#------------------------------------------------------------------------------
#$Date: 2021-02-19 08:01:46 +0200 (Fri, 19 Feb 2021) $
#$Revision: 262087 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/23/2022328.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_2022328
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 Structural Chemistry'
_journal_paper_doi 10.1107/S2053229621001455
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac 'C7 H9 N2 O2 +, I3 -'
_chemical_formula_moiety 'C7 H9 N2 O2 +, I3 -'
_chemical_formula_sum 'C7 H9 I3 N2 O2'
_chemical_formula_weight 533.86
_chemical_name_systematic
;
2-Methyl-6-nitroanilinium triiodide
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_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 98.738(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.0840(2)
_cell_length_b 11.5247(4)
_cell_length_c 16.3921(6)
_cell_measurement_reflns_used 6876
_cell_measurement_temperature 295.0(10)
_cell_measurement_theta_max 26.6320
_cell_measurement_theta_min 3.0290
_cell_volume 1322.73(8)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2018)
;
_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
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 295.0(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.937
_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_unetI/netI 0.0669
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 5822
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.679
_diffrn_reflns_theta_min 3.074
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 7.070
_exptl_absorpt_correction_T_max 0.988
_exptl_absorpt_correction_T_min 0.966
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
{CrysAlis PRO (Rigaku OD, 2015), based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour 'clear dark black'
_exptl_crystal_density_diffrn 2.681
_exptl_crystal_description block
_exptl_crystal_F_000 960
_exptl_crystal_size_max 0.208
_exptl_crystal_size_mid 0.105
_exptl_crystal_size_min 0.085
_refine_diff_density_max 0.702
_refine_diff_density_min -0.776
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.800
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 130
_refine_ls_number_reflns 5822
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.800
_refine_ls_R_factor_all 0.0787
_refine_ls_R_factor_gt 0.0306
_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^)+(0.0302P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0551
_refine_ls_wR_factor_ref 0.0586
_reflns_number_gt 3181
_reflns_number_total 5822
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file dv3005sup1.cif
_cod_data_source_block 4
_cod_database_code 2022328
_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 2-12.5274 83.3132 1
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0 0 -4 50854.4 127.965 1
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0 0 6 135973. 191.867 1
0 0 -8 1531.51 41.4719 -2
0 0 -8 1531.51 41.4719 1
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0 0 10 27141.2 99.9037 1
0 0 -12 3191.46 61.0528 -2
0 0 -12 3191.46 61.0528 1
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0 -1 -2 18359.6 55.6657 -2
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0 -1 -3 122.045 20.9999 1
