#------------------------------------------------------------------------------
#$Date: 2021-04-06 04:16:15 +0300 (Tue, 06 Apr 2021) $
#$Revision: 263878 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/23/2022326.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_2022326
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 +, H S O4 -'
_chemical_formula_moiety 'C6 H6 Cl N2 O2 +, H O4 S -'
_chemical_formula_sum 'C6 H7 Cl N2 O6 S'
_chemical_formula_weight 270.65
_chemical_name_systematic
;
2-Chloro-4-nitroanilinium hydrogen sulfate
;
_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 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 101.584(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 16.1771(6)
_cell_length_b 4.95335(16)
_cell_length_c 12.8431(5)
_cell_measurement_reflns_used 1898
_cell_measurement_temperature 295.0(10)
_cell_measurement_theta_max 31.7380
_cell_measurement_theta_min 3.2170
_cell_volume 1008.17(6)
_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 1.000
_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 0.0223
_diffrn_reflns_av_unetI/netI 0.0334
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 6028
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.994
_diffrn_reflns_theta_min 2.570
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.602
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.96704
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_density_diffrn 1.783
_exptl_crystal_description plate
_exptl_crystal_F_000 552
_exptl_crystal_size_max 0.56
_exptl_crystal_size_mid 0.46
_exptl_crystal_size_min 0.06
_refine_diff_density_max 0.517
_refine_diff_density_min -0.550
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.072
_refine_ls_hydrogen_treatment hetero
_refine_ls_matrix_type full
_refine_ls_number_parameters 161
_refine_ls_number_reflns 2923
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.072
_refine_ls_R_factor_all 0.0490
_refine_ls_R_factor_gt 0.0359
_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^)+(0.0452P)^2^+0.2615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0921
_refine_ls_wR_factor_ref 0.0991
_reflns_number_gt 2351
_reflns_number_total 2923
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file dv3005sup1.cif
_cod_data_source_block 2
_cod_depositor_comments
'Adding full bibliography for 2022325--2022329.cif.'
_cod_original_cell_volume 1008.17(7)
_cod_database_code 2022326
_cod_database_fobs_code 2022326
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.729
_shelx_estimated_absorpt_t_max 0.965
_shelx_hkl_file
;
2 0 0 53973.2 863.686 2
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5 0 0 150542. 2327.98 1
-5 0 0 150807. 2364.08 2
5 0 0 149702. 2358.96 2
6 0 0 151838. 2396.07 1
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7 0 0 159407. 2569.61 1
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13 0 0 58077.3 1510.38 1
14 0 0 22947.7 911.649 1
15 0 0 11263.9 645.365 1
16 0 0 2408.47 318.253 1
17 0 0 20679.4 955.956 1
18 0 0 933.785 237.328 1
19 0 0 8387.50 645.669 1
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11 1 0 48.7471 67.8871 1
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-11 1 0-63.7901 123.042 2
