.89 2.45 3.295(2) 159.3 yes
N1 H1C Br1 3_466 0.89 2.41 3.266(3) 162.5 yes
C3 H3 Br1 1_445 0.93 2.79 3.712(3) 172.0 yes
C5 H5 O2 4_656 0.93 2.56 3.199(4) 126.2 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
Cl1 C2 C3 C4 . . . . 179.9(2) ?
O1 N2 C4 C3 . . . . 10.1(5) ?
O1 N2 C4 C5 . . . . -170.2(3) ?
O2 N2 C4 C3 . . . . -168.8(3) ?
O2 N2 C4 C5 . . . . 10.9(5) ?
N1 C1 C2 Cl1 . . . . -0.1(4) ?
N1 C1 C2 C3 . . . . 179.3(3) ?
N1 C1 C6 C5 . . . . -179.5(3) ?
N2 C4 C5 C6 . . . . -179.8(3) ?
C1 C2 C3 C4 . . . . 0.6(4) ?
C2 C1 C6 C5 . . . . 0.7(5) ?
C2 C3 C4 N2 . . . . 179.7(3) ?
C2 C3 C4 C5 . . . . -0.1(5) ?
C3 C4 C5 C6 . . . . -0.1(5) ?
C4 C5 C6 C1 . . . . -0.2(5) ?
C6 C1 C2 Cl1 . . . . 179.7(2) ?
C6 C1 C2 C3 . . . . -0.9(4) ?