0 1 -4 15441.4 47.3499 -2
0 -1 -4 15441.4 47.3499 1
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0 1 12 2175.17 57.2491 -2
0 -1 12 2175.17 57.2491 1
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0 -1 -13 2825.02 56.0024 1
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0 1 -14 192.238 47.8574 1
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0 -1 18 122.428 107.516 1
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0 -1 -20 296.137 124.202 1
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0 -1 21 68.9258 178.813 1
0 1 22-35.2789 550.077 -2
0 -1 22-35.2789 550.077 1
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0 -2 5 5708.99 43.0906 1
0 2 -6 16630.7 65.2366 -2
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0 -2 -7 827.963 33.3603 -2
0 2 -7 827.963 33.3603 1
0 2 -8 1136.51 38.5954 -2
0 -2 -8 1136.51 38.5954 1
0 2 -9 12643.4 69.9867 -2
0 -2 -9 12643.4 69.9867 1
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0 2 -11 112.676 46.1629 -2
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0 -2 -14 3960.14 68.7121 1
0 -2 -15 278.768 64.5848 -2
0 2 -15 278.768 64.5848 1
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0 -2 16 161.166 72.2071 1
0 2 17 545.575 104.643 -2
0 -2 17 545.575 104.643 1
0 2 18 277.841 117.800 -2
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0 -2 -19 142.106 126.193 -2
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0 -3 -5 1070.53 31.2466 1
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0 3 6 77.8318 26.8950 1
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0 -3 13 834.640 61.9102 1
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0 -3 16 199.311 71.5293 -2
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0 3 19 77.5870 133.900 -2
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0 -3 22-106.053 540.533 1
0 -4 0 4250.84 59.1896 -2
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0 5 -4 21166.4 108.247 1
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0 5 -21 294.992 363.155 1
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0 6 6 33855.5 132.702 1
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-5 8 3 53.5210 101.241 2
5 8 -2 885.581 119.822 2
-5 8 1 87.7061 100.475 2
-5 8 0 79.0308 98.5310 2
-5 8 -1 158.244 91.2208 2
-5 8 -2 1080.72 93.0646 2
-5 8 -3 415.869 102.011 2
-5 8 -4 227.241 144.768 2
-5 8 -5 289.931 153.977 2
-5 8 -6 64.8533 156.080 2
-5 8 -7 273.468 150.966 2
-5 -8 -8 200.257 141.297 2
-5 -8 -9-3.90437 135.098 2
-5 8 -10 58.0321 172.807 2
-5 -8 -11 49.2004 216.264 2
-5 -8 -12-164.344 296.174 2
-5 -8 -13 86.8143 297.916 2
-5 -9 14 41.0288 306.033 2
-5 9 13 117.867 194.783 2
-5 9 12 22.4443 160.315 2
-5 9 11-24.7550 162.831 2
-5 9 10 255.991 120.849 2
-5 9 9 674.604 139.743 2
-5 9 8 203.481 122.444 2
-5 9 7 180.833 132.426 2
-5 9 6 114.686 128.572 2
-5 9 5 7.60360 125.580 2
-5 9 4 366.652 111.040 2
-5 9 3 1338.86 111.981 2
-5 9 2 838.732 115.204 2
5 9 -1 215.882 115.409 2
-5 9 0 171.246 96.6309 2
-5 9 -1 82.8691 88.0975 2
5 -9 2-62.9995 143.176 2
-5 9 -3 570.186 153.847 2
5 -9 4 32.4165 141.121 2
-5 9 -5 32.2826 151.009 2
5 -9 6-36.6309 187.315 2
-5 9 -7-8.63219 166.906 2
-5 9 -8 50.3234 163.257 2
-5 -9 -9 172.961 160.431 2
-5 -9 -10-21.2715 236.280 2