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12 -1 0 7338.91 501.371 1
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13 -1 0 434.035 162.890 1
13 1 0 195.825 113.099 1
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8 5 0 213.892 110.375 3
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3 7 0 321.305 133.286 3
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18 0 -1 135.547 129.297 1
17 0 -1 96.1882 165.021 1
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15 0 -1 93.2075 115.767 1
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13 0 -1-24.8923 92.4734 1
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12 0 -1-90.6391 108.582 1
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11 0 -1-12.9519 76.1808 1
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10 0 -1 68.1363 66.3501 1
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-17 1 16 201.350 178.315 2
-16 1 16 697.827 257.377 2
-15 1 16 89.5351 144.748 2
-14 1 16-114.121 165.457 2
-13 1 16-81.9683 167.552 2
-12 1 16-201.751 219.608 2
-11 1 16 242.951 135.580 2
-10 1 16-178.501 202.570 2
-9 1 16 501.223 255.312 2
-8 1 16 2019.00 350.558 2
-7 1 16 383.245 197.350 2
-7 -1 16 460.973 186.712 2
-6 1 16-116.419 133.580 2
-6 -1 16 30.9613 145.116 2
-5 1 16 150.863 136.520 2
-5 -1 16 389.918 173.562 2
-4 -1 16 1488.32 252.766 2
-4 1 16 1429.22 281.920 2
-3 -1 16 2054.52 304.121 2
-3 1 16 1886.75 354.709 2
-2 -1 16 2643.66 362.823 2
-2 1 16 2129.75 340.961 2
-1 -1 16 221.706 142.533 2
-1 1 16 492.987 167.378 2
-1 -1 16 576.989 187.229 1
0 -1 16-92.2846 158.860 1
0 -1 16 245.094 164.860 2
0 1 16-314.716 220.531 2
1 -1 16 102.141 143.418 1
1 -1 16 153.840 123.105 2
1 1 16 389.122 174.424 2
2 -1 16-313.061 225.406 2
2 1 16 148.409 162.125 2
2 -1 16-76.4489 180.481 1
3 1 16 193.224 206.545 1
3 -1 16 275.989 184.871 1
3 -1 16 271.061 142.770 2
3 1 16 484.541 262.374 2
4 -1 16 608.127 231.639 1
4 1 16 247.278 192.036 1
4 1 16 669.324 216.027 2
5 -1 16 742.054 261.132 1
5 1 16 544.734 246.090 1
5 1 16 27.6568 190.970 2
6 -1 16 87.7088 148.707 1
6 1 16 138.533 182.179 1
6 1 16 123.368 159.788 2
-14 2 16 3348.66 485.120 2
-13 2 16 131.988 192.074 2
-12 2 16 22.1349 122.138 2
-11 2 16 289.752 204.511 2
-10 2 16 3724.51 487.445 2
-9 2 16 6925.10 665.592 2
-8 2 16 10195.9 791.570 2
-7 2 16 1532.84 324.253 2
-6 2 16 144.378 176.975 2
-5 2 16 223.145 162.091 2
-4 2 16 2295.53 400.429 2
-3 2 16 4702.98 529.076 2
-2 -2 16 8269.67 655.223 1
-2 2 16 9723.14 779.039 2
-1 -2 16 3995.72 463.775 1
-1 2 16 3946.23 507.999 2
0 -2 16-273.934 160.693 1
0 2 16-234.083 225.260 2
1 -2 16 1302.17 270.010 1
1 2 16 1636.02 351.353 2
2 -2 16 3807.70 471.494 1
2 2 16 3985.61 515.209 2
3 -2 16 113.002 143.775 1
3 2 16-57.6118 210.412 2
4 -2 16 7076.48 671.325 1
4 2 16 7136.93 701.413 2
5 -2 16 928.145 273.530 1
6 -2 16 227.611 165.252 1
-9 3 16 85.9392 237.318 2
-8 3 16-204.936 216.956 2
-7 3 16-156.986 162.705 2
-6 3 16-32.4271 148.440 2
-5 3 16 3899.12 517.315 2
-4 3 16 369.820 236.526 2
-3 3 16 5702.07 621.912 2
-2 3 16 1541.12 334.904 2
-1 3 16 48.0664 226.350 2
0 3 16-264.411 206.053 2
3 -3 16 4925.03 547.350 1
4 -3 16 1414.30 308.654 1