-5 -9 -11 63.2334 290.298 2
-5 10 12 119.082 379.638 2
-5 10 11 90.9698 148.898 2
-5 10 10 104.980 165.501 2
-5 10 9 58.5295 143.177 2
-5 10 8 115.906 136.087 2
-5 10 7 13.1474 144.293 2
-5 10 6 87.1522 133.293 2
-5 10 5 18.8762 132.156 2
-5 10 4-22.5595 104.188 2
-5 10 3-7.37839 109.845 2
-5 10 2 318.493 106.062 2
-5 10 1 260.720 102.147 2
-5 10 0 44.1658 106.665 2
-5 10 -1 10.8323 121.246 2
-5 10 -2 50.7767 142.412 2
5 -10 3 106.657 174.456 2
-5 10 -4 592.621 167.232 2
-5 10 -5 381.716 167.566 2
5 -10 6 289.347 197.046 2
5 -10 7 55.0884 189.490 2
-5 10 -8 80.3816 203.280 2
5 10 9 190.687 400.782 2
5 10 10 158.131 350.696 2
-5 -11 11 233.779 278.909 2
-5 11 10 13.6902 198.252 2
-5 11 9-54.2664 148.754 2
-5 11 8 85.5000 148.044 2
-5 11 7 125.208 154.065 2
-5 11 6 48.2214 153.010 2
-5 11 5 528.086 178.085 2
-5 11 4 45.2890 124.807 2
-5 11 3 145.860 146.532 2
-5 11 2 83.5688 125.276 2
-5 11 1 307.754 108.584 2
-5 11 0 195.569 147.673 2
-5 11 -1 112.088 141.960 2
5 -11 2 16.4144 151.021 2
5 -11 3 100.225 185.323 2
5 -11 4 38.3786 196.067 2
5 -11 5 51.7302 173.425 2
5 11 6 252.202 354.385 2
5 11 7 87.7143 366.817 2
-5 -12 10-152.436 311.729 2
-5 12 9 26.2787 239.766 2
-5 12 8 3.05464 186.719 2
-5 12 7 76.6979 174.571 2
-5 12 6 295.110 173.505 2
-5 12 5-0.18591 166.914 2
-5 12 4 36.0225 158.804 2
5 -12 -3-10.5404 184.694 2
-5 12 2 37.0200 193.063 2
5 -12 -1-31.7112 195.424 2
5 -12 0 419.711 253.498 2
5 -12 1 33.3679 385.682 2
5 12 2-8.37082 282.453 2
5 12 3-109.400 334.059 2
-5 12 -4-106.155 251.906 2
5 12 5 71.4354 354.258 2
5 -12 6 102.323 265.375 2
-5 13 8 188.409 378.410 2
-5 13 7 6.57657 208.744 2
5 -13 -6-4.33187 251.790 2
5 -13 -5 34.0148 241.934 2
5 -13 -4 28.6180 353.725 2
5 -13 -3 98.0543 380.926 2
5 -13 4 194.285 408.184 2
6 0 -6 9336.54 408.006 2
-6 1 2 345.122 218.500 2
6 -3 -16 122.933 294.612 2
-6 5 2 109.015 198.944 2
-6 -8 13-59.5708 274.836 2
7 0 -17-19.3532 293.376 2
7 0 -15-0.54317 197.704 2
7 0 -13 199.197 169.637 2
7 0 -11 40.4004 136.371 2
-7 0 9 424.435 159.920 2
-7 0 7 766.897 150.170 2
-7 0 5 2212.21 161.575 2
-7 0 3 68.3184 130.315 2
-7 0 1 73.2537 113.664 2
-7 0 -1 923.471 151.510 2
-7 0 -3 73.9325 125.464 2
-7 0 -5 215.280 166.884 2
-7 0 -7 92.7631 169.578 2
-7 0 -9 360.968 180.778 2
-7 0 -11-22.0305 289.580 2
-7 0 -13 67.9382 412.702 2
-8 0 12 531.314 360.234 2
-8 0 10 91.4057 347.572 2
-8 0 8 140.846 313.944 2
-8 0 6 1880.76 260.664 2
-8 0 4 134.420 207.928 2
-8 0 2 422.670 223.228 2
-8 0 0 792.362 233.044 2
-8 0 -2-72.4881 227.056 2
-8 0 -4 183.927 214.912 2
-8 0 -6 142.699 292.636 2
-8 0 -8-81.9588 285.814 2
-8 -1 14 128.855 366.675 2
-8 -1 13 136.831 366.622 2
-8 -1 12 49.9753 346.934 2
-8 1 11 43.5122 232.469 2
-8 1 10 217.673 246.269 2
-8 1 9 16.5780 181.848 2
-8 1 8 199.979 155.942 2
-8 1 7-1.87181 188.260 2
-8 -1 6 180.960 141.749 2
-8 1 5 509.088 145.814 2
-8 1 4 59.2513 132.315 2
-8 1 3-24.9599 128.106 2
-8 1 2-4.01922 149.787 2
-8 1 1-35.0039 136.643 2
-8 1 0 746.620 159.158 2
-8 1 -1 486.617 163.638 2
-8 1 -2-3.78681 149.223 2
-8 1 -3 53.0347 143.971 2
-8 1 -4 227.848 127.160 2
-8 1 -5 120.470 171.568 2
-8 1 -6 69.4520 161.050 2
-8 1 -7 62.4895 178.223 2
-8 1 -8 144.369 178.308 2
-8 1 -9 135.583 202.898 2
-8 -2 15-2.86655 356.633 2
-8 -2 14 55.5518 338.285 2
-8 -2 13 29.9249 337.006 2
-8 -2 12-6.18885 323.960 2
-8 -2 11 138.627 350.695 2
-8 -2 10-86.0128 204.404 2
-8 -2 9 40.4774 177.464 2
-8 2 8 26.2147 163.606 2
-8 2 7 361.855 136.931 2
-8 2 6 84.3265 149.787 2
-8 2 5 114.220 171.637 2
-8 2 4 33.5950 149.120 2
-8 2 3 465.860 158.772 2
-8 2 2 557.187 161.976 2
-8 2 1 28.5614 145.550 2
-8 2 0 106.993 150.464 2
-8 2 -1 41.5866 149.840 2
-8 2 -2-22.5315 135.801 2
-8 2 -3 265.815 129.122 2
-8 2 -4 231.857 143.148 2
-8 2 -5-48.2370 156.152 2
-8 2 -6 89.8635 178.640 2
-8 2 -7 111.233 176.241 2
-8 2 -8-28.0586 174.289 2
-8 -2 -9 26.5360 294.451 2
-8 -3 14-203.891 341.498 2
-8 -3 13 135.721 330.263 2
-8 -3 12-127.798 332.766 2
-8 -3 11 25.6213 309.251 2
-8 -3 10 16.3173 341.024 2
-8 -3 9 1200.00 236.801 2
-8 -3 8 55.7372 205.292 2
-8 -3 7-77.6522 165.577 2
-8 -3 6 130.482 173.309 2
-8 3 5-23.3763 178.118 2
-8 3 4-51.5860 177.750 2
-8 3 3 1003.63 182.871 2
-8 3 2 175.284 169.761 2
-8 3 1 86.4244 164.394 2
-8 3 0-131.292 174.635 2
-8 3 -1 99.0945 150.827 2
-8 3 -2 3.48594 154.683 2
-8 3 -3 202.850 123.677 2
-8 3 -4 9.42502 180.423 2
-8 3 -5-40.0053 206.206 2
-8 3 -6-25.2774 170.961 2
-8 3 -7 25.9817 211.529 2
-8 3 -8 5.59560 202.675 2
-8 -4 14 151.273 340.519 2
-8 -4 13 144.579 336.571 2
-8 -4 12 35.3209 333.806 2
-8 -4 11 117.834 322.752 2
-8 -4 10 122.521 251.895 2
-8 -4 9 50.7819 211.704 2
-8 -4 8 249.420 157.673 2
-8 -4 7 115.027 177.588 2
-8 -4 6-30.7721 170.329 2
-8 -4 5 69.6444 182.243 2
-8 4 4 18.2841 179.320 2
-8 4 3 644.239 190.537 2
-8 4 2 499.242 181.558 2
-8 4 1-13.2228 170.952 2
-8 -4 0-46.7508 207.512 2
-8 4 -1 113.489 165.550 2
-8 -4 -2 137.228 211.593 2
-8 -4 -3 170.835 223.607 2
-8 -4 -4 291.834 228.659 2
-8 -4 -5-92.0349 279.372 2
-8 -4 -6-68.5790 308.943 2
-8 -5 13 22.9861 334.293 2
-8 -5 12-57.9187 324.021 2
-8 -5 11-81.0989 312.087 2
-8 -5 10 100.742 339.305 2
-8 5 9 16.0773 179.281 2
-8 5 8 55.9777 179.947 2
-8 5 7-26.7166 177.941 2
-8 5 6 194.534 182.976 2
-8 5 5 139.886 194.492 2
-8 5 4 280.071 181.717 2
-8 5 3-31.5090 179.862 2
-8 5 2-19.7021 181.014 2
-8 5 1 40.9456 169.243 2
-8 5 0 174.686 166.408 2
-8 -5 -1 78.5137 235.494 2
-8 5 -2-5.68734 169.968 2
-8 -5 -3 229.855 229.424 2
-8 -5 -4 273.252 206.170 2
-8 -6 10 29.9751 310.060 2
-8 6 9-121.973 247.347 2
-8 6 8-14.3150 188.488 2
-8 6 7-13.6016 195.620 2
-8 6 6 584.017 199.504 2
-8 6 5 134.445 188.076 2
-8 6 4 184.506 196.560 2
-8 6 3-3.90219 194.732 2
-8 6 2 113.312 184.394 2
-8 6 1 15.4979 178.491 2
-8 6 0 370.083 187.461 2
8 -6 1 381.728 387.329 2
-8 7 8 61.8991 242.054 2
-8 7 7 195.694 252.570 2
-8 7 6 173.638 249.964 2
-8 7 5 223.059 254.132 2
-8 7 4-104.836 246.584 2
-8 7 3 20.9294 242.418 2
-8 7 2-40.2517 232.536 2
8 -7 -1 368.236 403.370 2
8 -7 0 125.615 367.166 2
8 7 5 155.115 347.319 2
-8 8 7 204.582 260.132 2
-8 8 6-0.83605 249.664 2
-8 8 5 24.3305 252.919 2
-8 8 4 162.652 243.313 2
8 -8 -3 138.497 358.684 2
8 -9 -6-52.4704 362.841 2
9 1 -12 323.189 441.233 2
9 2 -10-71.9806 424.389 2
9 -4 -8 247.114 368.274 2
;
_shelx_hkl_checksum 30447
_shelx_res_file
;
TITL v316_15_twin+abs2_twin1_hklf4_a.res in P2(1)/n
v316_15_twin+abs2_twin1_hklf4.res
created by SHELXL-2018/3 at 12:23:34 on 09-Jul-2020