5 -3 16 2664.49 425.645 1
-11 0 17 313.184 141.601 2
-10 0 17 45.5782 144.536 2
-9 0 17-109.444 124.459 2
-8 0 17 47.0954 153.920 2
-7 0 17 174.541 143.137 2
-6 0 17 103.548 134.522 2
-5 0 17 120.803 154.505 2
-4 0 17-146.082 157.473 2
-3 0 17-52.6393 156.143 2
-2 0 17-188.906 175.285 2
-1 0 17 87.1181 156.671 2
0 0 17 158.089 167.575 2
1 0 17-180.330 193.241 2
2 0 17 201.405 178.009 1
2 0 17-164.586 182.051 2
3 0 17-35.1881 170.260 1
3 0 17 290.519 193.768 2
4 0 17-24.1166 141.402 2
4 0 17-18.0785 123.697 1
5 0 17 442.743 197.234 2
-15 1 17 735.301 291.705 2
-14 1 17 1240.26 307.608 2
-13 1 17 2344.53 407.566 2
-12 1 17 13065.5 897.956 2
-11 1 17 8785.38 725.649 2
-10 1 17 1603.66 332.698 2
-9 1 17 3626.31 476.950 2
-8 1 17 11616.5 820.110 2
-7 1 17 882.151 245.295 2
-6 1 17 9183.73 732.812 2
-5 1 17 7075.49 647.678 2
-4 1 17 4090.41 496.314 2
-3 -1 17 285.432 142.641 2
-3 1 17 204.581 180.225 2
-2 -1 17 4468.35 467.050 2
-2 1 17 5068.33 545.989 2
-1 -1 17 4218.49 468.148 2
-1 1 17 3292.29 458.406 2
0 -1 17 1953.54 370.576 1
0 -1 17 1841.83 323.087 2
0 1 17 2403.85 404.393 2
1 -1 17 4209.79 532.935 1
1 -1 17 4341.18 487.912 2
1 1 17 3920.88 507.320 2
2 -1 17 236.971 178.847 2
2 1 17 154.957 154.042 2
3 -1 17-118.585 164.207 1
3 -1 17-114.660 161.155 2
3 1 17-56.3823 176.720 2
4 -1 17 1057.23 302.289 2
4 -1 17 491.852 221.282 1
-11 2 17 1427.91 291.117 2
-10 2 17-78.3806 223.026 2
-9 2 17-150.925 159.524 2
-8 2 17 5478.77 600.612 2
-7 2 17 102.365 169.044 2
-6 2 17 1001.16 287.713 2
-5 2 17 1678.59 351.220 2
-4 2 17-121.447 173.943 2
-3 2 17 611.913 249.170 2
-2 2 17 1863.32 383.142 2
-1 -2 17 121.263 130.459 1
-1 2 17 549.051 246.370 2
0 2 17 1093.36 270.832 2
0 -2 17 772.083 213.445 1
1 -2 17 325.826 223.055 1
1 2 17-132.771 208.320 2
2 -2 17 3235.15 463.230 1
3 -2 17 3226.03 480.429 1
4 -2 17 1643.56 362.103 1
-9 0 18 446.005 207.352 2
-8 0 18 5872.49 571.947 2
-7 0 18 3192.55 429.735 2
-6 0 18 7732.56 653.944 2
-5 0 18 9282.44 733.235 2
-4 0 18 2519.60 393.496 2
-3 0 18 290.486 167.304 2
-2 0 18 1490.76 331.303 2
-1 0 18 1063.76 287.919 2
0 0 18-627.424 252.937 2
1 0 18 11168.3 841.146 2
2 0 18 10640.5 833.002 2
-12 1 18 249.314 205.418 2
-11 1 18 143.500 145.057 2
-10 1 18-751.655 239.412 2
-9 1 18-65.2900 212.317 2
-8 1 18 1721.54 362.869 2
-7 1 18 81.4021 207.109 2
-6 1 18 180.412 204.629 2
-5 1 18 624.186 275.765 2
-4 1 18-147.968 187.370 2
-3 1 18 207.596 131.579 2
-2 1 18 13.5916 165.987 2
-1 1 18-466.753 263.598 2
0 1 18 49.2925 193.134 2
1 -1 18 360.675 195.135 1
1 -1 18-81.1905 184.967 2
2 -1 18-198.371 216.347 1
2 -1 18 781.601 252.073 2
3 -1 18 798.702 224.680 2
-6 0 19-122.445 153.049 2
-5 0 19-194.737 142.008 2
-4 0 19-23.6047 131.124 2
-3 0 19-65.8648 162.242 2
-2 0 19-4.70828 123.845 2
-1 0 19-545.434 240.452 2
0 0 0 0.00 0.00 0
TITL V257_1 in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 16.177107 4.953351 12.843085 90.0000 101.5842 90.0000
ZERR 4.00 0.000645 0.000165 0.000479 0.0000 0.0039 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H
UNIT 20.00 40.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 37338
_shelx_res_file
;
TITL V257_1 in P21/c #14
v257_1.res
created by SHELXL-2018/3 at 11:35:27 on 21-May-2020
REM reset to P21/c #14
CELL 0.71073 16.177107 4.953351 12.843085 90 101.5842 90
ZERR 4 0.000645 0.000165 0.000479 0 0.0039 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl N O S
UNIT 24 28 4 8 24 4
EQIV $1 +X,0.5-Y,-0.5+Z
EQIV $2 +X,1+Y,+Z
EQIV $3 -X,1-Y,-Z
EQIV $4 1-X,2-Y,-Z
EQIV $5 -X,-0.5+Y,0.5-Z
L.S. 8
PLAN 5
SIZE 0.06 0.46 0.56
TEMP 21.9(10)
CONF
HTAB N1 O3
HTAB N1 O6_$1
HTAB N1 O3_$2
HTAB N1 O5_$3
HTAB C3 O1_$4
HTAB C6 O3
HTAB O4 O5_$5
BOND
MORE -1
BOND $H
fmap 2
acta
OMIT 0 60
REM
REM
REM
WGHT 0.045200 0.261500
FVAR 5.63574
CL1 3 0.236258 0.967447 -0.129143 11.00000 0.03961 0.03724 =
0.03318 0.01494 0.00216 -0.00251
O1 5 0.534641 0.749898 0.093111 11.00000 0.03214 0.06559 =
0.06192 0.01419 0.00768 -0.01639
O2 5 0.523939 0.406801 0.190994 11.00000 0.03226 0.05816 =
0.05677 0.01707 -0.00220 0.00502
N1 4 0.141046 0.555340 -0.031153 11.00000 0.02335 0.02779 =
0.02099 0.00158 0.00431 0.00090
H1A 2 0.119909 0.422385 0.007751 11.00000 0.03480
H1B 2 0.131704 0.517150 -0.101224 11.00000 0.05362
H1C 2 0.116754 0.706481 -0.021471 11.00000 0.05233
N2 4 0.493336 0.580166 0.128568 11.00000 0.02752 0.04239 =
0.03282 -0.00174 0.00296 -0.00289
C1 1 0.231013 0.573273 0.014426 11.00000 0.02193 0.02561 =
0.01952 -0.00161 0.00386 -0.00035
C2 1 0.281089 0.751993 -0.028136 11.00000 0.03025 0.02433 =
0.02089 0.00263 0.00568 0.00129
C3 1 0.367335 0.758604 0.010548 11.00000 0.02915 0.03040 =
0.03001 0.00261 0.00820 -0.00575
AFIX 43
H3 2 0.401763 0.877371 -0.017358 11.00000 -1.20000
AFIX 0
C4 1 0.400549 0.584361 0.091436 11.00000 0.02244 0.03264 =
0.02658 -0.00143 0.00269 -0.00235
C5 1 0.351954 0.412408 0.138195 11.00000 0.02847 0.03691 =
0.02892 0.01075 0.00005 -0.00169
AFIX 43
H5 2 0.376323 0.302298 0.194717 11.00000 -1.20000
AFIX 0
C6 1 0.266070 0.407885 0.098898 11.00000 0.02959 0.03328 =
0.02584 0.00691 0.00338 -0.00593
AFIX 43
H6 2 0.231691 0.293888 0.129073 11.00000 -1.20000
AFIX 0
S1 6 0.069054 0.003693 0.159579 11.00000 0.02285 0.01866 =
0.01607 -0.00065 0.00517 -0.00072
O3 5 0.095831 0.066968 0.061329 11.00000 0.03244 0.02783 =
0.01953 0.00183 0.01064 -0.00375
O4 5 0.062045 -0.311069 0.154777 11.00000 0.04765 0.01945 =
0.02896 -0.00064 0.01755 -0.00355
H4 2 0.047537 -0.360750 0.207175 11.00000 0.05330
O5 5 -0.014235 0.107893 0.163316 11.00000 0.02964 0.03788 =
0.02407 -0.00039 0.00883 0.00821
O6 5 0.130907 0.074141 0.253376 11.00000 0.03313 0.03896 =
0.02070 -0.00106 -0.00047 -0.00708
HKLF 4
REM V257_1 in P21/c #14
REM wR2 = 0.0991, GooF = S = 1.072, Restrained GooF = 1.072 for all data
REM R1 = 0.0359 for 2351 Fo > 4sig(Fo) and 0.0490 for all 2923 data
REM 161 parameters refined using 0 restraints
END
WGHT 0.0452 0.2615
REM Highest difference peak 0.517, deepest hole -0.550, 1-sigma level 0.066
Q1 1 0.2609 0.8655 -0.1595 11.00000 0.05 0.52
Q2 1 0.2494 0.5313 0.0644 11.00000 0.05 0.34
Q3 1 0.1960 0.5762 0.0012 11.00000 0.05 0.27
Q4 1 0.2567 0.6099 -0.0217 11.00000 0.05 0.26
Q5 1 0.3152 0.6763 -0.0302 11.00000 0.05 0.25
;
_shelx_res_checksum 3763
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
Cl Cl1 0.23626(3) 0.96745(10) -0.12914(4) 0.03739(14) Uani d 1 . .
O O1 0.53464(9) 0.7499(4) 0.09311(14) 0.0535(4) Uani d 1 . .