REM Old TITL V316_15_TWIN+ABS2_twin1_hklf4 in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.150, Rweak 0.011, Alpha 0.019
REM 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C9 N O I3
CELL 0.71073 7.084 11.5247 16.3921 90 98.738 90
ZERR 4 0.0002 0.0004 0.0006 0 0.003 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O I
UNIT 28 36 8 8 12
EQIV $1 1+X,+Y,+Z
EQIV $2 1.5-X,0.5+Y,0.5-Z
L.S. 16 0 0
PLAN 6
TEMP 21.9(10)
CONF
HTAB N1 O1
HTAB N1 I1
HTAB N1 I1_$1
HTAB C5 O1_$2
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
MERG 0
OMIT 0 60
OMIT -4 -6 -3
OMIT 0 0 2
OMIT 1 0 -1
OMIT 0 1 -2
OMIT 0 -1 -3
OMIT 0 -1 -4
OMIT 0 1 -5
REM
REM
REM
WGHT 0.030200
BASF 0.24074
FVAR 1.20629
I1 5 0.234119 0.646765 0.491736 11.00000 0.04853 0.04621 =
0.06893 -0.00626 0.00820 -0.00020
O1 4 0.726833 0.635164 0.306610 11.00000 0.12596 0.05139 =
0.08935 -0.02660 0.03265 -0.00587
N1 3 0.726207 0.669148 0.462808 11.00000 0.04598 0.03859 =
0.06500 -0.00166 0.00918 -0.00075
AFIX 137
H1A 2 0.705654 0.624493 0.418041 11.00000 -1.20000
H1B 2 0.632377 0.658951 0.492567 11.00000 -1.20000
H1C 2 0.837132 0.649941 0.492907 11.00000 -1.20000
AFIX 0
C1 1 0.731900 0.791098 0.437960 11.00000 0.03109 0.03184 =
0.05196 -0.00250 0.00527 0.00028
O2 4 0.692378 0.775422 0.219436 11.00000 0.11249 0.10876 =
0.04966 -0.02102 0.01402 -0.00065
N2 3 0.712860 0.739279 0.289234 11.00000 0.05114 0.07641 =
0.05984 -0.01688 0.01730 -0.00508
C2 1 0.743478 0.873379 0.500621 11.00000 0.04255 0.03860 =
0.04863 0.00485 0.00433 0.00117
C3 1 0.745526 0.990416 0.476817 11.00000 0.05557 0.03570 =
0.05710 -0.00228 0.01015 0.00027
AFIX 43
H3 2 0.750588 1.047841 0.516951 11.00000 -1.20000
AFIX 0
C4 1 0.740278 1.021872 0.396366 11.00000 0.05737 0.03801 =
0.07330 0.01406 0.00974 -0.00409
AFIX 43
H4 2 0.744029 1.099935 0.382326 11.00000 -1.20000
AFIX 0
C5 1 0.729332 0.937506 0.335289 11.00000 0.04661 0.05537 =
0.05272 0.00840 0.00775 0.00341
AFIX 43
H5 2 0.724229 0.958706 0.280255 11.00000 -1.20000
AFIX 0
C6 1 0.726154 0.823634 0.356758 11.00000 0.04362 0.04141 =
0.03700 -0.00964 0.00786 -0.00233
C7 1 0.751295 0.841094 0.590668 11.00000 0.09664 0.04831 =
0.04979 0.00575 0.00771 -0.00586
AFIX 137
H7A 2 0.637762 0.799188 0.597706 11.00000 -1.50000
H7B 2 0.759889 0.910330 0.623588 11.00000 -1.50000
H7C 2 0.861188 0.793308 0.607767 11.00000 -1.50000
AFIX 0
I2 5 0.256508 0.483225 0.331988 11.00000 0.05486 0.04561 =
0.07984 0.01677 0.00274 -0.00325
I3 5 0.285803 0.330348 0.204034 11.00000 0.05358 0.06061 =
0.08162 0.00959 0.01894 0.00349
HKLF 5
REM v316_15_twin+abs2_twin1_hklf4_a.res in P2(1)/n
REM wR2 = 0.0586, GooF = S = 0.800, Restrained GooF = 0.800 for all data
REM R1 = 0.0306 for 3181 Fo > 4sig(Fo) and 0.0787 for all 5822 data
REM 130 parameters refined using 0 restraints
END
WGHT 0.0301 0.0000
REM Highest difference peak 0.702, deepest hole -0.776, 1-sigma level 0.111
Q1 1 0.2273 0.6257 0.5405 11.00000 0.05 0.70
Q2 1 0.3342 0.4527 0.2998 11.00000 0.05 0.66
Q3 1 -0.0238 0.4856 0.3269 11.00000 0.05 0.60
Q4 1 0.5171 0.6557 0.4920 11.00000 0.05 0.55
Q5 1 0.2869 0.3189 0.1724 11.00000 0.05 0.49
Q6 1 0.3249 0.2771 0.2438 11.00000 0.05 0.47
;
_shelx_res_checksum 87612
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
I I1 0.23412(5) 0.64676(3) 0.49174(2) 0.05463(12) Uani d 1 . .