O O2 0.52394(9) 0.4068(4) 0.19099(14) 0.0506(4) Uani d 1 . .
N N1 0.14105(9) 0.5553(3) -0.03115(12) 0.0241(3) Uani d 1 . .
H H1A 0.1199(14) 0.422(5) 0.0078(17) 0.035(6) Uiso d 1 . .
H H1B 0.1317(16) 0.517(5) -0.101(2) 0.054(8) Uiso d 1 . .
H H1C 0.1168(16) 0.706(5) -0.021(2) 0.052(7) Uiso d 1 . .
N N2 0.49334(10) 0.5802(4) 0.12857(14) 0.0347(4) Uani d 1 . .
C C1 0.23101(10) 0.5733(3) 0.01443(13) 0.0224(3) Uani d 1 . .
C C2 0.28109(11) 0.7520(3) -0.02814(13) 0.0251(3) Uani d 1 . .
C C3 0.36733(11) 0.7586(4) 0.01055(15) 0.0295(4) Uani d 1 . .
H H3 0.401763 0.877371 -0.017358 0.035 Uiso calc 1 . .
C C4 0.40055(11) 0.5844(4) 0.09144(14) 0.0275(4) Uani d 1 . .
C C5 0.35195(12) 0.4124(4) 0.13820(15) 0.0322(4) Uani d 1 . .
H H5 0.376323 0.302298 0.194717 0.039 Uiso calc 1 . .
C C6 0.26607(11) 0.4079(4) 0.09890(14) 0.0299(4) Uani d 1 . .
H H6 0.231691 0.293888 0.129073 0.036 Uiso calc 1 . .
S S1 0.06905(2) 0.00369(7) 0.15958(3) 0.01902(11) Uani d 1 . .
O O3 0.09583(8) 0.0670(2) 0.06133(9) 0.0258(3) Uani d 1 . .
O O4 0.06204(9) -0.3111(3) 0.15478(11) 0.0306(3) Uani d 1 . .
H H4 0.0475(16) -0.361(5) 0.207(2) 0.053(8) Uiso d 1 . .
O O5 -0.01424(8) 0.1079(3) 0.16332(10) 0.0300(3) Uani d 1 . .
O O6 0.13091(8) 0.0741(3) 0.25338(10) 0.0318(3) 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
Cl1 0.0396(3) 0.0372(3) 0.0332(3) -0.0025(2) 0.0022(2) 0.0149(2)
O1 0.0321(7) 0.0656(11) 0.0619(11) -0.0164(7) 0.0077(7) 0.0142(9)
O2 0.0323(8) 0.0582(10) 0.0568(10) 0.0050(7) -0.0022(7) 0.0171(9)
N1 0.0234(7) 0.0278(7) 0.0210(7) 0.0009(6) 0.0043(6) 0.0016(6)
N2 0.0275(8) 0.0424(9) 0.0328(8) -0.0029(7) 0.0030(7) -0.0017(7)
C1 0.0219(7) 0.0256(8) 0.0195(7) -0.0003(6) 0.0039(6) -0.0016(6)
C2 0.0302(8) 0.0243(8) 0.0209(8) 0.0013(7) 0.0057(7) 0.0026(6)
C3 0.0292(8) 0.0304(9) 0.0300(9) -0.0057(7) 0.0082(7) 0.0026(7)
C4 0.0224(8) 0.0326(9) 0.0266(8) -0.0023(7) 0.0027(7) -0.0014(7)
C5 0.0285(9) 0.0369(10) 0.0289(9) -0.0017(8) 0.0000(7) 0.0108(8)
C6 0.0296(9) 0.0333(9) 0.0258(8) -0.0059(7) 0.0034(7) 0.0069(7)
S1 0.0229(2) 0.01866(19) 0.01607(18) -0.00072(14) 0.00517(14) -0.00065(14)
O3 0.0324(6) 0.0278(6) 0.0195(6) -0.0037(5) 0.0106(5) 0.0018(5)
O4 0.0476(8) 0.0195(6) 0.0290(7) -0.0035(5) 0.0176(6) -0.0006(5)
O5 0.0296(6) 0.0379(7) 0.0241(6) 0.0082(6) 0.0088(5) -0.0004(5)
O6 0.0331(7) 0.0390(7) 0.0207(6) -0.0071(6) -0.0005(5) -0.0011(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
H1A N1 H1B . . 112(2) ?