O O1 0.7268(7) 0.6352(3) 0.3066(3) 0.0872(15) Uani d 1 . .
N N1 0.7262(6) 0.6691(3) 0.4628(2) 0.0498(11) Uani d 1 . .
H H1A 0.705654 0.624493 0.418041 0.060 Uiso calc 1 . .
H H1B 0.632377 0.658951 0.492567 0.060 Uiso calc 1 . .
H H1C 0.837132 0.649941 0.492907 0.060 Uiso calc 1 . .
C C1 0.7319(7) 0.7911(4) 0.4380(3) 0.0384(11) Uani d 1 . .
O O2 0.6924(7) 0.7754(4) 0.2194(3) 0.0901(15) Uani d 1 . .
N N2 0.7129(7) 0.7393(5) 0.2892(3) 0.0615(13) Uani d 1 . .
C C2 0.7435(7) 0.8734(4) 0.5006(3) 0.0435(12) Uani d 1 . .
C C3 0.7455(7) 0.9904(4) 0.4768(3) 0.0493(13) Uani d 1 . .
H H3 0.750588 1.047841 0.516951 0.059 Uiso calc 1 . .
C C4 0.7403(7) 1.0219(4) 0.3964(3) 0.0562(15) Uani d 1 . .
H H4 0.744029 1.099935 0.382326 0.067 Uiso calc 1 . .
C C5 0.7293(7) 0.9375(5) 0.3353(3) 0.0515(13) Uani d 1 . .
H H5 0.724229 0.958706 0.280255 0.062 Uiso calc 1 . .
C C6 0.7262(7) 0.8236(4) 0.3568(3) 0.0405(12) Uani d 1 . .
C C7 0.7513(9) 0.8411(4) 0.5907(3) 0.0653(17) Uani d 1 . .
H H7A 0.637762 0.799188 0.597706 0.098 Uiso calc 1 . .
H H7B 0.759889 0.910330 0.623588 0.098 Uiso calc 1 . .
H H7C 0.861188 0.793308 0.607767 0.098 Uiso calc 1 . .
I I2 0.25651(6) 0.48323(3) 0.33199(2) 0.06088(13) Uani d 1 . .
I I3 0.28580(6) 0.33035(3) 0.20403(2) 0.06437(13) 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
I1 0.0485(2) 0.0462(2) 0.0689(2) -0.00020(18) 0.00820(19) -0.00626(17)
O1 0.126(4) 0.051(3) 0.089(3) -0.006(3) 0.033(3) -0.027(2)
N1 0.046(3) 0.039(2) 0.065(3) -0.001(2) 0.009(2) -0.002(2)
C1 0.031(3) 0.032(2) 0.052(3) 0.000(2) 0.005(2) -0.002(2)
O2 0.112(4) 0.109(4) 0.050(3) -0.001(3) 0.014(3) -0.021(2)
N2 0.051(3) 0.076(4) 0.060(3) -0.005(3) 0.017(3) -0.017(3)
C2 0.043(3) 0.039(3) 0.049(3) 0.001(2) 0.004(2) 0.005(2)
C3 0.056(4) 0.036(3) 0.057(4) 0.000(3) 0.010(3) -0.002(2)
C4 0.057(4) 0.038(3) 0.073(4) -0.004(3) 0.010(3) 0.014(3)
C5 0.047(3) 0.055(3) 0.053(3) 0.003(3) 0.008(3) 0.008(3)
C6 0.044(3) 0.041(3) 0.037(3) -0.002(2) 0.008(2) -0.010(2)
C7 0.097(5) 0.048(3) 0.050(3) -0.006(3) 0.008(3) 0.006(3)
I2 0.0549(2) 0.0456(2) 0.0798(3) -0.00325(19) 0.00274(19) 0.01677(19)
I3 0.0536(3) 0.0606(3) 0.0816(3) 0.0035(2) 0.0189(2) 0.0096(2)
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'
I I -0.4742 1.8119 '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 -8 -20 0.0590
1 8 20 0.0262
10 2 -6 0.0885
-10 -2 7 0.0901
0 3 -22 0.0210
-1 -16 -1 0.0595
1 15 -8 0.0183
0 -12 15 0.0811
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 ?
C2 C1 N1 . . 116.7(4) ?
C6 C1 N1 . . 122.1(4) ?
C6 C1 C2 . . 121.2(4) ?
O1 N2 C6 . . 118.5(5) ?
O2 N2 O1 . . 123.3(5) ?
O2 N2 C6 . . 118.2(5) ?
C1 C2 C3 . . 116.8(4) ?
C1 C2 C7 . . 122.8(4) ?
C3 C2 C7 . . 120.4(4) ?
C2 C3 H3 . . 119.2 ?
C4 C3 C2 . . 121.6(4) ?
C4 C3 H3 . . 119.2 ?
C3 C4 H4 . . 119.9 ?
C3 C4 C5 . . 120.1(5) ?
C5 C4 H4 . . 119.9 ?
C4 C5 H5 . . 120.3 ?
C6 C5 C4 . . 119.4(5) ?
C6 C5 H5 . . 120.3 ?
C1 C6 N2 . . 122.6(4) ?
C5 C6 C1 . . 120.9(4) ?
C5 C6 N2 . . 116.5(5) ?
C2 C7 H7A . . 109.5 ?
C2 C7 H7B . . 109.5 ?
C2 C7 H7C . . 109.5 ?
H7A C7 H7B . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 N2 . 1.234(6) ?
N1 H1A . 0.8900 ?
N1 H1B . 0.8900 ?
N1 H1C . 0.8900 ?
N1 C1 . 1.466(5) ?
C1 C2 . 1.391(6) ?
C1 C6 . 1.378(6) ?
O2 N2 . 1.205(6) ?
N2 C6 . 1.465(6) ?
C2 C3 . 1.405(6) ?
C2 C7 . 1.515(6) ?
C3 H3 . 0.9300 ?
C3 C4 . 1.363(6) ?
C4 H4 . 0.9300 ?
C4 C5 . 1.389(7) ?
C5 H5 . 0.9300 ?
C5 C6 . 1.360(6) ?
C7 H7A . 0.9600 ?
C7 H7B . 0.9600 ?
C7 H7C . 0.9600 ?
I2 I3 . 2.7711(6) ?
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 O1 . 0.89 1.86 2.591(6) 138.1 yes
N1 H1B I1 . 0.89 2.82 3.598(4) 146.4 yes
N1 H1C I1 1_655 0.89 2.82 3.566(4) 143.0 yes
C5 H5 O1 2_655 0.93 2.54 3.304(6) 140.1 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
O1 N2 C6 C1 . . . . -7.5(8) ?
O1 N2 C6 C5 . . . . 173.6(5) ?
N1 C1 C2 C3 . . . . -178.9(4) ?
N1 C1 C2 C7 . . . . 0.4(7) ?
N1 C1 C6 N2 . . . . 0.4(7) ?
N1 C1 C6 C5 . . . . 179.2(5) ?
C1 C2 C3 C4 . . . . -1.3(8) ?
O2 N2 C6 C1 . . . . 173.9(5) ?
O2 N2 C6 C5 . . . . -5.0(7) ?
C2 C1 C6 N2 . . . . -179.6(5) ?
C2 C1 C6 C5 . . . . -0.8(8) ?
C2 C3 C4 C5 . . . . 1.1(8) ?
C3 C4 C5 C6 . . . . -0.7(8) ?
C4 C5 C6 C1 . . . . 0.6(8) ?
C4 C5 C6 N2 . . . . 179.5(5) ?
C6 C1 C2 C3 . . . . 1.1(7) ?
C6 C1 C2 C7 . . . . -179.6(5) ?
C7 C2 C3 C4 . . . . 179.4(5) ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.7593(5) 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 0.2407(5) -0.9996 0.0001 0.0000 0.0000 -0.9998 0.0000 0.7013 0.0000 0.9996
_cod_database_fobs_code 2022328