H1A N1 H1C . . 108(2) ?
H1B N1 H1C . . 110(2) ?
C1 N1 H1A . . 105.8(13) ?
C1 N1 H1B . . 111.5(16) ?
C1 N1 H1C . . 109.6(17) ?
O1 N2 C4 . . 117.82(17) ?
O2 N2 O1 . . 123.73(17) ?
O2 N2 C4 . . 118.45(17) ?
C2 C1 N1 . . 119.76(15) ?
C2 C1 C6 . . 120.46(16) ?
C6 C1 N1 . . 119.77(15) ?
C1 C2 Cl1 . . 120.14(13) ?
C3 C2 Cl1 . . 119.80(13) ?
C3 C2 C1 . . 120.06(16) ?
C2 C3 H3 . . 121.0 ?
C4 C3 C2 . . 117.99(16) ?
C4 C3 H3 . . 121.0 ?
C3 C4 N2 . . 117.99(16) ?
C3 C4 C5 . . 123.21(17) ?
C5 C4 N2 . . 118.79(17) ?
C4 C5 H5 . . 120.9 ?
C4 C5 C6 . . 118.16(17) ?
C6 C5 H5 . . 120.9 ?
C1 C6 H6 . . 120.0 ?
C5 C6 C1 . . 120.01(16) ?
C5 C6 H6 . . 120.0 ?
O3 S1 O4 . . 102.32(7) ?
O3 S1 O5 . . 113.18(8) ?
O5 S1 O4 . . 107.17(8) ?
O6 S1 O3 . . 113.31(8) ?
O6 S1 O4 . . 107.83(8) ?
O6 S1 O5 . . 112.21(8) ?
S1 O4 H4 . . 107.9(19) ?
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 . 1.7233(17) ?
O1 N2 . 1.218(2) ?
O2 N2 . 1.211(2) ?
N1 H1A . 0.93(2) ?
N1 H1B . 0.90(3) ?
N1 H1C . 0.87(3) ?
N1 C1 . 1.458(2) ?
N2 C4 . 1.481(2) ?
C1 C2 . 1.384(2) ?
C1 C6 . 1.387(2) ?
C2 C3 . 1.384(2) ?
C3 H3 . 0.9300 ?
C3 C4 . 1.374(3) ?
C4 C5 . 1.376(3) ?
C5 H5 . 0.9300 ?
C5 C6 . 1.380(2) ?
C6 H6 . 0.9300 ?
S1 O3 . 1.4483(12) ?
S1 O4 . 1.5636(13) ?
S1 O5 . 1.4526(12) ?
S1 O6 . 1.4457(12) ?
O4 H4 . 0.79(3) ?
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 O3 . 0.93(2) 1.96(2) 2.854(2) 161(2) yes
N1 H1B O6 4_565 0.90(3) 1.92(3) 2.813(2) 171(2) yes
N1 H1C O3 1_565 0.87(3) 2.14(3) 2.952(2) 156(2) yes
N1 H1C O5 3_565 0.87(3) 2.39(3) 2.911(2) 119(2) yes
C3 H3 O1 3_675 0.93 2.41 3.326(2) 167.6 yes
C6 H6 O3 . 0.93 2.47 3.184(2) 134.0 yes
O4 H4 O5 2_545 0.79(3) 1.85(3) 2.6350(18) 167(3) 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 . . . . 179.72(14) ?
O1 N2 C4 C3 . . . . 7.3(3) ?
O1 N2 C4 C5 . . . . -173.56(19) ?
O2 N2 C4 C3 . . . . -171.69(19) ?
O2 N2 C4 C5 . . . . 7.5(3) ?
N1 C1 C2 Cl1 . . . . 4.0(2) ?
N1 C1 C2 C3 . . . . -176.13(16) ?
N1 C1 C6 C5 . . . . 176.11(17) ?
N2 C4 C5 C6 . . . . -176.51(17) ?
C1 C2 C3 C4 . . . . -0.1(3) ?
C2 C1 C6 C5 . . . . -2.8(3) ?
C2 C3 C4 N2 . . . . 176.51(16) ?
C2 C3 C4 C5 . . . . -2.6(3) ?
C3 C4 C5 C6 . . . . 2.6(3) ?
C4 C5 C6 C1 . . . . 0.1(3) ?
C6 C1 C2 Cl1 . . . . -177.08(14) ?
C6 C1 C2 C3 . . . . 2.8(3) ?